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Quality Assurance Program Rev. 17 December 2012 Rev #: 17 Document Title: Local Work Instructions

Local Work Instructions ............................................................................................................... 1

1 Professional Sales Process Tools ........................................................................................ 3 1.1 Customer Specialty Gas Evaluation Offer ...................................................................................... 4 1.2 Customer Specialty Gas Evaluation ................................................................................................ 6 1.3 Customer Specialty Gas Evaluation Report .................................................................................... 9 1.4 Customer Instrument Survey ........................................................................................................ 12 1.5 Helium to Hydrogen Conversion Considerations ......................................................................... 16

2 Product Specifications ......................................................................................................... 19

3 Equipment Specifications/LWIs .......................................................................................... 30 3.1 Vacuum and Billing Gauges ......................................................................................................... 31 3.2 Thermometers ............................................................................................................................... 33 3.3 Cylinder Specifications ................................................................................................................. 35 3.4 Cylinder Paint Application Guide ................................................................................................. 38

4 Cylinder Filling LWIs ............................................................................................................ 40 4.1 High Pressure Cylinder Pre-Fill Inspection .................................................................................. 41 4.2 High Pressure Oxygen Cylinder Filling ........................................................................................ 45 4.3 High Pressure Inert Gas & Mixture Cylinder Filling .................................................................... 47 4.4 High Pressure Flammable Gas & Mixture Cylinder Filling ......................................................... 50 4.5 High Pressure Carbon Dioxide Cylinder Filling Procedures ........................................................ 54 4.6 Cryogenic Container Fill Procedures ............................................................................................ 58 4.7 Mixture Compatibilities ................................................................................................................ 60 4.8 Micro Cylinder Procedure ............................................................................................................. 61

5 Analytical LWIs ..................................................................................................................... 64 5.1 Standard Definitions ..................................................................................................................... 65 5.2 Conversion Factors ....................................................................................................................... 68 5.3 Oxygen PPM Analysis .................................................................................................................. 69 5.4 Illinois Instruments Model 6000 Oxygen Analysis ...................................................................... 70 5.5 Moisture PPM Analysis (Electrolytic Hygrometer) ...................................................................... 71 5.6 Moisture PPM Analysis (Panametrics Series 35) ......................................................................... 72 5.7 Total Hydrocarbon Analysis ......................................................................................................... 73 5.8 Baseline 8800 Total Hydrocarbon Analysis ................................................................................. 75 5.9 Cycle Purge Procedure .................................................................................................................. 76 5.10 Gas Chromatograph Analysis ..................................................................................................... 77 5.11 Gas Chromatograph System Suitability/Calibration/ Analysis Worksheet ................................ 78 5.12 Authorized Gas Chromatograph Methods .................................................................................. 80 5.13 GC Method Authorization .......................................................................................................... 81 5.14 EZ Chrom Procedures ................................................................................................................. 82 5.15 Chrom Perfect System Suitability, Calibration and Analysis ..................................................... 84 5.16 GOW-MAC Discharge Ionization Detector Setup ..................................................................... 88 5.17 Analyzers Not Listed in the Manual ........................................................................................... 89 5.18 Taylor OA 224 Oxygen Analyzer ............................................................................................... 90 5.19 MEECO Gemini Plus Analyzer .................................................................................................. 92 5.20 Meeco Aquamatic Plus Moisture Analyzer ................................................................................ 95 5.21 MEECO Model W Moisture Analyzer ....................................................................................... 97 5.22 F310-1 Supplier Assessment Questionnaire ............................................................................. 102 5.23 COCs and COAs ....................................................................................................................... 108 5.24 Calibration Standards ................................................................................................................ 111 5.25 Calibration Intervals .................................................................................................................. 113 5.26 Calibration Records ................................................................................................................... 115

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5.27 Breathing Mixtures ................................................................................................................... 120 5.28 Compressed Air ......................................................................................................................... 122 5.29 Beckman CO2/CO Analyzer System ......................................................................................... 124 5.30 Gaseous Product Odor Test ....................................................................................................... 126 5.31 MSA Infrared Analyzer ............................................................................................................ 127 5.32 Gas Detector Tubes ................................................................................................................... 129 5.33 Gow Mac Series 550 Gas Chromatograph ................................................................................ 131 5.34 Gow-Mac Thermal Conductivity Analyzer .............................................................................. 133 5.35 Beckman Hydrocarbon Analyzer – Model 400 ........................................................................ 135 5.36 Teledyne Trace Oxygen Analyzer Model 316 .......................................................................... 138 5.37 Teledyne 320 Series Oxygen Analyzer ..................................................................................... 140 5.38 Teledyne Trace Oxygen Analyzer Model 311 .......................................................................... 142 5.39 Delphi Electrochemical Oxygen Analyzer ................................................................................ 144 5.40 Teledyne Trace Oxygen Analyzer ............................................................................................ 147 5.41 Beckman Moisture Analyzer .................................................................................................... 150 5.42 Fuel Oxidizer System Self Assessment .................................................................................... 154 5.43 Periodic Scale Verifications ...................................................................................................... 158 5.44 Certification Period (Shelf Life) For Calibration Gas Standards .............................................. 160 5.45 Reporting Significant Digits In Analytical Results ................................................................... 161 5.46 Moisture Dewpoint Conversion Chart ...................................................................................... 162 5.47 Portable Calibration Gas Disposal Guidelines .......................................................................... 164 5.48 Preparing NIST Traceable Gravimetric Mixtures ..................................................................... 165 5.49 Gravimetric System Uncertainty Calculations .......................................................................... 168 5.50 Elements of Analytical Results ................................................................................................. 172 5.51 Considering Analytical Uncertainty Near Tolerance Limits .................................................... 174 5.52 Calibrating Electronic Scales By The Specialty Gas Lab ......................................................... 176

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Quality Assurance Program Rev. 9 Nov. 2011 Rev #: 0 Document Title: 1 Professional Sales Process Tools

This section contains the sales process tools for PurityPlus Specialty Gas sales and customer service professionals.

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Quality Assurance Program Rev. 9 Nov 2011 Rev #: 0 Document Title: 1.1 Customer Specialty Gas Evaluation Offer

1. OBJECTIVE To introduce an offer to conduct a specialty gas evaluation at a customer or prospect. 2. SCOPE This procedure applies to the PurityPlus specialty gases sales professional. 3. RESPONSIBILITIES It is the responsibility of sales personnel to determine how to best serve the company’s and customer’s

needs can be met through a systematic customer evaluation. 4. PROCEDURE 4.1. Use the template on the following pages to offer to conduct specialty gas assessment at the customer or

prospect. This assessment can help determine opportunities for the customer to improve their usage of specialty gases.

4.2. The following information is available as a file for editing. See the PurityPlus producer resource website. 4.3. Refer to PurityPlus Tier 2 Sales Training course for implementation instructions.

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Quality Assurance Program Rev. 9 Nov 2011 Rev #: 0 Document Title: 1.2 Customer Specialty Gas Evaluation

1 OBJECTIVE

To establish the procedures and for conducting a specialty gas evaluation at a customer or prospect. 2 SCOPE

This procedure applies to the PurityPlus specialty gases sales professional. 3 RESPONSIBILITIES

It is the responsibility of sales personnel to determine how to best serve the company’s and customer’s needs can be met through a systematic customer evaluation.

4 PROCEDURE 4.1 Use the template on the following pages to conduct specialty gas assessment at the customer or

prospect. This assessment can help determine opportunities for the customer to improve their usage of specialty gases.

4.2 The following information is available as a file for editing. See the PurityPlus producer resource website. 4.3 Refer to PurityPlus Tier 2 Sales Training course for implementation instructions.

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Quality Assurance Program Rev. 9 Nov 2011 Rev #: 0 Document Title: 1.3 Customer Specialty Gas Evaluation Report

1. OBJECTIVE To establish the report format for a specialty gas evaluation at a customer or prospect. 2. SCOPE This procedure applies to the PurityPlus specialty gases sales professional. 3. RESPONSIBILITIES It is the responsibility of sales personnel to report to the customer specific opportunities for process

improvements. 4. PROCEDURE

4.1. Use the template on the following pages to report specialty gas assessments for the customer or prospect.

4.2. The following information is available as a file for editing. See the PurityPlus producer resource website. 4.3. Refer to PurityPlus Tier 2 Sales Training course for implementation instructions.

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Date:

Prepared by:

A. Questions about gas use / mode of supply

B. Cylinder Handling / Storage Questions

Cylinder Handling, Cylinder Location,

C. Equipment/Gas Distribution Questions

Purge Assemblies, Pigtails/Flex Hoses, Purification, Valves & Accessories, Piping

D. Safety Questions

Gas Monitors, General

PERFORMANCE, EFFICIENCY AND SAFETEY RECOMMENDATIONS

AUDIT FORM

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Quality Assurance Program Rev. 9 Nov 2011 Rev #: 0 Document Title: 1.4 Customer Instrument Survey

1 OBJECTIVE

To establish the survey format for a specialty gas instrument evaluation at a customer or prospect. 2 SCOPE


It is the responsibility of sales personnel to determine how best to survey customer specific opportunities. 4 PROCEDURE 4.1 Use the templates on the following pages to survey specialty gas instrument for the customer or prospect.

Use the information learned to propose specific solutions/opportunities to the customer/prospect. 4.2 The following information is available as a file for editing. See the PurityPlus producer resource website. 4.3 Refer to PurityPlus Tier 2 Sales Training course for implementation instructions.

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Quality Assurance Program Rev. 12 June 2012 Rev #: 0 Document Title: 1.5 Helium to Hydrogen Conversion Considerations

1 OBJECTIVE

To identify the issues to consider when converting gas chromatographs from helium carrier gases to hydrogen carrier gases.

2 SCOPE


It is the responsibility of sales personnel to determine how best to introduce customers to the conversion options.

4. PROCEDURE

4.1. Negative Considerations - Consider the following items when converting a customer from helium to hydrogen support gases

4.1.1. Inert (non-flammable/non-reactive) nature of helium

4.1.2. Specific Detectors - Some instruments require the high ionization potential of helium. Helium has the highest ionization potential of any gas and must be used in “Helium Ionization Detectors” (HID), “Discharge Ionization Detectors” (DID), Pulsed Discharge Ionization Detectors (PDID), etc. These instruments simply will not work with gases other than helium.

4.1.3. Building Codes – Storage of hydrogen cylinders is restricted in some building codes. This can be mitigated by an onsite hydrogen generation system.

4.1.4. Utility Costs – The customer will have higher electricity costs with an onsite hydrogen generator. One estimate is about $200 per year to run a typical generator.

4.2. Positive Considerations - Consider the following items when converting a customer from helium to hydrogen support gases

4.2.1. Cost – for the short and long term, hydrogen will be less expensive than helium.

4.2.2. Availability – Hydrogen is much more abundant than helium. We have seen periodic shortages in the helium market, while the hydrogen market is diverse, larger and more available.

4.2.3. Purity – very high purity hydrogen is available – similar to helium purity

4.2.4. Sensitivity – Hydrogen has even a higher thermal conductivity than helium. This makes it a good carrier gas choice for thermal conductivity detectors.

4.2.5. Speed – Hydrogen allows a higher linear velocity (faster separations) than helium or nitrogen carrier gases for similar column efficiency.

4.3. Other considerations –

4.3.1. MFC – Some GCs have Mass Flow Controllers that are programmed for helium as the only carrier gas option. Usually, workarounds can be implemented. The GC manufacturer may be able to supply new factors for hydrogen. Consider using a flowmeter calibrated for hydrogen and manually set the flow. The MFC could be reset using the new indicated flow (“as helium”) in order to deliver the necessary hydrogen flow.

4.3.2. Regulators – The existing supply gas regulators may be designed for inert gases. Consider a regulator specifically designed for hydrogen. Adaptors are not recommended to convert a regulator to flammable gas service. See page 4.12 in the PurityPlus catalog for the 300 series brass regulator, or equivalent.

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4.3.3. Tubing and Accessories – Assure that the supply tubing and other components between the regulator and instrument are compatible

4.3.4. Leaks – Use a compatible leak detector to verify that there are no leaks before applying power to instruments. Assure the instrument is rated for hydrogen carrier/support gas.

4.3.5. Redundant Supply – Even if the customer decides to use a hydrogen generator, suggest a hydrogen cylinder onsite as a backup in case of generator/power failure.

4.4. GC Flame Ionization Detector - General Conversion Procedure - (Adapted from Parker Balston)

4.4.1. Review and document all existing run conditions

4.4.1.1. Leak check the system; leaks may affect the determination of the actual flows you are using for your analysis.

4.4.1.2. Measure and record the existing dead volume time and calculate the Linear Gas Rate (LGR).

4.4.1.3. Measure and record the Septum flow at the initial run temperature.

4.4.1.4. Measure and record the Make-up Gas rate.

4.4.1.5. Measure and record Vent flow at initial run temperature.

4.4.1.6. Measure and record the Fuel gas (Hydrogen) flow rate.

4.4.1.7. Measure and record the Air gas flow rate.

4.4.1.8. Document any flow changes that take place during the run.

4.4.1.9. Document any temperature program rates used.

4.4.1.10. Obtain a good sample chromatogram for comparison with the chromatogram obtained after conversion.

4.4.2. Perform all routine maintenance before switching to Hydrogen

4.4.2.1. Change purifiers - Add purifiers to lines as needed to obtain at least 99.9999% pure gas.

4.4.2.2. Change septa - Use a good low bleed septum.

4.4.2.3. Change Injection Port Liners/Inserts and Seals - Clean as needed and avoid contamination with oils. Clean parts with acetone before installation. Caution: Acetone is flammable and can cause health issues. Avoid open flames in the laboratory.

4.4.2.4. Clean Detector/Detector inserts/Jets.

4.4.3. Installation of new lines and purifiers

4.4.3.1. Carrier gas lines – Depressurize and vent the Hydrogen line. Then cut the fuel gas line (Hydrogen) and add a tee. Extend a line into the Carrier Gas in-port behind the GC from the other side of the tee.

4.4.3.2. Add purifiers to this line if gas purity does not meet at least 99.9999% purity. Use hydrocarbon, oxygen and moisture removing purifiers or a combination purifier to obtain the needed gas purity. Hint: Add purifiers that have indicators to show the percentage of usage of the purifier so that you know when to change the purifiers. See the PurityPlus catalog section 4.100 for purifiers.

4.4.3.3. Add new make-up gas line preferably for use with Nitrogen.

4.4.4. Establish Flows for Hydrogen and Nitrogen (Make-up Gas)

4.4.4.1. Carrier Gas

4.4.4.1.1. Turn gas on and establish column flow with the oven off. With some computer controlled systems, it may be necessary to change the carrier gas input to indicate you are using Hydrogen so that the system makes the correct flow adjustments based on the density of Hydrogen.

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4.4.4.1.2. Turn Oven, Injection port, and Detector on after one hour of flow. (It is important to purge all lines and purifiers before establishing temperatures in the various zones of the GC. It takes a considerable amount of time to purge lines and purifiers. Hint: If time permits, it would be best to purge the system overnight.

4.4.4.1.3. Establish Split Vent flow and measure Septum Vent flow.

4.4.4.1.4. Bring the column/oven up to run temperature and again measure the column flow.

4.4.4.2. Detector Flows

4.4.4.2.1. Establish the correct flow of Hydrogen to the detector (this includes the sum of all sources of hydrogen going into the detector).

4.4.4.2.2. Establish the correct Make-up gas flow.

4.4.4.2.3. Establish the correct Air flow.

4.4.4.3. System Adjustments

4.4.4.3.1. Ignite the detector and turn on any needed detector electronics. Give the system one hour to stabilize. Hint: A longer warm up period (e.g. overnight) may lead to a more stable response.

4.4.4.3.2. Recheck the system to make sure that all run conditions and temperatures are correct.

4.4.4.3.3. Inject and measure the dead volume time using methane and calculate the Linear Gas Rate (LGR). Make corrections to the LGR as needed.

4.4.4.4. Flow Calculations: Flow = π r2 L / TR ---Where π = 3.1416 ---r = radius of the column in cm (convert from mm) ---L = Length of the column in cm (convert from meters) ---TR = Retention time of a non retained peak typically methane Where LGR = L / TR = L / µ Simplified ….. Flow = π r2 µ (Remember to use units in cm.)

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Quality Assurance Program Rev. 8 April 2011 Rev #: 3 Document Title: 2 Product Specifications

1. OBJECTIVE This section contains the established specifications for PurityPlus Specialty Gas products. 2. SCOPE This procedure applies to the PurityPlus specialty gases lab. 3. RESPONSIBILITIES

It is the responsibility of all laboratory personnel to ensure that these specifications are maintained as described, that these specifications are reviewed and updated as necessary, and that proper support documentation is maintained.

4. Specifications

Acetylene PurityPlus Purified 2.6 Oxygen plus CH4 < 4000 ppm Gas Phase 1/batch (For Atomic Absorption) PH3 < 20 ppm Gas Phase 1/batch Use Draeger Tube P/N 8103341- Phosphine 0.1/b in acetylene 0.1 - 15 ppm, or equivalent. Air PurityPlus Ultra Zero Total Hydrocarbons < 0.1 ppm Gas Phase 1/batch Moisture < 3 ppm Gas Phase 1/batch Oxygen 19.5% to 23.5% Gas Phase 1/batch Carbon Dioxide < 1 ppm Gas Phase 1/batch Carbon Monoxide < 1 ppm Gas Phase 1/batch PurityPlus Zero Total Hydrocarbons 1 ppm Gas Phase 1/batch Oxygen 19.5% to 23.5% Gas Phase 1/batch PurityPlus Extra Dry Moisture < 8 ppm Gas Phase 1/batch Oxygen 19.5 - 23.5% Gas Phase 1/batch

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Argon Purity Plus 6.0 Oxygen < 0.15 ppm Gas Phase Individual Moisture < 0.15 ppm Gas Phase Individual Nitrogen < 0.40 ppm Gas Phase Individual THC < 0.10 ppm Gas Phase Individual CO / CO2 < 0.10 ppm Gas Phase Individual PurityPlus 5.0 Oxygen < 2 ppm Gas Phase 1/batch Moisture < 2 ppm Gas Phase 1/batch Total Hydrocarbons < 0.5 ppm Gas Phase 1/batch PurityPlus N2 Free 5.0 Oxygen < 2 ppm Gas Phase 1/batch Moisture < 2 ppm Gas Phase 1/batch Nitrogen < 5 ppm Gas Phase 1/batch Total Hydrocarbons < 0.5 ppm Gas Phase 1/batch PurityPlus 4.8 Oxygen < 5 ppm Gas Phase 1/batch Total Hydrocarbons < 2 ppm Gas Phase 1/batch Moisture < 5 ppm Gas Phase 1/batch PurityPlus Zero 4.8 Total Hydrocarbons < 0.5 ppm Gas Phase 1/batch PurityPlus 4.8 6000 psi Oxygen < 10 ppm Gas Phase 1/batch Moisture < 5 ppm Gas Phase 1/batch

Carbon Dioxide PurityPlus Laser 4.5 Moisture < 5 ppm Gas Phase 1/batch Oxygen < 5 ppm Gas Phase 1/batch Total Hydrocarbons < 1 ppm Gas Phase 1/batch PurityPlus Coleman 4.0 Moisture < 10 ppm Gas Phase 1/batch Oxygen < 20 ppm Gas Phase 1/batch Nitrogen < 50 ppm Gas Phase 1/batch PurityPlus Anaerobic 3.0 Oxygen < 20 ppm Gas Phase 1/batch PurityPlus 2.8 Moisture < 20 ppm Gas Phase 1/batch

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Helium PurityPlus 6.0 Oxygen < 0.5 ppm Gas Phase Individual Moisture < 1 ppm Gas Phase Individual Nitrogen < 1 ppm Gas Phase Individual Total Hydrocarbons < 0.2 ppm Gas Phase Individual Carbon Monoxide < 0.1 ppm Gas Phase Individual Carbon Dioxide < 0.1 ppm Gas Phase Individual Total of all impurities < 1 ppm Gas Phase Individual PurityPlus 5.5 Oxygen < 1 ppm Gas Phase 1/batch Nitrogen < 4 ppm Gas Phase 1/batch Moisture < 1 ppm Gas Phase 1/batch Total Hydrocarbons < 0.5 ppm Gas Phase 1/batch PurityPlus 5.0 Oxygen < 2 ppm Gas Phase 1/batch Moisture < 2 ppm Gas Phase 1/batch Total Hydrocarbons < 0.5 ppm Gas Phase 1/batch PurityPlus N2 Free 5.0 Oxygen < 2 ppm Gas Phase 1/batch Moisture < 2 ppm Gas Phase 1/batch Nitrogen < 6 ppm Gas Phase 1/batch Total Hydrocarbons < 0.5 ppm Gas Phase 1/batch PurityPlus Zero 4.8 Total Hydrocarbons < 0.5 ppm Gas Phase 1/batch PurityPlus 4.7 6000 psi Oxygen < 5 ppm Gas Phase 1/batch Moisture < 5 ppm Gas Phase 1/batch PurityPlus 4.7 Oxygen < 5 ppm Gas Phase 1/batch Moisture < 5 ppm Gas Phase 1/batch Hydrogen PurityPlus 5.0 Oxygen < 1 ppm Gas Phase 1/batch Moisture < 3 ppm Gas Phase 1/batch Nitrogen < 5 ppm Gas Phase 1/batch Total Hydrocarbons < 1 ppm Gas Phase 1/batch PurityPlus Zero 4.5 Total Hydrocarbons < 0.5 ppm Gas Phase 1/batch PurityPlus 4.0 Oxygen < 20 ppm Gas Phase 1/batch Moisture < 10 ppm Gas Phase 1/batch PurityPlus 4.8 6000 psi Oxygen < 5 ppm Gas Phase 1/batch Moisture < 3 ppm Gas Phase 1/batch

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Nitrogen Purity Plus 6.0 Oxygen < 0.15 ppm Gas Phase Individual Moisture < 0.15 ppm Gas Phase Individual THC 0.10 ppm Gas Phase Individual CO / CO2 0.10 ppm Gas Phase Individual PurityPlus 5.0 Oxygen < 2 ppm Gas Phase 1/batch Moisture < 3 ppm Gas Phase 1/batch Total Hydrocarbons < 0.5 ppm Gas Phase 1/batch PurityPlus 4.8 Oxygen < 5 ppm Gas Phase 1/batch Moisture < 5 ppm Gas Phase 1/batch PurityPlus Zero 4.8 Total Hydrocarbons < 0.5 ppm Gas Phase 1/batch PurityPlus O2 Free 4.8 Oxygen < 0.5 ppm Gas Phase 1/batch PurityPlus 4.8 6000 psi Oxygen < 5 ppm Gas Phase 1/batch Moisture < 5 ppm Gas Phase 1/batch PurityPlus 4.8 3500 psi Oxygen < 5 ppm Gas Phase 1/batch Moisture < 5 ppm Gas Phase 1/batch PurityPlus 4.5 Oxygen < 0.5 ppm Gas Phase 1/batch Moisture < 1 ppm Gas Phase 1/batch Total Hydrocarbons < 0.1 ppm Gas Phase 1/batch CO + CO2 < 2 ppm Gas Phase 1/batch Hydrogen < 1 ppm Gas Phase 1/batch

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Nitrous Oxide

PurityPlus VLSI Nitrogen < 5 ppm Liquid Phase 1/batch

Oxygen < 2 ppm Liquid Phase 1/batch

Carbon Dioxide < 2 ppm Liquid Phase 1/batch

Total Hydrocarbons < 1 ppm Liquid Phase 1/batch

Moisture < 3 ppm Liquid Phase 1/batch

Carbon Monoxide < 1 ppm Liquid Phase 1/batch

Ammonia < 5 ppm Liquid Phase 1/batch

Nitric Oxide < 0.5 ppm Liquid Phase 1/batch

Nitrogen Dioxide < 0.5 ppm Liquid Phase 1/batch

Halogens < 0.5 ppm Liquid Phase 1/batch

Purity Plus 4.5 Oxygen < 5 ppm Gas Phase 1/batch Moisture < 5 ppm Gas Phase 1/batch Nitrogen < 20 ppm Gas Phase 1/batch THC < 5 ppm Gas Phase 1/batch CO / CO2 < 5 ppm Gas Phase 1/batch

PurityPlus 3.0 Nitrogen < 400 ppm Gas Phase 1/batch Oxygen < 100 ppm Gas Phase 1/batch Carbon Dioxide < 250 ppm Gas Phase 1/batch Total Hydrocarbons < 30 ppm Gas Phase 1/batch Moisture < 50 ppm Gas Phase 1/batch Carbon Monoxide < 50 ppm Gas Phase 1/batch PurityPlus AA 2.6 Moisture < 30 ppm Gas Phase 1/batch Oxygen + N2 < 2000 ppm Gas Phase 1/batch Oxygen Purity Plus 5.0 Argon < 5 ppm Gas Phase 1/batch Moisture < 2 ppm Gas Phase 1/batch Nitrogen < 5 ppm Gas Phase 1/batch THC < 1 ppm Gas Phase 1/batch CO / CO2 < 1 ppm Gas Phase 1/batch PurityPlus 4.3 Moisture < 3 ppm Gas Phase 1/batch Total Hydrocarbons < 0.5 ppm Gas Phase 1/batch Nitrogen < 10 ppm Gas Phase 1/batch Argon < 40 ppm Gas Phase 1/batch PurityPlus Zero 2.8 Total Hydrocarbons < 0.5 ppm Gas Phase 1/batch PurityPlus Extra Dry 2.6 Moisture < 10 ppm Gas Phase 1/batch

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Other Gases Ammonia PurityPlus VLSI Oil < 0.5 ppm Gas Phase 1/batch Moisture < 3 ppm Gas Phase 1/batch PurityPlus 2.5 Ammonia > 99.5% Gas Phase 1/batch Total of all impurities < 0.5% Gas Phase 1/batch 1,3 Butadiene

PurityPlus 2.0 >99.0 Liquid Phase

(Chemically Pure) Total of all impurities < 1% Liquid Phase 1/batch

1-Butene PurityPlus 2.0 Total of all impurities < 1% Gas Phase 1/batch (Chemically Pure) PurityPlus 3.0 Total of all impurities < 1000ppm Gas Phase 1/batch (Research) CIS-2-Butene

PurityPlus 2.0 Total of all impurities < 1% Liquid Phase 1/batch

(Chemically Pure)

PurityPlus 1.5 Total of all impurities 5% Liquid Phase 1/batch

Boron Trichloride PurityPlus 5.0 Total of all impurities 10 ppm Gas Phase 1/batch (Research) PurityPlus 3.0 Total of all impurities < 1000ppm Gas Phase 1/batch (Electronic) PurityPlus 2.5 Total of all impurities < 0.5% Gas Phase 1/batch (Chemically Pure) Boron Trifluoride PurityPlus 2.5 Total of all impurities < 0.5% Gas Phase 1/batch (Chemically Pure) Carbon Monoxide PurityPlus 4.0 Nitrogen < 10 ppm Gas Phase 1/batch Oxygen < 2 ppm Gas Phase 1/batch Carbon Dioxide < 20 ppm Gas Phase 1/batch Hydrogen < 10 ppm Gas Phase 1/batch Total Hydrocarbons < 5 ppm Gas Phase 1/batch Moisture < 5 ppm Gas Phase 1/batch PurityPlus 2.5 Carbon Monoxide > 99.5% Gas Phase 1/batch total of all impurities < 0.5% Gas Phase 1/batch Carbonyl Sulfide PurityPlus 3.0 Oxygen < 0.01% Gas Phase 1/batch Nitrogen < 0.03% Gas Phase 1/batch Moisture < 0.01% Gas Phase 1/batch Carbon Dioxide < 0.03% Gas Phase 1/batch Hydrogen Sulfide < 0.01% Gas Phase 1/batch

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Chlorine

PurityPlus 3.0 Chlorine > 99.9% Liquid Phase 1/batch

PurityPlus 2.5 Chlorine > 99.5% Liquid Phase 1/batch

Deuterium PurityPlus 5.0 Hydrogen < 100 ppm Gas Phase 1/batch Oxygen < 1 ppm Gas Phase 1/batch Nitrogen < 1 ppm Gas Phase 1/batch Moisture < 1 ppm Gas Phase 1/batch Deuterium Hydride < 3000 ppm Gas Phase 1/batch Total Hydrocarbons < 1 ppm Gas Phase 1/batch Carbon Monoxide < 1 ppm Gas Phase 1/batch Carbon Dioxide < 1 ppm Gas Phase 1/batch PurityPlus 4.0 Deuterium > 99.99% Gas Phase 1/batch total of all impurities < 0.01% Gas Phase 1/batch PurityPlus 2.7 Deuterium > 99.7% Gas Phase 1/batch total of all impurities < 0.3% Gas Phase 1/batch

Dinitrogen Tetroxide (Nitrogen Dioxide) PurityPlus 2.5 Moisture < 0.15% Gas Phase 1/batch Particle (Metal Residue) < 10 mg/L Gas Phase 1/batch Dimethyl Ether (DME) PurityPlus 2.8 Other Volatiles Misc 0.2wt% Gas Phase 1/batch (Chemically Pure) Sulfur Compounds Misc 500 ppmw Gas Phase 1/batch Moisture Misc 100 ppmw Gas Phase 1/batch Non-Volatile Residue Misc 50g/100ml Gas Phase 1/batch PurityPlus 2.5 Total of all impurities < 0.5% Gas Phase 1/batch Ethane PurityPlus 2.0 Ethane > 99.0% Gas Phase 1/batch total of all impurities < 1.0% Gas Phase 1/batch Ethylene PurityPlus 4.0 Ethane < 100 ppm Gas Phase 1/batch Total Impurities < 100 ppm Gas Phase 1/batch PurityPlus 3.0 Ethane < 0.1% Gas Phase 1/batch Total Impurities < 0.1% Gas Phase 1/batch PurityPlus 2.5 Ethane < 0.5% Gas Phase 1/batch Total Impurities < 0.5% Gas Phase 1/batch Hexafluoropropylene PurityPlus 3.0 Saturated Hydrocarbons < 0.2 ppm Gas Phase 1/batch Unsaturated Hydrocarbons < 0.3 ppm Gas Phase 1/batch Oxygen < 50 ppm Gas Phase 1/batch Acidity < 0.0001% Gas Phase 1/batch Hydrogen Bromide PurityPlus 2.8 Total of all impurities < 2000 ppm Gas Phase 1/batch (Chemically Pure)

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Hydrogen Chloride

PurityPlus 5.0 Nitrogen Liquid Phase 1/batch

Oxygen Liquid Phase 1/batch

CO + CO2 Liquid Phase 1/batch

Total Hydrocarbons Liquid Phase 1/batch

PurityPlus 4.5 Nitrogen Liquid Phase 1/batch

Oxygen Liquid Phase 1/batch

CO + CO2 Liquid Phase 1/batch

Total Hydrocarbons Liquid Phase 1/batch

PurityPlus 4.0 Hydrogen Chloride > 99.99% Liquid Phase 1/batch

PurityPlus 2.0 Hydrogen Chloride > 99.0% Gas Phase 1/batch

Hydrogen Sulfide

PurityPlus 2.5 Hydrogen Sulfide > 99.5% Liquid Phase 1/batch

Isobutane

PurityPlus 2.5 Isobutane > 99.5% Liquid Phase 1/batch

PurityPlus 2.0 Isobutane > 99.0% Liquid Phase 1/batch

Krypton PurityPlus 5.0 Nitrogen Gas Phase 1/batch Oxygen Gas Phase 1/batch Hydrogen Gas Phase 1/batch CO + CO2 Gas Phase 1/batch Tetrafluoromethane Gas Phase 1/batch Total Hydrocarbons Gas Phase 1/batch Moisture Gas Phase 1/batch Xenon Gas Phase 1/batch PurityPlus 4.5 Xenon < 20 ppm Gas Phase 1/batch Nitrogen < 10 ppm Gas Phase 1/batch Oxygen < 2 ppm Gas Phase 1/batch Hydrogen < 1 ppm Gas Phase 1/batch CO + CO2 < 1 ppm Gas Phase 1/batch Tetrafluoromethane < 1 ppm Gas Phase 1/batch Total Hydrocarbons < 1 ppm Gas Phase 1/batch Moisture < 1 ppm Gas Phase 1/batch PurityPlus 2.0 Krypton > 99% Gas Phase 1/batch total of all impurities < 1% Gas Phase 1/batch

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Methane PurityPlus 5.0 Methane > 99.999% Gas Phase 1/batch total of all impurities < 0.001% Gas Phase 1/batch PurityPlus 4.0 Methane > 99.99% Gas Phase 1/batch total of all impurities < 0.001% Gas Phase 1/batch PurityPlus 2.0 Methane > 99.0% Gas Phase 1/batch total of all impurities < 1.0% Gas Phase 1/batch PurityPlus 1.3 (Natural Gas) Methane > 93.0% Gas Phase 1/batch Methyl Chloride PurityPlus 2.5 Total of all impurities < 0.5% Gas Phase 1/batch (Chemically Pure) Methyl Fluoride PurityPlus 2.0 Total of all impurities < 1% Gas Phase 1/batch (Chemically Pure)

Methyl Mercaptan PurityPlus 2.5 Total of all impurities < 0.5% Gas Phase 1/batch (Chemically Pure) Monomethylamine (MMA) PurityPlus 2.5 Total of all impurities < 0.5% Gas Phase 1/batch (Chemically Pure) Neon PurityPlus 5.0 Helium < 8 ppm Gas Phase 1/batch Nitrogen < 4 ppm Gas Phase 1/batch Oxygen < 1 ppm Gas Phase 1/batch Moisture < 1 ppm Gas Phase 1/batch Hydrogen < 1 ppm Gas Phase 1/batch Total Hydrocarbons < 0.5 ppm Gas Phase 1/batch Neopentane (Dimethylpropane) PurityPlus 2.0 Total of all impurities < 1% Gas Phase 1/batch (Chemically Pure) n-Butane PurityPlus 2.5 Total of all impurities < 0.1% Gas Phase 1/batch (Instrument) PurityPlus 2.0 Total of all impurities < 1% Gas Phase 1/batch (Chemically Pure) Nitric Oxide PurityPlus 3.0 Nitric Oxide > 99.9% Gas Phase 1/batch total of all impurities < 0.1% Gas Phase 1/batch PurityPlus 2.0 Nitric Oxide > 99.0% Gas Phase 1/batch total of all impurities < 1.0% Gas Phase 1/batch

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Nitrogen Trifluoride PurityPlus 4.0 Oxygen / Argon < 5 ppm Gas Phase 1/batch Nitrogen < 5 ppm Gas Phase 1/batch Tetrafluoromethane < 40 ppm Gas Phase 1/batch Carbon Dioxide < 3 ppm Gas Phase 1/batch Nitrous Oxide < 3 ppm Gas Phase 1/batch Sulfur Hexafluoride < 5 ppm Gas Phase 1/batch Moisture < 1 ppm Gas Phase 1/batch Hydrogen Fluoride < 1 ppm Gas Phase 1/batch Carbon Monoxide < 1 ppm Gas Phase 1/batch Methane < 1 ppm Gas Phase 1/batch Octafluoropropane (HC-218) PurityPlus 5.0 Organic Impurities < 10 ppm Gas Phase 1/batch Moisture Gas Phase 1/batch Carbon Monoxide Gas Phase 1/batch Carbon Dioxide Gas Phase 1/batch Nitrogen + Oxygen Gas Phase 1/batch Acidity (as HF) Gas Phase 1/batch PurityPlus 3.0 Octafluoropropane > 99.9% Gas Phase 1/batch total of all impurities < 0.1% Gas Phase 1/batch

Propane PurityPlus 3.0 Total of all impurities < 1000 ppm Gas Phase 1/batch (Research) PurityPlus 2.5 Total of all impurities < 0.5% Gas Phase 1/batch (Instrument) PurityPlus 2.0 Total of all impurities < 1.0% Gas Phase 1/batch (CP) Propylene PurityPlus 2.5 Total of all impurities < 0.5% Gas Phase 1/batch (Polymer) PurityPlus 2.0 Total of all impurities < 1.0% Gas Phase 1/batch Sulfur Dioxide PurityPlus 3.8 Moisture < 20ppm Gas Phase 1/batch (Anhydrous) Residue < 50ppm Gas Phase 1/batch Sulfuric Acid < 20 ppm Gas Phase 1/batch

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Sulfur Hexafluoride PurityPlus 5.0 Air < 6 ppm Gas Phase 1/batch Tetrafluoromethane < 2 ppm Gas Phase 1/batch Moisture < 2 ppm Gas Phase 1/batch PurityPlus 4.0 Air < 50 ppm Gas Phase 1/batch Tetrafluoromethane < 40 ppm Gas Phase 1/batch Moisture < 5 ppm Gas Phase 1/batch Oil < 2 ppm Gas Phase 1/batch Acidity (as HF) < 0.3 ppm Gas Phase 1/batch PurityPlus 3.0 Air < 300 ppm Gas Phase 1/batch Tetrafluoromethane < 300 ppm Gas Phase 1/batch Moisture < 8 ppm Gas Phase 1/batch Oil < 5 ppm Gas Phase 1/batch Acidity (as HF) < 0.3 ppm Gas Phase 1/batch Tetrafluoromethane (HC-14) PurityPlus 5.0 Oxygen + Argon < 1 ppm Gas Phase 1/batch Nitrogen < 4 ppm Gas Phase 1/batch CO + CO2 < 1 ppm Gas Phase 1/batch Other Halocarbons < 2 ppm Gas Phase 1/batch Sulfur Hexafluoride < 1 ppm Gas Phase 1/batch Moisture < 1 ppm Gas Phase 1/batch Acidity (as HF) < 0.1 ppmw Gas Phase 1/batch PurityPlus 4.0 Oxygen + Argon < 5 ppm Gas Phase 1/batch Nitrogen < 20 ppm Gas Phase 1/batch CO + CO2 < 10 ppm Gas Phase 1/batch Other Halocarbons < 5 ppm Gas Phase 1/batch Sulfur Hexafluoride < 5 ppm Gas Phase 1/batch Moisture < 3 ppm Gas Phase 1/batch Acidity (as HF) < 0.01 ppmw Gas Phase 1/batch

Trimethylamine (TMA) PurityPlus 2.5 Total of all impurities < 0.5% Gas Phase 1/batch (Chemically Pure) Xenon PurityPlus 5.0 Krypton Gas Phase 1/batch Moisture Gas Phase 1/batch Hydrogen Gas Phase 1/batch Oxygen Gas Phase 1/batch Nitrogen Gas Phase 1/batch Nitrous Oxide Gas Phase 1/batch Total Hydrocarbons Gas Phase 1/batch Tetrafluoromethane Gas Phase 1/batch Carbon Dioxide Gas Phase 1/batch Hexafluoroethane Gas Phase 1/batch Total impurities 10 ppm Gas Phase 1/batch

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 3 Equipment Specifications/LWIs

This section contains the specifications for PurityPlus Specialty Gas fill and analytical equipment. Each authorized PurityPlus location will have some of this equipment and additional equipment. The LWIs for equipment not mentioned in this section should be taken from the manufacturer’s instructions.

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 3.1 Vacuum and Billing Gauges

5. OBJECTIVE To establish the procedures and specifications for gauges when product is filled by Pressure and

Temperature method 6. SCOPE This procedure applies to the PurityPlus specialty gases lab. 7. RESPONSIBILITIES It is the responsibility of all laboratory personnel to ensure that this procedure is performed as described,

that this procedure is reviewed and updated as necessary, and that proper support documentation is maintained.

8. PROCEDURE 8.1. Vacuum And Billing Gauge Specifications Description: Analog - 6” 270 deg. Arc, 1.0% or 0.5% accuracy, cleaned and tagged for oxygen service. Certificate of

calibration required at purchase. Digital - 1.0% or 0.5% accuracy, cleaned and tagged for oxygen service. Certificate of calibration required

at purchase. Range : 0-3000 psig - 20 psig sub-divisions 0-4000 psig - 50 psig sub-divisions 0-5000 psig - 50 psig sub-divisions 0-6000 psig - 50 psig sub-divisions Vacuum –30 in Hg to 30 psi – 1 in Hg/1psig sub-divisions 8.2. Vacuum And Billing Gauge Calibration: Frequency: Annual Standard By: Master gauge or dead weight tester Accuracy: +/- 1.0% of full scale range. 8.3. Master Gauge Specifications Description: Analog - 6” 270 deg. Arc, 0.5% accuracy, cleaned and tagged for oxygen service. Certificate of calibration

required at purchase. Digital - 0.5% accuracy, cleaned and tagged for oxygen service. Certificate of calibration required at

purchase. Range : 0-3000 psig - 20 psig sub-divisions 0-4000 psig - 50 psig sub-divisions 0-5000 psig - 50 psig sub-divisions 0-6000 psig - 50 psig sub-divisions Vacuum –30 in Hg to 30 psi – 1 in Hg/1psig sub-divisions

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8.4. Master Gauge Calibration: Frequency: Every two years Standard Outside service contractor and/or dead weight tester Accuracy +/- 0.5% of full scale range 8.5. CALIBRATION OF PRESSURE GAUGES: NOTE: All billing gauges receive a five-point calibration

8.5.1. Mount billing gauge to manifold test stand or mount the master gauge to the fill manifold. 8.5.2. Note needle position at zero pressure. 8.5.3. Adjust zero mark on gauge if necessary. 8.5.4. For dead weight testers - Bleed any trapped air from system. 8.5.5. Pressurize the gauge to 20% of full scale and compare the reading to the Master Gauge. 8.5.6. Pressurize the gauge to 40% of full scale and compare the reading to the Master Gauge. 8.5.7. Pressurize the gauge to 60% of full scale and compare the reading to the Master Gauge. 8.5.8. Pressurize the gauge to 80% of full scale and compare the reading to the Master Gauge. 8.5.9. Pressurize the gauge to 100% of full scale and compare the reading to the Master Gauge. 8.5.10. NOTE: If gauge is found to be out of specification, repeat the calibration procedure to confirm the

reading was accurate. 8.5.11. The results are then recorded on the gauge calibration form and placed into the calibration file. 8.5.12. The calibration sticker is then applied to the face of the calibrated gauge. 8.5.13. If the gauge was filled with liquid, the gauge is then evacuated for at least two hours to remove

any traces of moisture. Note: the pressure media must be compatible with Oxygen. NOTE: if any gauge doses not fall within the allowable tolerances it will be removed from service and

repaired and recalibrated before being placed in service. 8.6. CALIBRATION OF VACUUM GAUGES: Frequency: Annual Standard By Master Gauge Accuracy +- 0.5psi. 8.7. CALIBRATION OF MASTER GAUGE: Frequency: Every two years Standard Outside service contractor and / or dead weight tester Accuracy +- 1% of full scale reading 8.8. MASTER VACUUM GAUGE SPECIFICATION: Same as above 8.9. CALIBRATION OF VACUUM GAUGE: NOTE: Before starting gauge calibration, record the gauge ID on the Vacuum gauge calibration form.

8.9.1. Mount vacuum gauge to master gauge manifold test stand/fill manifold. 8.9.2. Make note of the zero mark at atmosphere. 8.9.3. Draw vacuum down as low as it will go. 8.9.4. Close valve from vacuum pump to test manifold. 8.9.5. Make note of the gauge reading and record results on vacuum calibration log. 8.9.6. Slowly open the bleed valve to break vacuum. 8.9.7. Stop vacuum release at two set points before releasing to zero. 8.9.8. Record results of both set points comparing readings to the master gauge. 8.9.9. Break vacuum and allow gauge to return to zero point. 8.9.10. Make note if gauge returns to zero mark and record results. 8.9.11. Record final results on the vacuum gauge calibration form and place it on file. 8.9.12. Place calibration sticker onto the face of the gauge. 8.9.13. If gauge is not to be placed into immediate service, place gauge into a plastic bag or cap plug the

inlet before placing into storage.

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 3.2 Thermometers

1. OBJECTIVE To establish the procedures and specifications for thermometers when product is filled by Pressure and

Temperature method 2. SCOPE This procedure applies to the PurityPlus specialty gases lab. 3. RESPONSIBILITIES It is the responsibility of all laboratory personnel to ensure that this procedure is performed as described,

that this procedure is reviewed and updated as necessary, and that proper support documentation is maintained.

4. PROCEDURE 4.1. Thermometer Specifications

Description: Hand held thermometer gun or dial thermometer Range: at least 0 to + 150 degrees Fahrenheit.

4.2. Calibration

Frequency Annual Standard Certified Calibrated thermometer Accuracy +- 2 deg. F.

4.3. Calibration of certified thermometer: Frequency Every two years Standard NIST traceable Accuracy +/- 1 deg. F.

4.4. Certified thermometer specifications: Same as above

4.5. Annual Calibration Check And Field Calibration Every 12 months all thermometers used in the filling process are to be checked at three points of their scale and the results recorded on the thermometer calibration record form. Affixing the certified thermometer to a small cylinder does this. Place the cylinder and the certified thermometer into a cold environment. (i.e., refrigerator, freezer, etc.) Let the cylinder with the certified thermometer sit in this environment for a sufficient amount of time until the temperature has stabilized. Remove the cylinder and the certified thermometer from its environment and take a temperature reading of both the certified and the working thermometers. Record the results on the Thermometer Calibration Form. To do a calibration check on the high end, take your cylinder with the certified thermometer and place it in the warmest environment possible. (i.e., boiler room, etc.) Allow the cylinder and the certified thermometer to sit for a sufficient amount of time to stabilize in temperature. After this time, take a temperature reading of both the certified and working thermometers and record your readings on the Thermometer Calibration Form. To perform a normal or medium temperature check, allow the cylinder with the master thermometer to sit at room temperature for a sufficient amount of time. Once the temperature is stabilized, check your working thermometer against the master thermometer. Record your results on the Thermometer Calibration Form.

The thermometer being calibrated should be within +/- 2 degrees tolerance on all ends of the scale. If the thermometer passes and is within the allowable tolerance, record it on the calibration record. Apply a

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calibration sticker or tag and return it to service. If the thermometer does not fall within the tolerance of +/- 2 degrees, tag the thermometer and remove it from service. Record this on the calibration record and send the thermometer to an authorized source to have it repaired.

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 3.3 Cylinder Specifications

Style DOT Spec. Material Water Volume Tare OD Height

Liters Cu In CF 7 3E 1800 Steel 0.424755 25.92 0.015 4 2 14.25 EB/LB/RB 3E 1800 Steel 0.424755 25.92 0.015 4 2 14.25 C 3AA 1800 Steel 0.906144 55.296 0.032 4 3.5 12.25 3 3AA 2015 Steel 2.888334 176.256 0.102 10 4.25 20.75 D 3AA 2015 Steel 2.888334 176.256 0.102 10 4.25 20.75 10 3AA 2015 Steel 2.888334 176.256 0.102 10 4.25 20.75 F 3AA 2015 Steel 2.888334 176.256 0.102 10 4.25 20.75 MD 3AA 2015 Steel 2.944968 179.712 0.104 9.5 4.25 16.75 R 3A 2015 Steel 3.624576 221.184 0.128 0 5.5 14 005 3AA 2015 Steel 4.785573 292.032 0.169 13.5 4.25 26 ME 3AA 2015 Steel 4.785573 292.032 0.169 13.5 4.25 26 ER 3AA 2015 Steel 4.785573 292.032 0.169 13.5 4.25 26 A07 3AL 2216 Aluminum 5.94657 362.88 0.21 15 7 19.75 2(AL) 3AL 2216 Aluminum 5.94657 362.88 0.21 15 7 19.75 D-1(AL) 3AL 2216 Aluminum 5.94657 362.88 0.21 15 7 19.75 30A 3AL 2216 Aluminum 5.94657 362.88 0.21 15 7 19.75 32.1S 3AL 2216 Aluminum 5.94657 362.88 0.21 15 7 19.75 A3 3AL 2216 Aluminum 5.94657 362.88 0.21 15 7 19.75 3R 3AL 2216 Aluminum 5.94657 362.88 0.21 15 7 19.75 30AL 3AL 2216 Aluminum 5.94657 362.88 0.21 15 7 19.75 AG 3AL 2216 Aluminum 5.94657 362.88 0.21 15 7 19.75 CL 3AL 2216 Aluminum 5.94657 362.88 0.21 15 7 19.75 7 3AA 2015 Steel 7.07925 432 0.25 29 6 24 D-1 3AA 2015 Steel 7.07925 432 0.25 29 6 24 35 3AA 2015 Steel 7.07925 432 0.25 29 6 24 30.3 3AA 2015 Steel 7.07925 432 0.25 29 6 24 G3 3AA 2015 Steel 7.07925 432 0.25 29 6 24 3 3AA 2015 Steel 7.07925 432 0.25 29 6 24 35 3AA 2015 Steel 7.07925 432 0.25 29 6 24 G/UG 3AA 2015 Steel 7.07925 432 0.25 29 6 24 C 4BA 240 Steel 10.47729 639.36 0.37 20 9 19 FE 4BA 240 Steel 10.47729 639.36 0.37 20 9 19 16 3A 2215 Steel 14.72484 898.5599 0.52 65 7 35 C 3A 2215 Steel 14.72484 898.5599 0.52 65 7 35 80 3A 2215 Steel 14.72484 898.5599 0.52 65 7 35 F 3A 2215 Steel 14.72484 898.5599 0.52 65 7 35 2 3A 2215 Steel 14.72484 898.5599 0.52 65 7 35 Q/UQ 3A 2215 Steel 14.72484 898.5599 0.52 65 7 35 B 3A 2215 Steel 14.72484 898.5599 0.52 65 7 35

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Style DOT Spec. Material Water Volume Tare OD Height Liters Cu In CF

A16 3AL 2216 Aluminum 15.57435 950.4 0.55 30 7.25 37 22(AL) 3AL 2216 Aluminum 15.57435 950.4 0.55 30 7.25 37 C(AL) 3AL 2216 Aluminum 15.57435 950.4 0.55 30 7.25 37 80A 3AL 2216 Aluminum 15.57435 950.4 0.55 30 7.25 37 82.1S 3AL 2216 Aluminum 15.57435 950.4 0.55 30 7.25 37 A2 3AL 2216 Aluminum 15.57435 950.4 0.55 30 7.25 37 2R 3AL 2216 Aluminum 15.57435 950.4 0.55 30 7.25 37 80AL 3AL 2216 Aluminum 15.57435 950.4 0.55 30 7.25 37 AQ 3AL 2216 Aluminum 15.57435 950.4 0.55 30 7.25 37 BL 3AL 2216 Aluminum 15.57435 950.4 0.55 30 7.25 37 DEY 3A 2015 Steel 21.6625 1321.92 0.765 80 7 43 S 3AA 2015 Steel 26.90115 1641.6 0.95 80 7.4 46 A31 3AL 2015 Aluminum 29.44968 1797.12 1.04 48 8 52 30(AL) 3AL 2015 Aluminum 29.44968 1797.12 1.04 48 8 52 B(AL) 3AL 2015 Aluminum 29.44968 1797.12 1.04 48 8 52 130A 3AL 2015 Aluminum 29.44968 1797.12 1.04 48 8 52 152.1S 3AL 2015 Aluminum 29.44968 1797.12 1.04 48 8 52 AH 3AL 2015 Aluminum 29.44968 1797.12 1.04 48 8 52 1R 3AL 2015 Aluminum 29.44968 1797.12 1.04 48 8 52 AS 3AL 2015 Aluminum 29.44968 1797.12 1.04 48 8 52 485 3AA 6000 Steel 42.4755 2592 1.5 303 10 55 44HH 3AA 6000 Steel 42.4755 2592 1.5 303 10 55 BX 3AA 6000 Steel 42.4755 2592 1.5 303 10 55 3HP 3AA 6000 Steel 42.4755 2592 1.5 303 10 55 500 3AA 6000 Steel 42.4755 2592 1.5 303 10 55 H2 3AA 6000 Steel 42.4755 2592 1.5 303 10 55 1U 3AA 6000 Steel 42.4755 2592 1.5 303 10 55 3HP 3AA 6000 Steel 42.4755 2592 1.5 303 10 55 6K 3AA 6000 Steel 42.4755 2592 1.5 303 10 55 44 3A 2015 Steel 43.60818 2661.12 1.54 110 9 55 44H 3AA 3600 Steel 43.60818 2661.12 1.54 189 10 55 B 3A 2015 Steel 43.60818 2661.12 1.54 110 9 55 200 3A 2015 Steel 43.60818 2661.12 1.54 110 9 55 H 3A 2015 Steel 43.60818 2661.12 1.54 110 9 55 H1 3AA 3600 Steel 43.60818 2661.12 1.54 189 10 55 1A 3A 2015 Steel 43.60818 2661.12 1.54 110 9 55 K/UK 3A 2015 Steel 43.60818 2661.12 1.54 110 9 55 3K 3AA 3600 Steel 43.60818 2661.12 1.54 189 10 55 A 3A 2015 Steel 43.60818 2661.12 1.54 110 9 55 AT 3AL 2216 Aluminum 48.1389 2937.6 1.7 95 10 58 49 3AA 2400 Steel 48.98841 2989.44 1.73 143 9.25 59 A 3AA 2400 Steel 48.98841 2989.44 1.73 143 9.25 59 J 3AA 2400 Steel 48.98841 2989.44 1.73 143 9.25 59 1L 3AA 2400 Steel 48.98841 2989.44 1.73 143 9.25 59 300 3AA 2400 Steel 48.98841 2989.44 1.73 143 9.25 59 T/UT 3AA 2400 Steel 48.98841 2989.44 1.73 143 9.25 59 K 3AA 2400 Steel 48.98841 2989.44 1.73 143 9.25 59 55 4BA 300 Steel 55.78449 3404.16 1.97 55 10 52 A-3 4BA 300 Steel 55.78449 3404.16 1.97 55 10 52

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Style DOT Spec. Material Water Volume Tare OD Height Liters Cu In CF

65 4BA 300 Steel 55.78449 3404.16 1.97 55 10 52 410 4BA 300 Steel 55.78449 3404.16 1.97 55 10 52 SC 4BA 300 Steel 55.78449 3404.16 1.97 55 10 52 1J 4BA 300 Steel 55.78449 3404.16 1.97 55 10 52 65 4BA 300 Steel 55.78449 3404.16 1.97 55 10 52 FC 4BA 300 Steel 55.78449 3404.16 1.97 55 10 52 XP 4BA 300 Steel 55.78449 3404.16 1.97 55 10 52 350 4BA 240 Steel 108.4541 6618.24 3.83 75 15 49 A-1 4BA 240 Steel 108.4541 6618.24 3.83 75 15 49 425 4BA 240 Steel 108.4541 6618.24 3.83 75 15 49 110 4BA 240 Steel 108.4541 6618.24 3.83 75 15 49 1F 4BA 240 Steel 108.4541 6618.24 3.83 75 15 49 XL 4BA 240 Steel 108.4541 6618.24 3.83 75 15 49 FX 4BA 240 Steel 108.4541 6618.24 3.83 75 15 49 PX 4BW 300 Steel 108.4541 6618.24 3.83 85 14.5 49 AA 4AA 480 Steel 126.0106 7689.6 4.45 150 15 56 AC 4AA 480 Steel 126.0106 7689.6 4.45 150 15 56 150 4AA 480 Steel 126.0106 7689.6 4.45 150 15 56 FA 4AA 480 Steel 126.0106 7689.6 4.45 150 15 56 XG 4AA 480 Steel 126.0106 7689.6 4.45 150 15 56 A5 4BW 240 Steel 454.4878 27734.4 16.05 315 29.75 55 HT 4BW 240 Steel 454.4878 27734.4 16.05 315 29.75 55 T 110

A 500 Steel 761.7273 46483.2 26.9 1115 30 82

FT 110A

500 Steel 761.7273 46483.2 26.9 1115 30 82

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Quality Assurance Program Rev. 26 May 2009 Rev #: 3 Document Title: 3.4 Cylinder Paint Application Guide

1. OBJECTIVE To establish the procedures and specifications for applying the PurityPlus Green paint. 2. SCOPE This procedure applies to the PurityPlus specialty gases plant and lab. 3. RESPONSIBILITIES It is the responsibility of all plant and laboratory personnel to ensure that this procedure is performed as

described, that this procedure is reviewed and updated as necessary. 4. PROCEDURE 4.1. Product type: Part number: Cyl-Tec PurityPlus Green Paint. This is a low VOC water reducible acrylic enamel

paint. Since it is a coating system containing water the full cure time will vary depending on the humidity, temperature, and the thickness of the coating applied. If faster dry time is needed, contact Cyl-Tec for PurityPlus green solvent based fast dry paint. Customer service toll free; 1 (888) 429-5832.

4.2. Typical cure schedule:

Dry to touch: 15 - 20 minutes (50% relative humidity, 70o F) Dry to recoat: 1 1/2 hours (50% relative humidity, 70o F) Dry to handle: 2 - 4 hours (50% relative humidity, 70o F) Full cure: 36 - 48 hours

4.3. Surface preparation: The cylinder surface should be clean, free from dirt and oil. This coating is designed to be

applied direct to bare shot blasted cylinders or compatible Acrylex brand primer painted cylinders. Painting over other finish coatings is possible, but should be tested on a cylinder first, as incompatibility between other coating systems may cause adhesion or durability problems.

4.4. Primer: Primer is not necessary. But, if you prefer using a primer, we recommend using Acrylex brand

(direct to metal) water reducible primer. 4.5. Acceptable application methods: Always mix the paint thoroughly before starting to coat cylinders. PurityPlus green is an

encapsulated hi sparkle metal flake coating system, and it will look best when the paint is thoroughly mixed.

4.5.1. Spray:

Conventional or HVLP spray equipment is recommended. Apply the 1st coat to the cylinder. A 1 mil thick 1st coat is recommended. Allow a minimum of 1 hour dry time, and apply second 1 mil coat. Check above cure schedule for typical full cure time.

4.5.2. Pipe roller: A segmented pipe roller is recommended for roll application. Do not use a conventional

straight roller or brush. Pre-condition the roller in the tray by rolling it in the paint to eliminate nap. Apply one even coat to the cylinder allow a minimum of 1 ½ hour dry time, and apply the second coat. Check above cure schedule for typical full cure time.

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4.6. Coverage comments: Since PurityPlus Green is an encapsulated type metal flake coating system, the pigment and

metal flake should stay in suspension. But some separation is possible, especially when the paint is applied by brush, or by roller. To avoid this separation in non spray applications, use a segmented roller, and apply two even coats, allowing for 1 ½ hour dry time between coats.

4.7. Paint areas: Paint the cylinder sidewall and shoulder using the PurityPlus Green Paint. Paint the collars and

caps using the PurityPlus Green Paint or according to local procedures. 4.8. Safety precautions: Consult MSDS.

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 4 Cylinder Filling LWIs

This section contains the specific guidelines to assure PurityPlus Specialty Gas products meet established production specifications. Use manufacturers’ instructions for equipment not mentioned in the LWIs.

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 4.1 High Pressure Cylinder Pre-Fill Inspection

1. OBJECTIVE

This procedure establishes the procedure for high pressure cylinder pre-fill inspection.

2. SCOPE The following procedures are to be used for the appropriate pre-fill inspecting of high pressure cylinders.

3. RESPONSIBILITIES It is the responsibility of all laboratory personnel to ensure that this procedure is performed as described, that this procedure is reviewed and updated as necessary, and that proper support documentation is maintained.

4. PROCEDURE 4.1. VALVE PROTECTION CAPS If the cylinder is equipped to receive a valve protection cap, follow the following procedure:

4.1.1. Inspect cylinder caps to insure they will protect the cylinder valve. 4.1.2. Remove any caps from service that:

4.1.2.1. Do not have enough vent holes, or if vent holes are too small. 4.1.2.2. Are so badly bent, cut or dented that they are hard to get off. 4.1.2.3. Are rough or jagged and may hurt someone. 4.1.2.4. Have threads so worn that only a few will engage neck ring.

4.1.3. Paint any caps that need painting. 4.1.4. Inspect neck rings for:

4.1.4.1. Worn threads. 4.1.4.2. Loose fit on cylinder.

4.1.5. Remove cylinder from service if: 4.1.5.1. Neck ring threads are so worn that only a few will engage cap 4.1.5.2. Neck ring is loose on cylinder.

4.2. TEST DATES 4.2.1. Check the retest date on every cylinder. High pressure cylinders must be retested hydrostatically at

least every five years. The DOT permits certain cylinders to be retested every ten years if specific conditions are met. See the ten year hydrotest requirements from 49 CFR 173.34(e)(16), below:

(16) DOT-3A or 3AA cylinders. (i) A cylinder made in conformance with specification DOT-3A or 3AA with a water capacity

of 125 pounds or less that is removed from any cluster, bank, group, rack or vehicle each time it is filled, may be retested every ten years instead of every five years, provided the cylinder complies with all of the following--

The cylinder was manufactured after December 31, 1945; The cylinder is used exclusively for air, argon, cyclopropane, ethylene, helium, hydrogen, krypton, neon, nitrogen, nitrous

oxide, oxygen, sulfur hexafluoride, xenon, permitted mixtures of these gases (see Sec. 173.301(a)) and permitted mixtures of these gases with up to 30 percent by volume of carbon dioxide, provided that the gas has a dew point at or below minus 52 deg.F at 1 atmosphere;

Before each refill, the cylinder passes the hammer test specified in CGA Pamphlet C-6; The cylinder is dried immediately after hydrostatic testing to remove all traces of free water; The cylinder is not used for underwater breathing; and Each cylinder is stamped with a five-point star at least one-fourth of an inch high immediately following the test date. (ii) If, since the last required hydrostatic retest, a cylinder has not been used exclusively as specified in paragraph

(e)(16)(i)(B) of this section, but currently conforms with all other provisions of paragraph (e)(16)(i) of this section, it may be retested every 10 years instead of every five years, provided it is first retested and examined as prescribed by Sec. 173.302(c)(2), (3) and (4).

(iii) Except as specified in paragraph (e)(16)(ii) of this section, if a cylinder marked with a star is charged with a compressed gas other than as specified in this paragraph (e)(16), the star following the most recent test date must be obliterated. The cylinder must be retested five years from the marked retest date, or prior to the first charging with a compressed gas, if the required five-year retest period has passed.

4.2.2. Remove any cylinders from service if they are due for test.

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4.3. SURFACE DAMAGE 4.3.1. Inspect for surface damage as follows:

4.3.1.1. Check for dents, cuts, gouges and digs. Measure any you find. 4.3.1.2. Check for rust and pits. Measure maximum depth of any you find.

NOTE.- Remove any scale or rust before measuring depth. 4.3.1.3. Check for bulges. Measure height of any you find. 4.3.1.4. Check for arc burns and torch burns. 4.3.1.5. Check for unstable bottoms. 4.3.1.6. If damage to any high pressure cylinder meets or exceeds the limits listed below, remove

the cylinder from service. 4.3.2. Dent - Any dent on cylinder sidewall is:

4.3.2.1. Between 1/32 and 3/64 in. deep and is less than 1 in. by 1 in. (1 sq. in.) in area, or is 4.3.2.2. Between 3/64 and 1/16 in. deep and is less than 2 in. by 2 in. (4 sq. in.) in area. 4.3.2.3. Any dent, anywhere on cylinder, is deeper than 1/16 in.

4.3.3. Cut, gouge or dig - Any cut, gouge or dig on cylinder sidewall is: 4.3.3.1. Longer than 3 inches, or deeper than 1/32 in. 4.3.3.2. Any cut, gouge or dig on cylinder bottom or should is deeper than 1/16 in.

NOTE: Where cuts, gouges or digs are found in dents, the above limits still apply. 4.3.4. Rust or pits:

4.3.4.1. Rust or pits on cylinder sidewall are deeper than 1/32 in. 4.3.4.2. Rust or pits on cylinder bottom or shoulder are deeper than 1/16 in.

4.3.5. Bulge - Any bulge on cylinder is over 1/16 in. high. NOTE: Remove any bulged cylinder from service if the bulge does not appear to be a manufacturing defect.

4.3.6. Arc Burn - Cylinder has an arc burn or a torch burn, no matter how small. 4.3.7. Unstable Bottom - Cylinder has an unstable bottom and is apt to fall over.

4.4. FIRE CYLINDERS

4.4.1. Fire cylinders may or may not be incident cylinders, i.e., cylinders that were involved in incidents involving persons or property.

4.4.2. Incident cylinders may not be altered or disassembled for inspection unless they are unsafe to store in the condition received. When incident cylinders are found notify your supervisor immediately. Decal and tag cylinders. Store them in a safe, dry location until they are evaluated by management.

4.4.3. Remove any cylinder from service if there is evidence that it was involved in a fire: Soot, paint removal, paint blistering or discoloration of the metal. Aluminum cylinders may have a clear coating designed to discolor in a fire or may have other excessive heat detection properties.

4.5. CONTAMINATION

4.5.1. Remove from service immediately any cylinder with oil, grease, tar or similar organic compounds found anywhere on its surface.

4.5.2. Clean and wash the cylinder prior to filling it. No cylinder with noticeable mud or dirt may be filled until it has been washed. Mud and dirt hide defects such as arc burns.

4.5.3. If the cylinder has evidence of contamination with bodily fluids (blood, etc.), notify supervision. This cylinder must be handled and decontaminated by persons with special training in dealing with bodily fluids.

4.6. MEDICAL GAS CYLINDERS

4.6.1. Paint should be in good condition; if paint is noticeably cracked, chipped or worn off, cylinder should be repainted.

4.6.2. Neck ring and cap threads should be clean and rust-free. 4.6.3. Cylinder caps should be clean inside and out. Caps must fit properly. 4.6.4. Report all customer complaints about a medical cylinder to your supervisor. Special complaint

handling procedures must be followed for medical gases.

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4.7. VALVE INSPECTION

4.7.1. All incoming cylinders must be given a valve inspection prior to filling. Conduct this inspection prior to odor testing cylinders.

4.7.2. Check the valve for contamination. A cylinder valve is contaminated if it has any of the following substances anywhere on its surface: oil, grease, any other lubricant, any petroleum product, chemical corrosion (mercury, etc.), embrittlement or any unknown substance.

4.7.3. Cylinders with contaminated valves may require internal as well as external cleaning. 4.7.4. Inspect the valve outlet to verify that the CGA connection threads are the correct style and in good

condition. 4.7.5. If a damaged or contaminated valve is found, tag the cylinder or mark it with a paint stick and move

the cylinder to the cylinder maintenance area. 4.7.6. VALVE SAFETY DEVICES 4.7.7. Compare the service pressure markings with the marking on the safety device nut. Cylinders with

disc bursting pressures greater than those specified are in violation of DOT regulations. Discs with lower bursting pressures than those specified may fail prematurely.

4.7.8. Cylinders with working pressures of: 1800 psi should have a safety rated for 3000 psi

2000 psi should have a safety rated for 3360 psi 2200 psi should have a safety rated for 3775 psi 2400 psi should have a safety rated for 4000 psi Consult your supervisor for other cylinder working pressures

4.7.9. Cylinders With Discs Backed by Fusible Metal: Cylinders in flammable gas service must have safety discs backed with fusible metal. Sometimes

government owned cylinders in nonflammable service, i.e., O2, N2, and Ar, will be presented for filling. If they meet the other requirements of this procedure, these cylinders may be filled only to their marked service pressures. Cylinders with discs backed by fusible metal are NOT eligible for over filling to 110% of their marked service pressures. DOT regulations specify that to be eligible for filling to 110% of marked service pressure, cylinders must be equipped with a valve having a disc safety device (without a fusible metal backing).

Cylinders with liquefied gases (Carbon Dioxide, Nitrous Oxide, etc.) may not be equipped with a

safety backed by fusible metal. Carefully verify that the large cylinder valve or post type cylinder valve of liquefied gases are not equipped with a safety backed by fusible metal.

4.8. HIGH-PRESSURE CYLINDER ODOR TEST

4.8.1. Odor testing is required to prevent compressing oxidizing gases into cylinders contaminated with hydrocarbons and to assure that the products are suitable for breathing.

4.8.2. WARNING - Odor test cylinders containing only the gases listed below. Do not odor test cylinders containing any other gases. Doing so can expose you to such hazards as fire, explosion, asphyxiation, caustic burns, and poisoning. NEVER ODOR TEST cylinders containing SPECIALTY GASES other than medical gases. They may contain substances that even in very small quantities can kill or seriously injure you. Noxious substances may be components of the original product or may be introduced by back feed from the customer's system.

4.8.3. Odor test high-pressure cylinders containing the following products prior to filling the cylinder: Industrial Oxygen, Oxygen USP, All industrial mixtures containing oxygen, including standard and nonstandard industrial oxygen/argon mixtures, Nitrogen NF, Helium USP and Medical Gases.

4.8.4. Other recommended actions: Ensure that any room deodorizers used are of the type that suppress odors, not the type that

suppress the sense of smell itself. Temporarily reassign personnel doing odor testing to other duties if they have colds or hay fever.

4.9. CONDUCTING THE ODOR TEST

4.9.1. WARNING - Only certain designated gases may be odor tested. These gases are listed above. Odor testing of other gases is not authorized and may be harmful or fatal. Read and make sure you understand all information in this item before performing any odor testing.

4.9.2. Stand at arms length from the cylinder. Position it so that the valve points 90 degrees from you.

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4.9.3. WARNING - Never allow the valve to point toward your face during the test. Eye or skin damage may result. If you detect an odor at any time during the test, immediately close the valve and stop the test.

4.9.4. Slowly open the valve until gas flows. Stay at arms length, cup your hand, and fan the gas toward your nose. Cautiously smell the gas fanned by your hand. If you do not detect an odor, proceed to the next step.

4.9.5. Continue the fanning motion while moving closer to the cylinder. If you still cannot detect an odor, proceed to the next step.

4.9.6. Cup your hand around the valve outlet and move your head in close. Smell the gas issuing from the cylinder valve into your cupped hand.

4.9.7. If an odor is found, write "ODOR" on the cylinder sidewall using a paint stick and move the cylinder to the cylinder maintenance area.

4.9.8. Odor testing cylinders with insufficient pressure 4.9.9. If no gas flows from the cylinder in the steps above, there may not be enough residual pressure to

conduct the test. Use the following procedure to test the cylinder. 4.9.10. WARNING - Never blow into a cylinder valve to pressurize the cylinder. Sudden release of high

pressure or of a dislodged object could injure you. Use only an approved clean gas supply (Nitrogen, NF or Oxygen, USP), or a rubber squeeze bulb.

4.9.11. Regulate gas supplied from sources other than the squeeze bulb to 5 to 10 psig. Only a small volume of gas is required for the test. If a cylinder is used to supply the regulated pressure, it must be secured in a upright position by chaining to keep it from failing over and injuring someone.

4.9.12. Pressurize the cylinder to be odor tested slightly. 4.9.13. Repeat the odor test using the procedure above. 4.9.14. If no gas escapes from the cylinder, the valve is blocked. Mark BLOCKED VALVE on the

sidewall, using a paint stick and set the cylinder aside for maintenance. 4.10. HAMMER TEST

4.10.1. All empty, high-pressure, steel cylinders filled must be hammer-tested prior to being filled. The purpose of this test is to detect cylinders that have serious internal corrosion. Such cylinders may rupture on the charging rack.

4.10.2. No steel cylinder may be filled until it has passed the hammer test. 4.10.3. All cylinders that fail the hammer test must pass a hydrostatic test, including the visual internal

inspection required as part of the hydrostatic test, before they are put back into service. 4.10.4. NOTE: Customer-owned cylinders that fail the hydrostatic test should be stamped with the failed

retest symbol. 4.10.5. A 1/2-pound ball peen hammer is required for the test. 4.10.6. Position the cylinder so it is standing straight up. Be sure that the sidewall is not touching

anything. This could deaden the sound. 4.10.7. Tap the cylinder lightly with the hammer. 4.10.8. NOTE: The hammer blow must be light. Any cylinder will ring if it is hit hard enough. 4.10.9. Listen for a clear, bell-like tone. A dead cylinder has a flat tone. The purpose in conducting the

hammer test is to find dead cylinders and remove them from service. 4.10.10. Remove any cylinder from service at once if it sounds dead. Mark DEAD on the cylinder

sidewall, using a paintstick. 5. REFERENCES

CGA C-6 and C-6.1

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 4.2 High Pressure Oxygen Cylinder Filling

1. OBJECTIVE This procedure establishes the guideline for high pressure oxygen cylinder filling. 2. SCOPE This procedure applies to the PurityPlus specialty gases lab. 3. RESPONSIBILITIES

It is the responsibility of all laboratory personnel to ensure that this procedure is performed as described, that this procedure is reviewed and updated as necessary, and that proper support documentation is maintained.

4. PROCEDURE

4.1. Filling Procedure 4.1.1. Assure the Oxygen high pressure cryogenic pump is cooling down. If the liquid and return

valves are not open, open the pump liquid and return valves. These valves will be found outside at the pump.

4.1.2. Select the style of cylinders from the empty pile. The type of cylinders is determined by customer orders and direction from supervision. Move the cylinders to the inspection area adjacent to the fill manifold. Record the total number of cylinder’s to be filled by size on the PCR. Indicate whether they are steel or aluminum cylinders.

4.1.3. Perform all the pre-fill inspection procedures on the cylinders and record on the PCR as the steps are performed. Check all the pigtails to make sure they are in proper working order. If they are not in proper working order, replace the defective pigtails. Connect the cylinders to the manifold leads.

4.1.4. Open the cylinder valves and verify that the manifold to pigtail valves are open for each cylinder.

4.1.5. On duplex panels: open the manifold selector valve (A, B, etc.) at the top and sides of the panel which connects the panel to the appropriate manifold. Assure all other unused manifold selector valves are closed. (Note: It is possible and safe to be venting and vacuum operations on the opposite fill side while conducting fill operations.)

4.1.6. Open the vent valve for the selected manifold. 4.1.7. Once the cylinders have vented to atmospheric pressure, close the selected vent valve. 4.1.8. Start the vacuum pump. 4.1.9. Open the selected manifold vacuum valve. Use care not to over pressurize the vacuum

pump. Observe the vacuum level and assure that no more than 0 psig is indicated on the vacuum gauge. Also listen for the vacuum safety relief valve. If the safety relief valve functions or more than 0 psig are indicated on the vacuum gauge, immediately close the vacuum valve and further vent the cylinders before proceeding.

4.1.10. Evacuate the cylinders until the vacuum gauge reads the specified vacuum level – 29 inches Hg (see product specifications table).

4.1.11. Close the selected vacuum valve. 4.1.12. Shut off the vacuum pump. 4.1.13. Open the master product valve to the selected fill side (A, B, etc.) 4.1.14. Start the product filling by starting the high pressure Oxygen cryogenic pump. Assure the

pump has been cooled down to prevent pump damage. 4.1.15. Between 1000 psi and 1500 psi, perform the first leak check. Record this on the PCR. If

any leaks are found, close the cylinder valve and tag the cylinder indicating the location of the leak.

4.1.16. Between 1000 psi and 1500 psi, perform your heat check and record it on the PCR. 4.1.17. Once the cylinders are full as determined by the product specifications table, shut the high

pressure cryogenic pump off.

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4.1.18. Check the actual cylinder pressure and temperature and compare to the estimated pressure and temperature for this product and style of cylinder. If the actual pressure and temperature differ from what you expected, see your supervisor before proceeding.

4.1.19. Shut off all the cylinder valves. Then close the master product valve. Open the manifold vent valve. Vent down the pressure out of the line and close the main vent valve.

4.1.20. Record the full pressure/temperature on the PCR. 4.1.21. If the piping between the high pressure cryogenic pump and the manifold is pressurized

above 2500 psi, drain the line pressure to below 2500 psi by opening the master product valve and vent valve. This will prevent the pump safety from opening.

4.1.22. Assure master product valve and vent valves are closed. 4.1.23. Once line is vented, remove the pigtails from the cylinders. 4.1.24. Perform the final leak check. If any leaks are found, tag the cylinder indicating the location

of the leak. Move the cylinder to the cylinder repair area. 4.1.25. For medical Oxygen, connect a cylinder from the lot to the sample line and notify the lab

that the lot is ready for testing. Apply the “Quarantine” sign to the rack/lot. The “Quarantine” sign is removed only after a member of the Quality Control Unit has released the lot.

4.1.26. For medical Oxygen, record all remaining steps on the PCR. 4.1.27. Record the number of cylinders filled on the compression sheet. 4.1.28. If another rack will not be filled during the day, close the high pressure Oxygen cryogenic

pump liquid and return valves. These will be found outside at the pump. 5. REFERENCES

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 4.3 High Pressure Inert Gas & Mixture Cylinder Filling

1. OBJECTIVE This procedure establishes the guideline for high pressure inert gas and mixture cylinder filling. 2. SCOPE This procedure applies to the PurityPlus specialty gases lab using the multi-product control panel

described herein. 3. RESPONSIBILITIES


4. PROCEDURE 4.1. Safety precautions:

4.1.1. Eye protection (glasses or face shield)

4.1.2. Work gloves

4.1.3. Do not fill any cylinder unless it has passed all required external and prefill inspections.

4.1.4. The pigtail connecting the cylinder on the scale to the manifold must be stainless steel tubing. A hose may not be used for the cylinder on the scale because a hose gives unreliable readings under pressure.

4.2. Filling Procedure

4.2.1. For Nitrogen and Mixtures Only - Assure the appropriate high pressure cryogenic pump is cooling down. If the liquid and return valves are not open, open the pump liquid and return valves. These valves will be found outside at the pump. The Argon cryogenic pump will be cooled down later.

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4.2.2. Select the style of cylinders from the empty pile. The type of cylinders is determined by customer orders and direction from supervision. Move the cylinders to the inspection area adjacent to the fill manifold.

4.2.3. Perform all the pre-fill inspection procedures on the cylinders as the steps are performed. Check all the pigtails to make sure they are in proper working order. If they are not in proper working order, replace the defective pigtails. Connect the cylinders to the manifold leads. For Helium cylinders only – pressurize the manifold over 1000 psi and check for leaks. Repair any leaks that are found before proceeding.

4.2.4. Open the cylinder valves and verify that the manifold to pigtail valves are open for each cylinder. For Helium cylinders only - pressure check each cylinder and open the cylinder valves which contain less than 50 psi. Assure the cylinder which is placed on the scale is one that is less than 50 psi so that it will be evacuated.

4.2.5. If the panel is equipped with a swing arm product selector system, drain the swing arm and move the swing arm to the correct product. Close the swing arm drain valve.

4.2.6. Open the manifold selector valve (F or G) at the sides of the panel which connects the panel to the appropriate manifold. Assure all other unused manifold selector valves are closed. (Note: It is possible and safe to be venting and vacuum operations on the opposite fill side while conducting fill operations.)

4.2.7. Open the vent valve for the selected manifold.

4.2.8. Once the cylinders have vented to atmospheric pressure, close the selected vent valve.

4.2.9. Start the vacuum pump.

4.2.10. Open the selected manifold vacuum valve. Use care not to over pressurize the vacuum pump. Observe the vacuum level and assure that no more than 0 psig is indicated on the vacuum gauge. Also listen for the vacuum safety relief valve. If the safety relief valve functions or more than 0 psig are indicated on the vacuum gauge, immediately close the vacuum valve and further vent the cylinders before proceeding.

4.2.11. For Argon Only - Assure the Argon high pressure cryogenic pump is cooling down. If the liquid and return valves are not open, open the pump liquid and return valves. These valves will be found outside at the pump.

4.2.12. Evacuate the cylinders until the vacuum gauge reads the specified vacuum level (see product specifications table).

4.2.13. Close the selected vacuum valve.

4.2.14. If additional vacuums are specified in the products table, perform the additional vacuums by slowly opening the product valve until the appropriate grams or pressure are indicted. Close the product valve and slowly open the selected vacuum valve. Use care not to over pressurize the vacuum pump. Observe the vacuum level and assure that no more than 0 psig is indicated on the vacuum gauge. Also listen for the vacuum safety relief valve. If the safety relief valve functions or more than 0 psig are indicated on the vacuum gauge, immediately close the vacuum valve and further vent the cylinders before proceeding. Evacuate the cylinders until the vacuum gauge reads the specified vacuum level (see product specifications table). Close the selected vacuum valve.

4.2.15. Shut off the vacuum pump.

4.2.16. Press the “Tare” button on the scale display. The reading should change to “0”. If the reading does not change to “0” notify a supervisor.

4.2.17. Open the master product valve for the product selected on the swing arm.

4.2.18. For Helium cylinders only – open the cylinder valves on all the cylinders. This will equalize the pressure on residual cylinders with the evacuated cylinders.

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4.2.19. Start the product filling by starting the high pressure cryogenic pump, if necessary. Assure the pump has been cooled down to prevent pump damage. For Helium cylinders only – operate the high pressure receivers and diaphragm compressor to fill the cylinders.

4.2.20. For mixtures:

4.2.20.1. Once the cylinders have received the correct weight of the gas (as determined by the product specifications table), shut the high pressure pump off and close the master product valve. Note: use care in filling the correct number of grams for each product. You may need to shut the product flow before the target grams in order to have the correct grams in the cylinder. Also close the manifold selector valve (F or G).

4.2.20.2. Open the swing arm vent valve to bleed the pressure from the swing arm and move the swing arm to the next gas. Close the swing arm vent valve.

4.2.20.3. Slowly open the new master product valve corresponding to the swing arm position. Close the new master product valve. Open the swing arm vent valve to bleed the pressure from the swing arm and purge contaminants from the swing arm. Close the swing arm vent valve. Also open the manifold selector valve (F or G).

4.2.20.4. Continue with steps 16 through 19 until the final gas in the mixture has been selected, then proceed with this procedure.

4.2.21. Between 1000 psi and 1500 psi, perform the first leak check. If any leaks are found, close the cylinder valve and tag the cylinder indicating the location of the leak.

4.2.22. Between 1000 psi and 1500 psi, perform your heat check.

4.2.23. Once the cylinders are full as determined by the product specifications table, shut the high pressure cryogenic pump off (or diaphragm compressor) and close the master product valve. Note: use care in filling the correct number of grams for each product. You may need to shut the product flow before the target grams in order to have the correct grams in the cylinder.

4.2.24. Shut off all the cylinder valves. Then open the manifold vent valve. Vent down the pressure out of the line and close the main vent valve.

4.2.25. If the piping between the high pressure cryogenic pump and the manifold is pressurized above 2500 psi, drain the line pressure to below 2500 psi by opening the master product valve and vent valve. This will prevent the pump safety from opening.

4.2.26. Assure master product valve and vent valve are closed.

4.2.27. Once line is vented, remove the pigtails from the cylinders.

4.2.28. Perform the final leak check. If any leaks are found, tag the cylinder indicating the location of the leak.

4.2.29. Connect a cylinder from the lot to the sample line and notify the lab that the lot is ready for testing.

4.2.30. Record the number of cylinders filled on the compression sheet.

4.2.31. For Nitrogen and Mixtures - If another rack will not be filled during the day, close the high pressure cryogenic pump liquid and return valves. These will be found outside at the pump. For Argon - Close the high pressure Argon cryogenic pump liquid and return valves. These will be found outside at the pump. For Helium cylinders only – close the high pressure receivers and diaphragm compressor valves.

5. REFERENCES

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Quality Assurance Program Rev. 18 May 2009 Rev #: 2 Document Title: 4.4 High Pressure Flammable Gas & Mixture Cylinder Filling

1. OBJECTIVE This procedure establishes the guideline for flammable high pressure gas and mixture cylinder filling. 2. SCOPE This procedure applies to the PurityPlus specialty gases lab using the multi-product control panel



4. PROCEDURE 4.1. Safety precautions:

4.1.1. Prior to filling flammable gas cylinders, verify adequate fire protection is available (sprinklers, deluge systems, water cannon, etc.). Immediately suspend filling if fire protection water supply is unavailable or fails during filling.

4.1.2. PURGE and EVACUATE repaired or newly hydrotested cylinders prior to equalizing. Cylinders from hydrotest or repair must not be opened to the manifold with other cylinders containing flammable gas.


4.1.4. Work gloves

4.1.5. Do not fill any cylinder unless it has passed all required external and prefill inspections.

4.1.6. Although hydrogen, methane and other flammable gases may require the same CGA connection, change of service procedures must be followed to convert a cylinder from one gas service to another.

4.1.7. The pigtail connecting the cylinder on the scale to the manifold must be stainless steel tubing. A hose may not be used for the cylinder on the scale because a hose gives unreliable readings under pressure.

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4.2.1. Assure the appropriate high pressure cryogenic pump, if any, is cooling down. If the liquid and return valves are not open, open the pump liquid and return valves. These valves will be found outside at the pump.

4.2.2. Select the style of cylinders from the empty pile. The type of cylinders is determined by customer orders and direction from supervision. Move the cylinders to the inspection area adjacent to the fill manifold.

4.2.3. Perform all the pre-fill inspection procedures on the cylinders as the steps are performed. Check all the pigtails to make sure they are in proper working order. If they are not in proper working order, replace the defective pigtails. Attach a thermometer if the cylinders are being filled by pressure/temperature.

4.2.4. Pre-fill leak check - Connect the cylinders to the manifold leads. Pressurize the manifold over 1000 psi with a non-flammable, inert gas (helium, nitrogen, argon) and check for leaks. Repair any leaks that are found before proceeding.

4.2.5. Open the cylinder valves and verify that the manifold to pigtail valves are open for each cylinder.

4.2.6. If the panel is equipped with a swing arm product selector system, drain the swing arm and move the swing arm to the correct product. Close the swing arm drain valve.

4.2.7. Open the manifold selector valve (F or G, etc.) at the sides of the panel which connects the panel to the appropriate manifold. Assure all other unused manifold selector valves are closed. (Note: It is possible and safe to be venting and vacuum operations on the opposite fill side while conducting fill operations.)

4.2.8. Open the vent valve for the selected manifold.

4.2.9. Once the cylinders have vented to atmospheric pressure, close the selected vent valve.

4.2.10. Start the vacuum pump.

4.2.11. Open the selected manifold vacuum valve. Use care not to over pressurize the vacuum pump. Observe the vacuum level and assure that no more than 0 psig is indicated on the vacuum gauge. Also listen for the vacuum safety relief valve. If the safety relief valve functions or more than 0 psig are indicated on the vacuum gauge, immediately close the vacuum valve and further vent the cylinders before proceeding.

4.2.12. Evacuate the cylinders until the vacuum gauge reads the specified vacuum level (see product specifications table).

4.2.13. Close the selected vacuum valve.

4.2.14. If additional vacuums are specified in the products table, perform the additional vacuums by slowly opening the product valve until the appropriate grams or pressure are indicated. Close the product valve and slowly open the selected vacuum valve. Use care not to over pressurize the vacuum pump. Observe the vacuum level and assure that no more than 0 psig is indicated on the vacuum gauge. Also listen for the vacuum safety relief valve. If the safety relief valve functions or more than 0 psig are indicated on the vacuum gauge, immediately close the vacuum valve and further vent the cylinders before proceeding. Evacuate the cylinders until the vacuum gauge reads the specified vacuum level (see product specifications table). Close the selected vacuum valve.

4.2.15. Shut off the vacuum pump.

4.2.16. If the cylinders are being filled by weight, press the “Tare” button on the scale display. The reading should change to “0”. If the reading does not change to “0” notify a supervisor.

4.2.17. Open the master product valve for the product selected on the swing arm.

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4.2.18. Start the product filling by starting the high pressure cryogenic pump, if necessary. Assure the pump has been cooled down to prevent pump damage. For product supplied in a tube trailer, receivers or banks – operate the high pressure gas source and/or diaphragm compressor to fill the cylinders.

4.2.19. For mixtures:

4.2.19.1. Once the cylinders have received the correct pressure or weight of the gas (as determined by the product specifications table), shut the high pressure pump off and close the master product valve. Note: use care in filling the correct pressure or number of grams for each product. You may need to shut the product flow before the target grams in order to have the correct pressure of grams in the cylinder. Also close the manifold selector valve (F or G, etc.).

4.2.19.2. Open the swing arm vent valve to bleed the pressure from the swing arm and move the swing arm to the next gas. Close the swing arm vent valve.

4.2.19.3. Slowly open the new master product valve corresponding to the swing arm position. Close the new master product valve. Open the swing arm vent valve to bleed the pressure from the swing arm and purge contaminants from the swing arm. Close the swing arm vent valve. Also open the manifold selector valve (F or G, etc.).

4.2.19.4. Continue with steps 16 through 19 until the final gas in the mixture has been selected, then proceed with this procedure.

4.2.20. Between 1000 psi and 1500 psi, perform the first leak check. If any leaks are found, close the cylinder valve and tag the cylinder indicating the location of the leak.

4.2.21. Between 1000 psi and 1500 psi, perform the heat of compression check.

4.2.22. Once the cylinders are full as determined by the product specifications table, shut the high pressure cryogenic pump off (or tube trailer, receivers, diaphragm compressor, etc.) and close the master product valve. Note: use care in filling the correct pressure or number of grams for each product. You may need to shut the product flow before the target pressure or grams in order to have the correct grams in the cylinder.

4.2.23. Shut off all the cylinder valves. Then open the manifold vent valve. Vent down the pressure out of the line and close the main vent valve.

4.2.24. If the piping between the high pressure cryogenic pump and the manifold is pressurized above 2500 psi, drain the line pressure to below 2500 psi by opening the master product valve and vent valve. This will prevent the pump safety from opening.

4.2.25. Assure master product valve and vent valve are closed.

4.2.26. Once line is vented, remove the pigtails from the cylinders.

4.2.27. Perform the final leak check. If any leaks are found, tag the cylinder indicating the location of the leak.

4.2.28. Install plugs or caps on valve outlets, if required.

4.2.29. Connect a cylinder from the lot to the sample line and notify the lab that the lot is ready for testing.

4.2.30. Record the number of cylinders filled on the compression sheet.

4.2.31. If another rack will not be immediately filled, close the high pressure cryogenic pump liquid and return valves. These will be found outside at the pump. For product supplied in a tube trailer, receivers or banks – close the high pressure tube trailer, receivers, diaphragm compressor valves, etc..

5. REFERENCES

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Quality Assurance Program Rev. 16 Oct 2009 Rev #: 0 Document Title: 4.5 High Pressure Carbon Dioxide Cylinder Filling Procedures

A. Safety precautions:

• Eye protection (glasses or face shield)

• Work gloves

• The following method uses the scale to fill the cylinders by weight.

B. CYLINDER PREPARATION AND FILLING

Do not fill any cylinder unless it has passed all required prefill inspections. DOT Requirements - Requirements for cylinders in carbon dioxide service are the same as those for cylinders in standard gas service. Hydrostatic Retest -Cylinders in carbon dioxide service must be given a hydrostatic retest every five (5) years.

C. CYLINDER TARE WEIGHT All cylinders being filled with carbon dioxide must have a tare weight stamped on the shoulder to allow for proper filling of carbon dioxide liquid by weight. If a cylinder does not bear the tare weight stamping, do not fill the cylinder. Inform the customer of the tare weight requirement and offer to tare-weigh the cylinder. If the weight of an empty cylinder does not agree with the tare weight stamped on the cylinder, allowing for the weight of the valve, remove the cylinder from service and internally inspect it. Treat the cylinder as though it had failed the hammer test. NOTE: The tare weight of cylinders may or may not include the weight of the valve.

D. CYLINDER VALVES CO2 cylinders must have a bursting disc safety device. CO2 cylinders may NOT have a fusible metal safety.

The proper rating is listed below.

Stamped Cylinder Service Pressure 1800 psig 3000 psig 2000-2200 psig 3360 psig 2400 psig 4000 psig

Eductor Tubes (Dip Tubbes/Siphon Tubes)-Cylinders for customers who require liquid carbon dioxide withdrawal should have valves equipped with eductor tubes and marked as such.

E. CYLINDER PROCESSING Carbon dioxide cylinders must be blown down before filling.

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F. PUMP OPERATING PROCEDURES

Whenever starting the filling unit from a shut down condition follow the start-up procedures below:

1. Open Pump Inlet Valve B. This will pressurize the strainer and the pump.

2. Assure Bypass Valve C is open. Carbon dioxide from the liquid storage tank will now pressurize the complete cylinder filling unit. The bypass returning to the storage tank is now open.

3. Open the Vent Valve E to prime the pump. Close the Vent Valve E when liquid Carbon

Dioxide is discharged from the valve. 4. Open Pump Recirculation Valve A.

5. Press the "START" button on the pump.

The cylinder filling unit is designed to fill high pressure cylinders either singly or in pairs with continuous charging of one cylinder taking place. The following operational procedure is applicable to both types of filling operations except where specified.

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Filling a Single Cylinder-

1. Before starting to fill a cylinder, assure the Pump Discharge Valve D is open, the Cylinder Fill Valve F is closed and the Vent Valve E is closed.

2. Zero the scale by pressing the Zero or Tare button on the scale display. 3. Place a cylinder to be filled on the scale. Check the weight of the cylinder against the tare

weight stamped on the cylinder. The tare weight should include the cylinder and valve. *** For cylinders with a 20 pounds or more CO2 capacity: If the actual weight of the cylinder is more than 1 pound different than the stamped tare weight set the cylinder aside for inspection by supervision.

*** For cylinders with less that a 20 pound CO2 capacity: If the actual weight of the

cylinder is more than 1/2 pound different than the stamped tare weight set the cylinder aside for inspection by supervision.

4. Connect flexible charging hose to the cylinder and tare the scale.

5. Open the Cylinder Fill Valve F and cylinder valve.

6. Close the Bypass Valve C.

NOTE: As the empty cylinder starts filling, the charging pressure indicated on the pressure gauge will decrease and gradually increase as filling proceeds. CAUTION: Do not overfill the cylinder. If a Cylinder is overfilled, the excess carbon dioxide must be vented so that the safety disc on the cylinder will not rupture.

7. Allow carbon dioxide to fill the high-pressure cylinder until the correct amount of product

has been added, as indicated on the scale. When the cylinder is full, open the Bypass Valve C.

8. Close the Cylinder Fill Valve F and then the cylinder valve. WARNING: Never discharge or bleed off carbon dioxide through the flexible charging hose unless they are connected to the cylinder or firmly secured. If not firmly secured, a flexible charging line will whip around and may cause serious personal injury.

9. Carefully disconnect flexible charging hose. Avoid being splashed with the liquid CO2

which will vent from the fill connection.

10. Recordkeeping - Complete fill/compression logs

11. If no more cylinders are to be filled, refer to the shut-down procedures below.

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G. FILLING ALTERNATE CYLINDERS If cylinders of the same size are being filled alternately in pairs, with continuous charging taking place, one Cylinder Fill Valve F is open for filling while the other is closed for attaching or removing the second cylinder. CAUTION: Do not allow the equipment to idle at charging pressure for long periods of time. This will cause pressure buildup within the storage tank and excessive wear to the cylinder filling unit.

H. SHUT-DOWN PROCEDURES If no more cylinders are to be filled, follow the procedures below. WARNING: Never discharge or bleed off carbon dioxide through the flexible charging lines unless they are connected to a cylinder or are firmly secured. A flexible charging line will whip around if not firmly secured and may cause serious personal injury. 1. Assure Bypass Valve C is open. Then stop the electric motor by pressing the STOP button on

the motor switch.

2. Close the Pump Inlet Valve B and Pump Recirculation Valve A.

3. Bleed the carbon dioxide from the cylinder filling unit assembly and from the interconnecting piping by opening the Vent Valve E.

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 4.6 Cryogenic Container Fill Procedures

1. OBJECTIVE This guideline establishes the procedure to use the fill cryogenic containers. 2. SCOPE This procedure applies to the PurityPlus specialty gases lab/plant when using the equipment



4. PROCEDURE

4.1. Safety precautions:


4.1.2. Work gloves

4.1.3. Do not fill any containers unless it has passed all required external and prefill inspections.

4.1.4. The following medical containers must be purged with the same gas that will be filled in the container: 1) New containers 2) Containers returning from maintenance 3) Containers that are returned from the customer with any outlet valves open (use, vent or liquid). The container is approved for use if the gas in the container is free of odor and passes the ID and assay requirements for the product.

4.1.5. The following method uses the scale to fill the containers by weight. The vent valve is not to be used as a fill termination method unless approved by the Operations Manager. This approval shall apply only to the indicated cylinders and only on the approved date.


4.2.1. Before filling medical cryogenic containers:

4.2.1.1. You must perform and fill out all the necessary information on the PCR.

4.2.1.2. Remove the old lot sticker and affix the new lot sticker to the container and the PCR.

4.2.2. Perform the pre-fill inspections on the container.

4.2.3. Verify that the “Pull On-Push Off” button is pulled out on the scale panel.

4.2.4. Verify that the “Emergency” stop on control panel is pulled out.

4.2.5. Verify that the toggle switch on control panel is in the “On” position for the product that you plan on filling on the scale. Assure the other product toggle switches are off.

4.2.6. Make sure manual shut-off valve is open on fill manifold and hose drain valve is closed. Also, the shut-off valve from bulk tank supply source should be open.

4.2.7. Verify that the scale is empty and that the scale indicator shows two diamonds.

4.2.8. Push “Select” on scale panel.

4.2.9. Push “Preset” on scale panel.

4.2.10. Push “Enter” (if this reading is zero, input 1000 and push enter).

4.2.11. Push “Enter” a second time.

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4.2.12. Enter gross filling weight (tare weight plus product weight) of container style to be filled. See product specifications table for the net weight.

4.2.13. Push “Enter” on scale panel.

4.2.14. Push “Start” button on scale panel.

4.2.15. Put liquid cylinder on the scale platform.

4.2.16. Connect flex hoses for fill and vent.

4.2.17. Open “Fill” and “Vent” valves on the container. Assure the other valves (use, pressure building, etc.) valves are closed on the container.

4.2.18. When ready to start fill operation, push “Reset” on control panel to start filling cycle: opens solenoid valve and fill light comes on.

4.2.19. When required weight is achieved the scale will shut down the fill process.

4.2.20. Close “Liquid” and “Vent” valves on liquid cylinder.

4.2.21. Open hose drain valve on liquid fill manifold to empty residual pressure in the flex hose. Close hose drain valve

4.2.22. Remove liquid cylinder from the scale.

4.2.23. For next liquid cylinder to fill of the same product, start at step 8 (Push “Select” on scale panel…) and continue until all necessary containers of this product are full. If container is the same product and final gross weight, start at step 14 (Push “Start” button …) and continue until all necessary containers of this product are full.

4.2.24. Perform final visual leak check. Leak check all piping, pressure gauge, burst disk, safety and liquid level gauge. Record leak check on the PCR

4.2.25. Assure all necessary testing requirements are performed. Follow testing procedures as written in the manual.

5. REFERENCES:

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 4.7 Mixture Compatibilities

1. OBJECTIVE This procedure establishes the procedure for Mixture Compatibility Guidelines 2. SCOPE

The following mixture guidelines are to be used for PurityPlus Specialty Gas mixtures. 3. RESPONSIBILITIES


4. PROCEDURE 4.1. The maximum amount of a flammable gas allowed to be mixed with an oxidizing gas is such that

amount of the flammable gas, which if it completely reacted with the oxidizing gas, would release a maximum of 1299 BTU of energy for each cubic foot water volume in the cylinder.

4.2. Mixtures of a flammable gas and oxidizers are not to be made in low pressure cylinders. 4.3. Mixtures containing carbon monoxide will not be pressurized over 5/6 the working pressure of the

cylinder (or 2000 psig, whichever is lower). 4.4. Fuel/oxidizer mixtures shall be authorized in writing by the highest operations officer in the

company, or designee. Special care will be given to fuel rich mixtures and mixtures over the UEL. These are potentially hazardous mixtures requiring special procedures.

4.5. Fuel/oxidizer mixtures and toxic gas mixtures shall be authorized in writing by the highest operations officer in the company, or designee.

4.6. Seventy percent of the vapor pressure of a liquefied gas component will not be exceeded. 4.7. DOT regulations specify that cylinders containing fusible metal safeties may not be filled over their

working pressure. (10% overfill is not permitted with fuse plug safeties.) 4.8. The chemical compatibility of acid or basic gases with a fuel or oxidizing gas will be determined in

writing before the mixture is made. 4.9. The chemical compatibility of carbon monoxide with corrosive or sulfur containing gases will be

determined in writing before the mixture is made. 4.10. The partial pressure of acetylene in a mixture will not exceed 22 psia. 4.11. The chemical compatibility of hydrogen sulfide and sulfur dioxide containing gases will be

determined in writing before the mixture is made. 4.12. The chemical compatibility of hydrogen and unsaturated hydrocarbons (ethylene, acetylene,

propylene, etc.) will be determined in writing before the mixture is made. 4.13. Mixtures containing both acid and basic gases will not be made.

5. REFERENCES

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 4.8 Micro Cylinder Procedure

1. OBJECTIVE This guideline establishes the mixture fill procedures for using micro-cylinders 2. SCOPE

These mixture guidelines may be used for making mixtures using a micro-cylinder. 3. RESPONSIBILITIES


4. PROCEDURE 4.1. Make sure all valves on the panel are closed. (Scale Isolation, Vacuum, Vent, Vacuum Isolation

Valve, etc.) 4.2. Open cylinder valve on the micro cylinder to drain the pressure. 4.3. Vacuum the system following these procedures: 4.4. Open Vacuum valve. 4.5. Open Vacuum Isolation valve. 4.6. After a rise is indicated on the vacuum gauge, hold the vacuum for another 2-3 seconds. 4.7. Close Cylinder valve on micro cylinder. 4.8. Close Sample Cylinder valve. 4.9. Remove micro cylinder and weigh until you get good repeatability. Prefer 3 repeatable weighs. 4.10. Reconnect micro cylinder to panel making sure the safety is at the top. Tighten only hand tight. 4.11. Pull vacuum on system using the following procedures: 4.12. Open Sample Inlet valve. 4.13. Open Vacuum valve. 4.14. Open Vacuum Isolation Gauge valve. 4.15. After a rise is indicated on the vacuum gauge, hold the vacuum for another 2-3 seconds. 4.16. Close Vacuum Isolation Gauge valve. 4.17. Close Vacuum Gauge valve. 4.18. Move Swing arm to gas that is desired. 4.19. Open Vacuum valve. 4.20. Open Low Pressure Gauge Isolation valve. 4.21. Close Vacuum valve. 4.22. Open cylinder valve on micro cylinder. 4.23. Open Supply valve. 4.24. Fill to predetermined pressure. 4.25. Close Low Pressure Gauge Isolation valve. 4.26. Close cylinder valve on micro cylinder. 4.27. Remove micro cylinder. 4.28. Weigh micro cylinder until repeatability is achieved. Three repeatable weighs are preferred. 4.29. Reattach micro cylinder to panel. 4.30. Move Supply cylinder to scale. 4.31. Attach fill line. 4.32. Switch the solenoid valve to ON, if applicable. 4.33. Close ALL valves. 4.34. Open Scale Isolation valve. 4.35. Move Swing Arm to Balance Gas (i.e. Nitrogen). 4.36. Pressurize system to 1000 psi with balance gas. 4.37. Check all connection for leaks using a soapy solution.

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NOTE: If a leak is found, drain all pressure and correct leaks. Never correct leaks with the system pressurized. 4.38. Dry cylinder and scale of leak detection solution. 4.39. Vent system. 4.40. Vacuum System using the following procedures: 4.41. Open Vacuum valve. 4.42. Open Vacuum Isolation Gauge valve. 4.43. Open Sample Isolation Gauge valve. 4.44. Open Sample Out valve. 4.45. Open Sample In valve. 4.46. Open Cylinder valve. 4.47. Tare Cylinder on scale. 4.48. Close Scale Isolation valve. 4.49. Open micro cylinder outlet valve. 4.50. Close Sample Inlet valve. 4.51. Close Vacuum valve. 4.52. Open micro cylinder Inlet valve. 4.53. Open Supply Valve to 1000 psi. 4.54. Open Sample Inlet valve. 4.55. Open Supply valve to flush micro cylinder. 4.56. Close Supply valve. 4.57. Close Sample Inlet and Outlet valve. 4.58. Open Supply valve to fill to desired weight. 4.59. Open Scale Isolation valve to control filling supply. 4.60. Slow gas flow as you approach fill weight. 4.61. Stop filling at desired weight. It is preferred to Underfill than Overfill. 4.62. Close Cylinder valve. 4.63. Close Supply valve. 4.64. Open Scale Isolation valve. 4.65. Vent system 4.66. Disconnect Fill line from cylinder. 4.67. Close Scale Isolation valve. 4.68. Open top and bottom valves on micro cylinder. 4.69. Close bottom valve on micro cylinder. 4.70. Close Sample Outlet valve. 4.71. Close Vent. 4.72. Open Vacuum valve. 4.73. Open Vacuum Isolation Gauge valve. 4.74. Connect fill line from Oxidizer panel to cylinder. 4.75. Vacuum Panel to Cylinder using the following procedure: 4.76. Open Vacuum valve. 4.77. Open Vacuum Isolation Gauge valve. 4.78. After a rise is indicated on the vacuum gauge, vacuum for an additional 2-3 seconds. 4.79. Close Vacuum Isolation Gauge valve. 4.80. Close Vacuum valve. 4.81. Open Supply Gas valve slowly to 1600 psi. 4.82. Close Scale Isolation valve. 4.83. Leak Check connections with soapy solution. NOTE: If a leak is detected, drain all pressure before correcting any leaks. Never correct a leak with pressure on the lines. 4.84. Tare the cylinder on the scale. 4.85. Slowly open cylinder valve to equalize pressure in fill line. 4.86. Open Supply valve. 4.87. Open Scale Isolation valve slowly and use this valve to throttle filling. 4.88. Fill to desired weight. 4.89. Close cylinder valve. 4.90. Close Supply valve. 4.91. Open Scale Isolation valve. 4.92. Vent panel.

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4.93. Close vent. 4.94. Close Scale Isolation valve. 4.95. Disconnect fill line from cylinder. 4.96. Tag and label cylinder before removing from scale.

5. REFERENCES

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 5 Analytical LWIs

This section contains the specific procedures to assure PurityPlus Specialty Gas products meet established analytical specifications.

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 5.1 Standard Definitions

1. OBJECTIVE

This procedure establishes standard definitions to be used throughout the equipment, fill and analytical procedures.

2. SCOPE This procedure applies to the PurityPlus specialty gases lab. 3. RESPONSIBILITIES It is the responsibility of all laboratory personnel to understand the definitions in this procedure. 4. PROCEDURE

The following definitions are used at the PurityPlus specialty gas lab. Anhydrous: A material that contains no water.

Annealing Gas: A hydrogen-nitrogen mixture used to provide a reducing atmosphere during heating of metals to render them less brittle on cooling.

Bursting Disc: See Frangible Disk.

Calibration Gas: A gas mixture of known composition used for the calibration of an instrument or control of a process reaction.

CGA: Denotes Compressed Gas Association. Usually used to refer to a cylinder valve outlet connection detailed in the CGA pamphlet V-1.

Compressed Gas: Any material or mixture having in the container, pressure exceeding 40 psia at 70oF or having an absolute pressure exceeding 104 psia at 130oF.

Corrosive: Electrochemical disintegration or decomposition; to gnaw or eat away. A product which will deteriorate many substances it comes into contact with, such as metals, polymers or tissue.

CP: Abbreviation for Chemically Pure. Indicates a grade and purity of a product. However, the purity may not be the same from product to product.

Critical Pressure and Temperature: That state at which the densities of the gas and liquid phases and all other intensive properties of these phases become identical.

Critical Volume: Volume occupied by unit mass of a substance at its critical pressure and temperature.

Cryogenic: Refers to the field of low temperatures usually -200oF or below.

Dew Point: Temperature at which the liquefaction of a vapor begins. Usually applied to the amount of water vapor in some gas.

Doping Gas: A gas or gas mixture used by the electronics industry to add controlled amounts of impurities to dope silicons or other semiconductors. Also applied in a general way to all gases used in the manufacture of semiconductors.

DOT: Abbreviation for Department of Transportation. Their 49th code of federal regulations regulate the movement of hazardous materials.

Filling Density: The percent ratio of the weight of the gas in a container to the weight of water that the container will hold at 60oF.

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Flammable Gas: According to DOT 49 CFR, it is any gas at N.T.P.(1) that forms a flammable mixture with air at a concentration of 13% or less or (2) that has a flammable range wider than 12% with air regardless of the lower flammable limit.

Flammable Range: The range over which a gas at N.T.P. will form a flammable mixture with air.

Forming Gas: A mixture of 5.7% or more of hydrogen in nitrogen.

Frangible Disk: A metal disk which is part of a safety device, and which is intended to burst and allow the gas to escape within predetermined pressure limits to prevent the rupture of the container. Sometimes used in conjunction with a fusible plug.

Fusible Plug: A safety device which has a channel, filled with a suitable low melting alloy and is intended to yield at a predetermined temperature and allow the gas to escape, preventing the rupture of the container. Sometimes used in conjunction with a frangible disk.

Hydrostatic Test: A container test required at definite intervals by DOT to determine the wall thickness via measuring elastic expansion. Purpose of the test is to assure the container is safe for continued use.

Inert: A material which under normal temperatures and pressures does not react with other materials.

Inhibited: A gas which has had a substance added to prevent or deter its reaction either with other materials or itself (polymerization). Usually used to deter polymerization.

Liquefied Compressed Gas: A gas which is partially liquid at its charging pressure and 70oF.

L.E.L.: Abbreviation for Lower Explosive Limit - The minimum percent by volume of a gas which when mixed with air at N.T.P. will form a flammable mixture. See Flammable Gas.

Mole: One molecular weight (or formula weight) in the appropriate units such as rams, pounds, etc. A gram-mole is the weight in grams equal to the molecular weight.

Molecular Weight: The relative mass of a molecule in relation to a fixed standard.

N.T.P.: Refers to normal temperature and pressure which is defined as 70oF and 14.696 psia.

Olfactory Fatigue: The loss of the sense of smell, due to exposure to high concentrations of a gas or prolonged exposure to the gas (either low or high concentrations).

Oxidizer: A substance which yields oxygen readily, removed hydrogen from a compound, or attracts negative electrons. Usually refers to a gas that causes or supports combustion such as oxygen, nitrous oxide, chlorine triflouride, or fluorine.

Partial Pressure: In any mixture of gases the total pressure is equal to the sum of the pressures each gas would exert were it alone present in the volume occupied by the mixture (Dalton's Law); i.e., the total pressure is equal to the sum of the partial pressures of the individual gases.

Polymerization: Reaction in which two or more molecules of the same substance combine to form a compound, usually in the form of extended chains of molecules.

ppm: Abbreviation for parts per million. A convenient means of expressing low concentrations of gas by volume.

psia: Abbreviation for pounds per square inch absolute. One atmosphere pressure equals 14.696 psia. psia = psig + 14.696.

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psig: Abbreviation for pounds per square inch gauge. Gauge pressure always ignores the first atmosphere absolute (14.696 psia).

Pyropnoric: Materials which spontaneously ignite on contact with air at normal conditions.

Rare Gas: Refers to those constituents of air which comprise less than 1% of air and are generally considered inert: argon, helium, krypton, neon, and xenon.

Safety Relief Valve: A safety relief device containing an operating part that is held normally in a position closing a relief channel by spring force and is intended to open and close at a predetermined pressure. Also referred to as a spring loaded POP.

Span Gas: Usually a gas mixture used to "span" or calibrate a process or laboratory instrument.

Specific Heat: Amount of heat required to raise a unit weight of substance one degree of temperature at either constant pressure or constant volume. usually expressed in BTU per pound per degree F.

Specific Volume: Volume of a unit weight of substance at a given temperature. Expressed as cubic feet per pound at 70oF as used in this manual.

Stable Isotope: Forms of the same element which are not radioactive having the same atomic number but different atomic weights due to the variance in the number of neutrons in the nucleus. These differences cause very slight changes in physical properties.

S.T.P.: Refers to standard temperature and pressure which is defined as 0oC and 760 mm of mercury (14.696 psia).

TECH: Abbreviation for technical. Indicates a grade and purity of product. However, the purity may not be the same from product to product.

T.L.V.: Refers to Threshold Limit Value. It is a time weighted concentration expressed as parts per million by volume for gases and vapors that represents conditions under which it is believed that nearly all workers may be repeatedly exposed day after day, without adverse effect.

Toxicity: The ability of a chemical compound to produce injury once it reaches a susceptible site in or on the body.

THC: Refers to total hydrocarbon content. Usually used to describe the quantity of a hydrocarbon impurity present, expressed as methane equivalents.

USP: Abbreviation for United States Pharmacopoeia. An organization which sets standards of purity, packaging, etc. for materials many of which are recognized by the Food and Drug Administration.

Vapor Pressure: The pressure at which a liquid or solid and its vapor are in equilibrium at a definite temperature.

Zero Gas: Gases which have low THC content and are used as a reference point to "zero" a THC analyzer..

5. REFERENCES None

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 5.2 Conversion Factors

1. OBJECTIVE This procedure establishes standard conversion factors. 2. SCOPE This procedure applies to the PurityPlus specialty gases lab. 3. RESPONSIBILITIES


4. PROCEDURE 4.1. Water Volumes - In order to determine the internal volume of various cylinders, water volumes are

used. This unit is nothing more than the number of cubic feet contained within the cylinder. It is determined by taring an empty cylinder and then filling it with water and weighing it again. Using the constant for 62.3 lbs. of water per cubic foot, it becomes an easily obtainable volume.

For example: 200/K cylinders contain 96 lbs. of water 96 lbs. / 62.3 lbs./cu.ft. = 1.54 cu.ft.

4.2. Density - The density of a gas is at times a very useful piece of information. Basically, it is the weight in grams of one liter of gaseous product.

4.3. PSIA and PSIG - The two methods of reporting pounds of pressure are PSIG and PSIA. PSIA is an abbreviation for pounds per square inch absolute. One atmosphere equals 14.69 psia. PSIG is an abbreviation for pounds per square in gauge. Gauge pressure always ignores the first atmosphere absolute.

PSIA = PSIG + 14.69 It is of critical importance to know the units of the gauges you use and to report pressure in the proper form.

4.4. Grams Per Cubic Foot of Gas - In the preparation of weight mixtures, a very useful piece of information is the number of grams needed of each component. This number is easily obtained by multiplying the cubic foot volumes of the specific component by the grams per cubic foot value. These values are simply the product of the gas density and the constant of 28.317 l/cu.ft.

Gas Density (g / L of gas) X 28.317 L / cu.ft. = g / cu.ft. Argon = 1.664 g / L X 28.317 L / cu.ft. = 47.12 g / cu.ft.

4.5. Per Cent - PPM - One important relationship to be totally familiar with is that of ppm and per cent. The table below illustrates the relationship:

100% = 1,000,000 ppm = 1 = 1 X 100 10% = 100,000 ppm = 0.1 = 1 X 10-1 1% = 10,000 ppm = 0.01 = 1 X 10-2 0.1% = 1,000 ppm = 0.001 = 1 X 10-3 0.01% = 100 ppm = 0.0001 = 1 X 10-4 0.001% = 10 ppm = 0.00001= 1 X 10-5 0.0001%= 1 ppm = 0.000001= 1 X 10-6

4.6. Cubic Feet Per Liter - 1 cubic foot = 28.317 liters 4.7. Millimeters Of Mercury To Psi - One extremely valuable constant is that of the number millimeters

of mercury per pound of absolute pressure. This is used extensively in low ppm millimeter additions to cylinders. The constant is derived as follows:

1 atm. = 14.7 psia 1 atm. = 760 mm of Hg

5. REFERENCES None

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 5.3 Oxygen PPM Analysis

1. OBJECTIVE

This procedure establishes the general procedures to use Trace Oxygen Analyzers.

2. SCOPE This procedure applies to the PurityPlus specialty gases lab.


4. PROCEDURE 4.1. Span Procedure

4.1.1. Apply the certified span gas to the instrument.

4.1.2. Adjust flow and pressure according to the instrument specifications.

4.1.3. Wait for the span reading to stabilize. If the instrument does not indicate the certified value of the span cylinder, then adjust with the span control until the instrument reading agrees with the certified Oxygen concentration in the span cylinder.

4.1.4. Record the readings on the calibration record.

4.1.5. This process should be repeated weekly or when readings are suspect.

4.2. Sample Procedure

4.2.1. Apply the sample gas to the instrument.

4.2.2. Adjust flow and pressure according to the instrument specifications.

4.2.3. Wait for the sample reading to stabilize.

4.2.4. Record the readings on the analysis record.

4.2.5. This process should be repeated every time a sample is to be analyzed.

5. REFERENCES Trace Oxygen Analyzer manual

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 5.4 Illinois Instruments Model 6000 Oxygen Analysis

1. OBJECTIVE

This procedure establishes the procedures to use Illinois Instruments Model 6000 Oxygen Oxygen Analyzers.



4. PROCEDURE 4.1. Span Procedure


4.1.2. Adjust flow to read between 100 and 200 ml/min. according to the instrument specifications.

4.1.3. Wait for the span reading to stabilize. If the instrument does not indicate the certified value of the span cylinder, then adjust with the span control menu until the instrument reading agrees with the certified Oxygen concentration in the span cylinder.


4.1.5. This process should be repeated daily or when readings are suspect.

4.1.6. Alternately, the system can be programmed to auto calibrate daily. See instrument manual for programming instructions.



4.2.2. Adjust flow to read between 100 and 200 ml/min. according to the instrument specifications.




5. REFERENCES Illinois Instruments Model 6000 Precision Oxygen Analyzer manual

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 5.5 Moisture PPM Analysis (Electrolytic Hygrometer)

1. OBJECTIVE This procedure establishes the general procedures to use the electrolytic moisture analyzer. 2. SCOPE This procedure applies to the PurityPlus specialty gases lab. 3. RESPONSIBILITIES


4. PROCEDURE

4.1. Open the valve on your sample gas cylinder.

4.2. Assure the sample regulator is adjusted to 15 to 25 psi. This is not a critical parameter and is important only to make the hygrometer flow adjustments consistent.

4.3. Open the bypass flowmeter on the sample line as wide as practical. This will reduce the cycle purge time.

4.4. Cycle purge the sample.

4.5. Set the bypass flowmeter on the sample line to read approximately 0.5 SCFH.

4.6. Turn the “Sample/Purge” valve on the hygrometer panel to the “Purge” position.

4.7. Turn the sample selector valve on the hygrometer panel to “SC-1” or “SC-2” if so equipped. This indicates through which Sample Common that the sample will be flowing.

4.8. Set the bypass flowmeter on the hygrometer panel to read approximately 0.5 to 1.5 SCFH.

4.9. Fasten the quick connect pigtail from the appropriate sample common to the flowmeter indicating the source of the sample.

4.10. Turn the “Sample/Purge” valve to the “Sample” position.

4.11. Assure the sample flowball on the front of the hygrometer is set for a true 100 ml/min. A true 100 ml/min will require different apparent settings on the flowmeter. Use a flowmeter calibrated to the sample gas to verify the hygrometer flow settings.

4.12. Observe the Hygrometer meter until it stabilizes (typically approximately 2 minutes). This will give you the sample reading. Turn the “Sample/Purge” valve to the “Purge” position.

4.13. Record the ppm Moisture reading on the analytical record.

4.14. Close the sample cylinder valve.

4.15. This process should be repeated every time a sample is to be analyzed.

4.16. This instrument is intrinsically calibrated and should be checked at least quarterly using “Intermediate Testing”.

5. REFERENCES Hygrometer Users Manual

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 5.6 Moisture PPM Analysis (Panametrics Series 35)

1. OBJECTIVE This procedure establishes the procedure to use the Panametrics Series 35 Moisture analyzer. 2. SCOPE This procedure applies to the PurityPlus specialty gases lab. 3. RESPONSIBILITIES


4. PROCEDURE 4.1. Calibration Verification Procedure

4.1.1. This procedure simply verifies that the sensor remains in calibration. This is not required by the manufacturer, but is required by PurityPlus labs.

4.1.2. The Panametrics Hygrometer is insensitive to flow changes in the ranges present in PurityPlus laboratories. Up to 5,000/10,000 cm/sec. are tolerated well.

4.1.3. Apply the certified span verification gas to the instrument. Because of the difficulty acquiring certified moisture standards, the certified span gas is verified when a freshly calibrated sensor is installed.

4.1.4. Wait for the span verification reading to stabilize. If the instrument does not indicate the certified value of the span cylinder within +/- 2 degrees C (above 1 ppm), then consult the factory for troubleshooting/maintenance. Consult instrument manual, page A-23 (User’s Manual 910-140A1, © 1995, 6/23/89) to convert dewpoint in degrees C to ppmv.


4.1.6. This process should be repeated quarterly, or when readings are suspect.






5. REFERENCES Panametrics Hygrometer Users Manual, P/N 910-140A1, © 1995

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 5.7 Total Hydrocarbon Analysis

1. OBJECTIVE This procedure establishes the general analytical steps for the Total Hydrocarbon Analyzer. 2. SCOPE This procedure applies to the PurityPlus specialty gases lab. 3. RESPONSIBILITIES


4. PROCEDURE

4.1. Setup: Set the support gas regulators as follows:

4.2. Fuel – 50 psi, or as specified in the user manual

4.3. Air – 50 psi, or as specified in the user manual

4.4. THA Zero – 20 psi (using the same balance gas as the intended sample gas, e.g. Helium Zero) , or as specified in the user manual

4.5. THA Span – 20 psi (using the same balance gas as the intended sample gas, e.g. 20 ppm Methane in Helium) , or as specified in the user manual

4.6. Set the Total Hydrocarbon Analyzer (THA) instrument as follows:

4.7. Set the “Range” switch to display the span gas over 50% of the full scale.

4.8. Set the “FID” “Samp.” regulator control to 4.0 psi. Adjust as needed to calibrate the span gas.

4.9. Set the “FID” “Fuel” regulator control to 20 psi, or as specified in the user manual

4.10. Set the “FID” “Air” regulator control to 15 psi, or as specified in the user manual

4.11. Set the Total Hydrocarbon Analyzer (THA) sample selection panel as follows:

4.12. Turn the “THC Span” selection valve to the choose the same balance gas as the intended sample gas, e.g. Helium)

4.13. Turn the “THC Zero” selection valve to the choose the same balance gas as the intended sample gas, e.g. Helium)

4.14. Light the flame

4.15. Set the “Flame Out Mode” switch to “Bypass”

4.16. Momentarily depress the “Igniter” button and observe the “Flame On” and “Flame Out” lights.

4.17. If the “Flame On” light is illuminated, proceed with the next steps. If not, adjust the “FID Air” regulator and try to light the flame until the flame lights and stays lit.

4.18. Set the “Flame Out Mode” switch to “Operate”. This mode protects the instrument in case the Air cylinder becomes empty. If the Air runs out and the “Flame Out Mode” switch is in the “Bypass” mode, pure Hydrogen will vent into the instrument case and the lab. This can form an explosive atmosphere.

4.19. Calibrate the THA

4.20. Set the “Purge” “Sample” selection valve on the sample selection panel to “Sample”.

4.21. Set the “SC-1”, “SC-2”, “Zero”, ”Span” selection valve on the sample selection panel to the “Zero” position, if so equipped.

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4.22. Verify that the “FID” “Samp” pressure in the THA instrument maintains the desired pressure. Adjust the sample needle valve on the sample selection panel, as necessary, to maintain the desired sample pressure.

4.23. When the reading stabilizes, adjust the “Course Zero” and “Fine Zero” knobs on the THA instrument until the display indicates the same value as reported on the zero gas certificate of analysis.

4.24. Set the “SC-1”, “SC-2”, “Zero”, ”Span” selection valve on the sample selection panel to the “Span” position.


4.26. When the reading stabilizes, adjust the “Span” knob on the THA instrument until the display indicates the same value as reported on the span gas certificate of analysis.

4.27. Continue to alternately adjust the zero and span settings, as above, until no further adjustment is necessary in either position. The zero reading should be maintained within 0.1 ppm of the certified zero concentration and the span reading should be maintained within 2% of the certified span concentration (19.6 ppm to 20.4 ppm). If the zero and span reading fall within these ranges, no further adjustment is necessary.

4.28. Analyze the sample gas

4.29. Set the “SC-1”, “SC-2”, “Zero”, ”Span” selection valve on the sample selection panel to the “SC-1” or “SC-2” position according to the position of the sample gas you intend to analyze.


4.31. When the reading stabilizes, read the THA display. This indicates the concentration of Total Hydrocarbons in the sample gas.

4.32. Record the reading on the quality assurance record.

4.33. Place the instrument in stand-by mode

4.34. Set the “Purge” “Sample” selection valve on the sample selection panel to “Purge ”.

4.35. Close the fuel gas, air, zero and span

5. REFERENCES Total Hydrocarbon Analyzer manual

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 5.8 Baseline 8800 Total Hydrocarbon Analysis

1. OBJECTIVE This procedure establishes the analytical steps for the Baseline 8800 Total Hydrocarbon Analyzer. 2. SCOPE This procedure applies to the PurityPlus specialty gases lab. 3. RESPONSIBILITIES


4. PROCEDURE

4.1. Setup: Set the support gas regulators as follows:

4.1.1. Fuel – 20 psi

4.1.2. Air – 20 psi

4.1.3. Sample – 20 psi

4.1.4. THA Zero – 20 psi (using the same balance gas as the intended sample gas, e.g. Helium Zero)

4.1.5. THA Span – 20 psi (using the same balance gas as the intended sample gas, e.g. 20 ppm Methane in Helium)

4.2. Calibration Procedure

4.2.1. Apply the certified zero gas to the instrument.

4.2.2. Wait for the reading to stabilize. If the instrument does not indicate the certified value of the cylinder, then adjust reading until the instrument reading agrees with the certified concentration in the cylinder.


4.2.4. Wait for the reading to stabilize. If the instrument does not indicate the certified value of the cylinder, then adjust reading until the instrument reading agrees with the certified concentration in the cylinder.

4.2.5. Repeat the calibration steps, above, until the zero and span gas cylinder indicate the certified values within 0.1 ppm.


4.2.7. This process should be repeated each day the instrument is used.






5. REFERENCES Series 8800 Continuous Analyzer User’s Manual Rev. C 4/28/97

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 5.9 Cycle Purge Procedure

1. OBJECTIVE

This procedure establishes the steps to assure the sample flowing through a regulator is representative of the gas in the cylinder.

2. SCOPE This procedure applies to the PurityPlus specialty gases lab. 3. RESPONSIBILITIES


4. PROCEDURE

4.1. Cycle purge the regulator and sample line by:

4.2. Connect the regulator and sample line to the sample cylinder and the instrument (or panel) to be used.

4.3. Carefully open the sample cylinder valve until the regulator pressurizes.

4.4. Close the sample cylinder valve

4.5. Wait until the regulator low pressure gauge indicates 0 psig.

4.6. Repeat these steps for a total of five cycles. Leave the cylinder valve open after the fifth cycle.

5. REFERENCES None

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 5.10 Gas Chromatograph Analysis

1. OBJECTIVE

This procedure establishes the steps to document a gas chromatograph system suitability, calibration and analysis.

2. SCOPE This procedure applies to the PurityPlus specialty gases lab using Chrom Perfect data acquisition software and a gas chromatograph.


4. PROCEDURE

4.1. Select the appropriate GC method for the analysis. Assure the gas chromatograph parameters have stabilized at the approved settings before proceeding.

4.2. Assure the correct System Suitability/Calibration gas is cycle purged through the sample system.

4.3. Start Chrom Perfect using the Chrom Perfect procedure.

4.4. Complete the Gas Chromatograph System Suitability/Calibration/Analysis Worksheet

5. REFERENCES See the following Gas Chromatograph System Suitability/Calibration/Analysis Worksheet.

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Quality Assurance Program Rev. 15 April 2012 Rev #: 2.1 Document Title: 5.11 Gas Chromatograph System Suitability/Calibration/ Analysis Worksheet

GC Method No: Actual GC parameters at the time of analysis: GC Parameter Actual Value GC Parameter Actual Value

Gas Chromatograph Carrier Gas Flowrate (ml/min)

Integrator

Detector Type (TCD, FID, DID, etc.)

q TCD q FID q DID q Other:_____

Integration Method (ESTD, ISTD, Norm)

External Standardization (ESTD)

Detector Temperature (deg. C)

Column

Detector Current (mA)

Column Oven Temperature (deg. C)

Attenuation

Carrier Gas (Helium, Argon, etc.)

q Helium q Other:_____ q Argon

Range (DID/FID only)

System Suitability Summary Worksheet Attach all chromatograms to this worksheet. System Suitability Parameter Result Satisfactory?

1 Precision Worksheet – Enter the Relative Standard Deviation (%RSD) of the area counts of the peak of interest in the cell to the right. The %RSD must be less than or equal to 2% for this step of the System Suitability to be satisfactory. The peak of interest must also have been correctly identified on the chromatogram for this step to be satisfactory.

q Satisfactory

q Unsatisfactory

2 Resolution - Enter the Resolution between the peak of interest (checked above) and the closest peak on the first chromatogram using the system suitability gas. The Resolution must be equal to or greater than 2.0 for this step of the System Suitability to be satisfactory.

q Satisfactory

q Unsatisfactory

3 Column Efficiency – Enter the Theoretical Plates from the minor component of the first injection in the cell to the right. The Theoretical Plates must be greater than 1500 for this step of the System Suitability to be satisfactory.

q Satisfactory

q Unsatisfactory 4 Unidentified Components - Are there any unidentified peaks? Be aware that the

injection upset may look like a peak. It will be a small upset just after injection. Examine the peaks and injection upsets to assure that there are no unidentified peaks. This answer must be “NO” for this step of the System Suitability to be satisfactory.

q Yes

q No

q Satisfactory

q Unsatisfactory

5 Unstable Baseline – The baseline should be interpreted by the integration software without omitting minor components in the system suitability chromatograms. Were all minor components identified and quantified? This answer must be “Yes” for this step of the System Suitability to be satisfactory.

q Yes

q No

q Satisfactory

q Unsatisfactory

6 Minimum Peak Height – Can the Peak Height of the peak of interest in the system suitability gas be scaled on the screen to greater than 70% of the chart width? This answer must be “Yes” for this step of the System Suitability to be satisfactory. The report may scale the peak differently.

q Yes

q No

q Satisfactory

q Unsatisfactory

7 Overall System Suitability – Are all the steps above satisfactory? If all steps are satisfactory the System Suitability is satisfactory. If any step above fails, then the System Suitability is unsatisfactory and the chromatographic system must be corrected before an analysis can be considered valid.

q Yes

q No

q Satisfactory

q Unsatisfactory

Analytical Results: Standard: Cylinder No.: Expiration Date: Sample: Cylinder No.: Lot Number: Tester: Date: Reviewed and Approved By: Date:

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 5.12 Authorized Gas Chromatograph Methods

1. OBJECTIVE This procedure establishes the authorized analytical methods for gas chromatographs. 2. SCOPE This procedure applies to the PurityPlus specialty gases lab. 3. RESPONSIBILITIES


4. PROCEDURE 4.1. Enter the location. 4.2. Enter the gas chromatograph method number. 4.3. Enter the component being analyzed, and in what mixture. 4.4. Enter the name of the gas chromatograph being used. 4.5. Enter the name of the integrator used. 4.6. Enter the integration method. 4.7. Enter the column specifications. 4.8. Enter the column (oven) temperature. 4.9. Enter the name of the carrier gas used. 4.10. Enter the carrier gas flow rate. 4.11. Enter the detector type. 4.12. Enter the detector temperature. 4.13. Enter the detector current (TCD only). 4.14. Enter the attenuation. 4.15. Enter the electrometer range (FID/DID only). 4.16. Enter the signature of the person the method was developed by, and the date. 4.17. Enter the signature of the person approving the method, and the date. The approver must be a

member of the Quality Control Unit. 4.18. Enter the date the method was instituted. 4.19. When the GC analytical method is retired, enter the date the method was retired.

5. REFERENCES See the attached GC Method Authorization Form

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 5.13 GC Method Authorization

Location: GC Method No:

Analysis of component(s) in

See reverse side for additional components analyzed by this method

GC Parameter Actual Value GC Parameter Actual Value Gas Chromatograph Carrier Gas Flowrate

(ml/min)

Integrator

Detector Type (TCD, FID, DID, etc.)

q TCD q FID q DID q Other:_____

Integration Method (ESTD, ISTD, Norm)

External Standardization (ESTD)

Detector Temperature (deg. C)

Column (Type and dimensions)

Detector Current (TCD only - mA)

Column Oven Temperature (deg. C)

Attenuation

Carrier Gas (Helium, Argon, etc.)

q Helium q Other:_____ q Argon

Range (DID/FID only)

Sample Flow (ml/min)

Other:

Attach a sample chromatogram to this form.

Method developed by: Date:

Method approved by: Date:

Method instituted (date):

Method retired (date):

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Quality Assurance Program Rev. 24 Feb 2011 Rev #: 1 Document Title: 5.14 EZ Chrom Procedures

1. OBJECTIVE

1.1. To describe fundamental elements of the activities performed in order to analyze a high-pressure compressed gas mixture.

2. SCOPE 2.1. Approved non-liquefied, toxic, corrosive, reactive or fuel/oxidizer gas blends, using the

GOW-MAC 580 DID Gas Chromatograph.

3. RESPONSIBILITIES 3.1. Overview: It is the responsibility of all laboratory personnel to ensure that these instructions

are safely performed as described; this LWI will be reviewed and updated as necessary. All applicable personnel will maintain the proper support documentation and any records accompanying the product produced, as described in this manual.

4. PROCEDURE 4.1. Prerequisites: Ensure that conditions on the GC METHOD AUTHORIZATION FORM for

the applicable method are in effect. 4.2. Activate Client

4.2.1. On Desktop Taskbar, left click on EZChrom Elite icon. 4.2.2. On the EZChrom Elite Client/Server window, double left click the GC icon 4.2.3. A previous chromatogram may be displayed. This can be closed by left clicking the red X 4.2.4. In the Select channel dropdown field, verify the correct channel is selected.

4.3. Calibration 4.3.1. In the Menu Bar, left click on File, Method, Open… 4.3.2. In the Open Method File screen, select the applicable Method.met file 4.3.3. Left click on the file icon to select it and then click on Open button. 4.3.4. Click on the Blue Arrow indicating a Single Run 4.3.5. Edit/Verify Sample/File information and data paths, RUN 4.3.6. The bottom of the main window will show that the Method is being downloaded; then verify the

“Waiting For Trigger…” message at the bottom of the window before making the injection. 4.3.7. Connect the appropriate Certified Calibration gas cylinder to the GC sample system. 4.3.8. Verify pressure is [per SOP]. Adjust regulator and valve as needed. 4.3.9. Cycle-purge line by opening and closing cylinder valve, allowing the pressure heard leaving the

Purge valve outlet to go to zero before re-opening and closing the cylinder valve. Repeat four times for a total of five cycles. On the last cycle, leave the cylinder valve open and move the Sample Line Purge valve to the sample position.

4.3.10. Start the GC Run. 4.3.11. At the end of the run, a chromatogram and report will print. 4.3.12. Enter the component of interest (e.g. Carbon Monoxide) area count in the %RSD data sheet

for the five runs for each component of interest. The acceptability limit is to not exceed 2%RSD for any component of interest.

4.3.13. The data sheet will also provide the Response Factor (RF) that can be manually placed into the Peak Table in lieu of an automated Calibration

4.4. Sample 4.4.1. Click on the Blue Arrow indicating a Single Run

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4.4.2. Edit/Verify Sample/File information and data paths, RUN 4.4.3. The bottom of the main window will show that the Method is being downloaded; then verify the

“Waiting For Trigger…” message at the bottom of the window before making the injection. 4.4.4. Connect the appropriate Certified Calibration gas cylinder to the GC sample system. 4.4.5. Verify pressure is [per SOP]. Adjust regulator and valve as needed. 4.4.6. Cycle-purge line by opening and closing cylinder valve, allowing the pressure heard leaving the

Purge valve outlet to go to zero before re-opening and closing the cylinder valve. Repeat four times for a total of five [or per SOP] cycles. On the last cycle, leave the cylinder valve open and move the Sample Line Purge valve to the sample position.

4.4.7. Start the GC Run. 4.4.8. At the end of the run, a chromatogram and report will print.

5. REFERENCES 5.1. None

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 5.15 Chrom Perfect System Suitability, Calibration and Analysis

1. OBJECTIVE

This procedure establishes the steps to perform a System Suitability and Calibration on a gas chromatograph using Chrom Perfect software.



4. PROCEDURE 4.1. Initial instrument setup. Refer to the method documentation for the correct settings for the

following gas chromatograph settings: column material, column dimensions, column temperature, detector temperature, range (if applicable), carrier gas, carrier gas flow, detector flow (if applicable), auxiliary flows (if applicable), purge flow (if applicable), aux. carrier flow (if applicable), attenuation, detector current (if applicable), detector polarity (if applicable), sample flowrate, etc.

4.1.1. Verify that the Sample/System Suitability System Suitability gas is flowing through the gas sample valve a the specified flow.

4.1.2. Turn on the computer. 4.1.3. Double click on the ChromPerfect icon to bring up the ChromPerfect Main Menu. 4.1.4. Click the “Acquisition” button from the ChromPerfect Main Menu

4.1.5. Press the “Claim” button for the instrument to be used.

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4.1.6. Press the “Status” tab on the far right corner

4.2. First System Suitability and Calibration Run

4.2.1. Press the Remote Control button (or right click on the row of the instrument to be used.)

4.2.2. Press the download button (or select Download from the right click menu.)

4.2.3. Verify the appropriate method file is entered in the Method File box.

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4.2.4. Verify the sample name is blank. 4.2.5. Verify the Base Name is the Lot number and Serial Number of the cylinder being analyzed 4.2.6. Verify the sample name is under Heading 1 (e.g. 5% CO2 in N2) 4.2.7. Verify the analyst name is under Heading 2 (e.g. Rozwell Mason, Sr.) 4.2.8. Enter “1” in the “Cycle Number” box for the first injection of the series (base name.) 4.2.9. Make sure the “Calibration Replace” radio button is checked for the “Type of Run” for the first

calibration run 4.2.10. Enter “1” for the Calibration Level” box 4.2.11. Press OK to download the file to Chrom Perfect 4.2.12. Verify the sample (calibration gas) is flowing through the flowmeter at specified flowrate.

Adjust as necessary. 4.2.13. Press “Start Run” on the remote control (or from the right-click menu)

4.3. Second System Suitability and Calibration Run 4.3.1. Press the Remote Control button (or right click on the row of the instrument to be used.) 4.3.2. Press the download button (or select Download from the right click menu.) 4.3.3. Verify the appropriate method file is still entered in the Method File box. 4.3.4. Verify the “Sample Name”, Base Name, Heading 1 and Heading 2 are entered as specified,

above. (This should not require editing.) 4.3.5. The “Cycle Number” should be 2 4.3.6. Press the “Calibration Average” radio button to check for the type of run for the second

calibration run 4.3.7. Verify “1” is entered for the Calibration Level” box. (This should not require editing.) 4.3.8. Press OK to download the file to Chrom Perfect 4.3.9. Verify the sample (calibration gas) is flowing through the flowmeter at specified flowrate.

Adjust as necessary. 4.3.10. Press “Start Run” on the remote control (or from the right-click menu).

4.4. Third, Fourth and Fifth System Suitability and Calibration Runs 4.4.1. Press “Start Run” on the remote control (or from the right-click menu). 4.4.2. Note that the amounts on the report will not be exactly correct according to the calibration

runs. This is normal. If you want to see the report with the correct calibration data, press the “Analysis” button on the ChromPerfect Main Menu. Select the file and run the “Fixed Long Form” from the report menu of the Analysis Module.

4.5. Chromatogram interpretation 4.5.1. Evaluate the precision for the area counts on the peaks of interest. Precision <= 2% RSD is a

typical acceptance criteria. (Higher precision RSD acceptance criteria may be necessary on very low ppm calibrations. Deviations from this acceptance criteria must be approved on the GC Method Authorization or deviation form.)

4.5.2. Proper integration – verify that the peaks and baseline are interpreted properly on the calibration chromatograms.

4.5.3. Resolution – verify that the resolution between peaks of interest is greater than 2.0. 4.5.4. Complete the Gas Chromatograph System Suitability/Calibration/Analysis Worksheet.

4.6. Analysis Procedure 4.6.1. Press the Remote Control button (or right click on the row of the instrument to be used.) 4.6.2. Press the download button (or select Download from the right click menu.) 4.6.3. Verify the appropriate method file is still entered in the Method File box. 4.6.4. Verify the “Sample Name”, Base Name, Heading 1 and Heading 2 are entered as specified,

above. (This should not require editing.) 4.6.5. Press the “Analysis” radio button. 4.6.6. Press OK to download the file to Chrom Perfect 4.6.7. Verify the sample gas is flowing through the flowmeter at specified flowrate. Adjust as

necessary. 4.6.8. Press “Start Run” on the remote control (or from the right-click menu). 4.6.9. Run three replicate chromatograms of the sample gas. Calculate the precision. The precision

should be less than 2% RSD. If the precision does not meet this acceptance criteria, check for leaks and fully purged sample lines. Repeat the three replicates as necessary.

4.6.10. Keep all chromatograms with the analytically paperwork. Document any investigations and anomalies on the chromatogram.

4.6.11. Sign all chromatograms. The signature on the chromatogram indicates that this is a true and original paper copy of an electronic record. The signature creates a hybrid electronic record.

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4.6.12. Average the three replicate concentrations and report this value as the concentration of the gas being analyzed.

5. REFERENCES GC Method Authorization Gas Chromatograph System Suitability/Calibration/Analysis Worksheet

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 5.16 GOW-MAC Discharge Ionization Detector Setup

1. OBJECTIVE

This procedure establishes the setup parameters for the GOW-MAC Discharge Ionization Detector Gas Chromatographs.

2. SCOPE This procedure applies to the PurityPlus specialty gases lab using the GOW-MAC DID. 3. RESPONSIBILITIES


4. PROCEDURE 4.1. For the GOW-MAC 590 DID – System 1, set the flows and temperatures as follows: 4.2. For normal operation:

Purge flow - between 5 and 30 ml/min (measured at “Purge Out”) Auxiliary Carrier flow - between 5 and 30 ml/min (measured at “Vent”) Carrier flow - between 30 and 40 ml/min (measured at “Detector Out” with the Discharge flow off) Detector (Discharge) flow - between 10 and 20 ml/min (measured at “Detector Out” – added to the Carrier flow) Sample flow - between 10 and 20 ml/min Column Oven Temperature - between ambient and 100 deg C, depending on the analysis Detector Oven Temperature – Set as low as possible. The temperature will “float’ with the column oven temperature. Attenuator – Set at 1 Range – Set at 10 -11 for low ppm analyses. Set at 10 -9 for high ppm analyses GOW-MAC Helium Purifier – Set at 350 deg C until the purifier heater generates periodic anomalies (“blips”) on the chromatogram. Then raise the temperature another 50 deg C. (max 450 deg C). Order a replacement purifier cartridge when you begin to see the anomalies.

4.3. For conditioning (“Bake-Out”), use the following settings overnight, or longer as needed: Column Oven Temperature - 120 deg C Detector Oven Temperature – 120 deg C GOW-MAC Helium Purifier – Set at 50 deg C over the normal operation (max 450 deg C)

5. REFERENCES See the following GOW-MAC DID Gas Chromatograph Manual.

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 5.17 Analyzers Not Listed in the Manual

These work instructions give instructions for most analyzers; however, it does not give instructions for every analyzer in use. For example, because the instructions for gas chromatographs are specific to model number and detector type, there are within too many variations to cover each one in the manual.

When an analyzer is not listed in the manual, follow the manufacturer’s instructions for operation, calibration (including frequency), and maintenance.

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 5.18 Taylor OA 224 Oxygen Analyzer

1. OBJECTIVE

This procedure describes the Taylor OA 224 Oxygen Analyzer.



4. PROCEDURE 4.1. PREPARATION FOR TEST

4.1.1. Caution: Over-pressurization can damage the measuring cell of this instrument. Pressure regulation and suitable pressure relief devices must be provided for any gases supplied from high-pressure cylinders. Pressure of gases supplied to the instrument must not exceed 10 psig.

4.1.2. The following gases must be supplied to the instrument: 4.1.2.1. Zero Gas – high purity dry nitrogen with a minimum purity of 99.997%. 4.1.2.2. Span Gas – high purity oxygen with a minimum purity of 99.5%. The purity of this gas

must be known and should be indicated on the analyzer CALBRATION GAS decal. 4.1.3. Both sample and span gases must be introduced to the analyzer at the same pressure, within

1 psig. 4.1.4. Prior to final calibration, the analyzer must, with the power on, come to final equilibrium at the

ambient temperature at which it will be used. 4.1.5. Any tubing attached to the vent connection must be properly sized to minimize pressure drop

at a sample flowrate of 5 liters/min. 4.1.6. During extreme changes in barometric pressure, frequent calibration will be required. 4.1.7. If the analyzer is in continuous use, the filter element should be checked for moisture and dirt

once a month. 4.1.8. The analyzer must not be operated without the filter element in place. 4.1.9. The Sample/Selector valve should be in the OFF position when no gas is flowing through the

analyzer. 4.2. TEST PROCEDURE

4.2.1. Switch the power ON. The Power Light should come on. 4.2.2. Turn the Sample/Standard selector valve to OFF.

4.2.2.1. Caution: Over tightening the Flow Knob may damage the valve seat, valve needle or both, causing erratic control of the flow of the sample and reference gases.

4.2.3. Close the Flow Valve on the front of the analyzer. 4.2.4. Close the By-pass Valve on the back of the analyzer. 4.2.5. Connect the Zero Gas supply to the Sample Inlet fitting and the Span Gas supply to the

Standard Inlet filling on the back of the analyzer. 4.2.6. Adjust the pressure reducing regulator on each gas supply to 5 + 1 psig. 4.2.7. Turn the Sample/Standard Valve to SAMPLE. 4.2.8. Open the By-pass Valve on the back of the analyzer until you obtain a by-pass flow of 2

liters/min. 4.2.9. Open the Flow Valve on the front of the analyzer until the ball of the sample flowmeter is

within + 2 mm of the mark on the flow tube. This corresponds to a flow rate of approximately 50 ml/min.

4.2.10. Hold the Range Switch to the “0-100%” position. When the output meter reading has stabilized, adjust the N2 Zero so that the meter reads 0%. Release the Range Switch.

4.2.11. Switch the Sample/Standard Selector Valve to STANDARD. 4.2.11.1. Note: The by-pass flow should still read 2 liters/min.

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4.2.12. Adjust the Flow Valve on the front of the analyzer until the ball of the sample flowmeter is within + 2 mm of the mark on the flow tube (corresponding tot eh 50 ml/min).

4.2.13. When the reading of the output meter has stabilized, adjust the Coarse and Fine Knobs so that the meter reading indicates the known purity of the Span Gas.

4.2.14. Turn the Sample/Standard selector valve to OFF. 4.2.15. Remove the nitrogen Zero Gas from the Sample Inlet. 4.2.16. Connect the Sample Gas to the Sample Inlet fitting on the back of the analyzer. Adjust the

pressure reducing regulator on the sample gas line to 5 + 1 psig (the same pressure as the sample gas, within + 1 psig).

4.2.17. Turn the Sample/Standard Valve to SAMPLE. 4.2.18. Adjust the Flow Valve on the front of the analyzer until the ball of the sample flowmeter is

within +2 mm of the mark on the flow tube (corresponding to 50 ml/min). 4.2.19. Allow the output meter to stabilize and read the purity of the Sample Gas. 4.2.20. Turn the Sample/Standard Selector Valve to the OFF position.

4.3. EQUIPMENT CALIBRATION 4.3.1. The accuracy of the instrument is dependent upon the ability to repeat the conditions of the

zero and span gases. The analyzer zero should be check once a week, after transportation, or if the analyzer has undergone a temperature change of 18 °F (10°C) or more. The analyzer span is calibrated prior to use using a Span Gas.

4.3.2. The span gas may also be a cylinder tested and certified by the plant using a Portable Oxygen Analyzer. Only this first-generation calibration cylinder or a second-generation plant certified cylinder (an acceptable National Bureau of Standards procedure) may be used as the span gas.

4.3.3. The zero and span gas cylinders are prepared and analyzed under laboratory conditions using accepted industry practices and standards traceable to the National Institute of Standards Technology (NIST) – formerly the National Bureau of Standards.

4.3.4. This test method is equal in accuracy and reliability to the USP/NF method. 5. REFERENCES

GENERAL DESCRIPTION The Taylor OA 244 oxygen analyzer is a transportable analyzer designed for use in determining the purity of gaseous oxygen from 98-100% purity. It is used to compare the purity of the sample gas to that of a span gas of known purity. The purity of the span gas has been accurately determined by an absolute method of analysis.

THEORY The paramagnetic susceptibility of oxygen is significantly greater than that of other common gases. This means that oxygen molecules are attracted much more strongly by a magnetic filed than are molecules of other gases, most of which are slightly diamagnetic (repelled by a magnetic field). The operation of magneto-dynamic oxygen analyzers is based on Faraday’s method of determining the magnetic susceptibility of a gas by measuring the force developed by a strong, non-uniform magnetic field on a diamagnetic test body suspended in the sample gas.

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 5.19 MEECO Gemini Plus Analyzer

1. OBJECTIVE

This procedure describes the MEECO Gemini Plus Analyzer.




4.1.1. Use only small diameter (1/8 in OD) stainless steel tubing for sample lines. 4.1.1.1. This reduces purge time and provides a fast, stable response.

4.1.2. Always use a metal diaphragm regulator for pressure regulation. 4.1.2.1. Do not use a composition diaphragm regulator. 4.1.2.2. Warning: pressure regulation and suitable pressure relief devices must be provided when

high-pressure cylinders are used. 4.1.3. Use an all-metal sampling system. 4.1.4. Keep sampling lines as short as possible. Eliminate all unnecessary tubing bends, fittings,

and dead legs. 4.1.5. Thorough purging of the sample lines is essential for start-up. 4.1.6. Because trace quantities of oxygen must be detected, the system must be free of all leaks. 4.1.7. All necessary hardware and fittings upstream of the analyzer should be leak tested under

pressure prior to startup. 4.1.8. A sample flowrate of 2.0 scfh must be maintained for the oxygen analyzer in order to obtain

an acceptable response time. 4.1.9. The oxygen analyzer should not be used in applications where oxygen is a major component

of the sample. 4.1.10. Mount the instrument in a 19-inch rack or use as a free-standing unit 4.1.11. The span gas required for the Trace Oxygen Analyzer is an 8-10 ppm oxygen, balance

nitrogen standard. 4.1.12. The Trace Oxygen Analyzer has a absolute zero. 4.1.13. The Gemini Plus Moisture Analyzer is designed to compensate for the recombination effect.

When the Select/Normal switch is in the SELECT (or up) position, the analyzer compensates for the recombination of oxygen at low-ppm moisture levels.

4.1.13.1. Note: In the Gemini Plus units supplied with an OLR cell, the Select/Normal switch compensation factor has been calculated for oxygen sampling. The switch should be turned to SELECT when the reading is in the NORMAL position is 3 ppm or lower.

4.1.14. Sample pressure may effect recombination in the moisture analyzer. The moisture analyzer contains an internal high purity gas pressure regulator that maintains a 3 psi pressure within the electrolytic cell when the inlet pressure is higher than 3 psi. contact MEECO if you are measuring moisture in oxygen at pressures under 3 psi. the compensation factor 13, above) will be incorrect at pressures below 3 psi.

4.2. TEST PROCEDURES 4.2.1. Moisture Analyzer

4.2.1.1. Note: The oxygen Select/Normal switch is used to obtain a direct readout of water in oxygen. When determining water in oxygen, make certain the Select/Normal switch is in the SELECT (up) position and that the light indicating the oxygen mode is on.

4.2.1.2. Warning: Make sure that the proper pressure regulation and safety relief device are provided.

4.2.1.2.1. Close all valves on the analyzer.

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4.2.1.2.2. Connect the sample line to the sample inlet. 4.2.1.2.3. Turn the Moisture Unit power on. 4.2.1.2.4. Purge the inlet system for about 2 minutes by opening the By-Pass Flow Control

to a flow setting of 1-2 scfh (500 to 1000 sccm). 4.2.1.2.5. Introduce the Sample Gas to the analyzer by opening the Sample Adjust H20

Valve slowly and permitting a minimum quantity (50 sccm or less) of gas to flow through the cell.

4.2.1.2.5.1. Note: The flow should be increased at a rate to allow the meter to maintain an on-scale (less than 19.99 ppm) reading.

4.2.1.2.6. Sample Adj (H20) Valve for proper flowrate, using Table 1. 4.2.1.2.7. Read the ppm H20 Meter when it has stabilized.

Table 1 – Sample Flow Controller Rates Gas Flow Controller Setting (cc/min)

Air 100 Argon 69 Helium 69 Hydrogen 100 Nitrogen 100 Oxygen 100

4.2.2. Oxygen Analyzer

4.2.2.1. Turn the Oxygen Unit power on and observe the PPM O2 Meter display. 4.2.2.2. Select the 25% range. 4.2.2.3. Wait until the PPM O2 Meter comes to equilibrium.

4.2.2.3.1. If the meter indicates a value close to 20.9%, the Cell Shut-Off Valve was probably left open. If so, it will take longer to obtain a low-ppm reading.

4.2.2.4. Open the Cell Shut-Off Valve, located on the rear panel of the unit, FIRST. 4.2.2.5. Open the Sample Flow (O2) Valve and adjust it until the flowmeter indicates a flow rate

of 2.0 scfh. 4.2.2.6. Move the Range switch to the appropriate range.

4.2.2.6.1. Note: The Over Range light will turn on at approximately 120% of the range value. Do not accept any values of the readout when the Over Range light is lit.

4.2.2.7. Record the results when the reading has stabilized. 4.2.2.8. Close the Sample Flow (O2) Valve completely. 4.2.2.9. Close the Cell Shut-Off Valve. 4.2.2.10. Disconnect the Sample Gas input.

4.2.2.10.1. The output indication will eventually come to equilibrium somewhere on the 0-1000 ppm scale.

4.2.3. EQUIPEMENT RECALIBRATION – MOISTURE ANALYZER Bulk Gases facilities are required to perform a Cell Check and a Cell Moisture Check monthly. Packaged Gases locations are required to perform a Cell Check daily prior to use and a Cell Moisture Check monthly. 4.2.3.1. Cell Check

4.2.3.1.1. Push the Cell Check Button. When the Cell Check Button is depressed, the PPM H2O Meter becomes a volumeter.

4.2.3.1.2. Read the PPM H2O Meter. 4.2.3.1.3. A reading of less than 6.75 indicates that the cell may be shorted or

contaminated. The PPM H2O Meter must not read below 67.5. 4.2.3.1.4. Record this check on the Equipment Calibration Log.

4.2.3.2. Monthly Cell Moisture Check Electrolytic cells become desensitized with use. A desensitized cell will always give a false (low) moisture content reading, but may pass the Cell Check. Perform the following Cell Moisture Check once a month to ensure that the cell has not become desensitized. 4.2.3.2.1. Use a moisture Check Gas of 5-50ppm moisture gas.

4.2.3.2.1.1. Note: the Check Gas is NOT a calibration gas. It is simply a gas with low-ppm moisture.

4.2.3.2.2. Following the steps in the General Test Procedure, run a moisture test using the 5-50 ppm moisture Check Gas as a sample source.

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4.2.3.2.3. Check for a positive moisture indication. If there is no positive moisture indication, the cell is bad and must be replaced.

4.2.3.2.4. Record the results on the Equipment Calibration Log. 4.2.3.2.4.1. Note: At Packaged Gases locations a test cylinder that reads above 5 ppm

moisture may be used for the Monthly Cell Moisture Check if the results are recorded on the Equipment Calibration Log.

4.2.4. EQUIPMENT RECALIBRATION – OXYGEN ANALYZER When used as a process or quality assurance analyzer, the oxygen analyzer should be checked once a month for calibration. when used intermittently, as at a customer service location, the analyzer should be check prior to use.

4.2.4.1. Open the Cell Shut-Off Valve located on the rear panel of the unit. 4.2.4.2. Open the Sample Flow (O2) Valve to introduce the Span Gas to the analyzer. Adjust this

valve until the flowmeter indicates a flowrate of 2.0 scfh. 4.2.4.3. Move the Range switch to the ppm 10 scale. 4.2.4.4. Unlock and adjust the Span Knob until the PPM O2 Meter reads the oxygen content of

the Span Gas. Be sure the reading is stable, and then relock the Span Knob. 4.2.4.5. Record the results on the Equipment Calibration Log. 4.2.4.6. The instrument is calibrated using a known Primary Standard Reference Gas. 4.2.4.7. Reference gases are prepared and analyzed under laboratory conditions using accepted

industry practices and standards traceable to the National Institute of Standards and Technology (NIST).

5. REFERENCES

GENERAL DESCRIPTION The MEECO Gemini Plus Analyzer combines the refined electrolytic technology for sub-ppm water determination with the electrochemical technology for sub-ppm oxygen determination. Though these two components share a common plug, the trace water and trace oxygen units operate as separate entities having separate readouts. The user may operate the units separately or simultaneously, depending on requirements.

THEORY Moisture Analyzer The heart of all electrolytic hygrometers is a cell in which water from a sample stream is continuously absorbed and electrodes. A dc potential applied to each of the electrodes causes the electrolysis; the resulting hydrogen and oxygen gases are carried off by the sample stream. The electric current resulting from the dissociation is a measure of the moisture concentration in the sample stream. In practical use the electrical circuitry and the sample flow rate and temperature are so chosen that the moisture concentration can be read in sub-parts per million, by volume, directly on a readout meter.

Oxygen Analyzer The oxygen in the sample stream is sensed by a small fuel cell. Oxygen diffusion into the cell reacts chemically to produce an electrical current that is proportional to the oxygen concentration in the gas phase immediately adjacent to the sensing surface of the cell. The minute but linear signal produced by the cell is amplified by a two-stage solid state amplifier in which power consumption per stage is less than three milliwatts. This amplified signal is read out on a precision panel meter.

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 5.20 Meeco Aquamatic Plus Moisture Analyzer

1. OBJECTIVE

This procedure describes the Meeco Aquamatic Plus Moisture Analyzer.




4.1.1. Mount the instrument in a 19-inch rack or use as a free standing unit. 4.1.2. Use an all-metal sampling system. 4.1.3. Always use a metal diaphragm regulator for pressure regulation. 4.1.4. Do not use a composition diaphragm regulator. 4.1.5. Use only small diameter (1/8 in OD) stainless steel tubing for sample lines.

4.1.5.1. This reduces purge time and provides a fast, stable response. 4.1.5.2. Warning: Pressure regulation and suitable pressure relief devices must be provided when

high-pressure cylinders are used. 4.1.6. Keep sampling lines as short as possible. Eliminate all unnecessary tubing bends, fittings,

and dead legs. 4.1.7. Purge the sample lines thoroughly at startup. This is essential. 4.1.8. Continuously purge the sampling system and analyzer with dry gas, i.e., house nitrogen,

when they are not in use or cap the lines to prevent exposing the system to atmospheric air. 4.1.9. Set the Select/Normal switch. The Aquamatic Plus is designed to compensate for the

recombustion effect. When the Select/Normal switch is in the up (O2 or H2) position, the analyzer compensates for recombination of oxygen or hydrogen at low ppm moisture levels. In units supplied with an OLR cell the compensation factor has been calculated for oxygen sampling. In units supplied with an HLR cell the compensation factor has been calculated for hydrogen sampling.

4.1.9.1. Set the Select/Normal switch to the up position in either of the following cases: 4.1.9.2. For oxygen – when the reading in the NORMAL position is 3 ppm or lower. 4.1.9.3. For hydrogen – when the reading in the NORMAL position is 2 ppm or lower.

4.1.10. Contact MEECO if you are measuring moisture in oxygen or hydrogen at less than 3 psig inlet pressure.

4.1.11. The Aquamatic Plus contains an internal high-purity gas pressure regulator that maintains 3 psi within the electrolytic cell providing the inlet pressure is above 3 psig. The compensation factors of the Aquamatic Plus assume a sample pressure of 3 psig. When the inlet sample pressure is lower than 3 psig, the compensation factors are incorrect.

4.2. TEST PROCEDURES 4.2.1. Warning: Make sure that the proper pressure regulation and safety relief device are provided.

Do not operate the analyzer above 100 psig. 4.2.2. Close all valves on the analyzer. 4.2.3. Connect the sample line to the sample inlet. 4.2.4. Turn the power on. 4.2.5. Purge the inlet system for about 2 minutes by opening the bypass flow control to a flow

setting between 500 and 1000 sccm (1-2 scfh). 4.2.6. Introduce the sample tot eh analyzer by slowly opening the sample flow control valve and

permitting a minimum quantity (50 sccm or less) of gas to flow through the cell. 4.2.6.1. Note: The flow should be increased at a rate to allow the meter to maintain an “on scale”

(less than 19.99 ppm) reading.

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Gas Flow Control Setting (cc/min) Air 100

Argon 69 Helium 69

Hydrogen 100 Nitrogen 100 Oxygen 100

4.2.7. Adjust the Sample Valve for proper flow rate, using Table 1. 4.2.8. Read the meter when it has stabilized.

4.3. EQUIPMENT RECALIBRATION 4.3.1. Bulk Gases facilities are required to perform a cell check and a Cell Moisture Check monthly. 4.3.2. Packaged Gases locations are required to perform a Cell Check daily prior to use and a Cell

Moisture Check monthly. 4.3.3. Cell Check: When the Cell Check button is depressed the analyzer meter becomes a 0-10 v

volumeter. 4.3.3.1. Push the Cell Check button. 4.3.3.2. Read the meter. 4.3.3.3. A reading of less than 6.75 indicates that the cell may be shorted or contaminated. The

meter must not read below 6.75. 4.3.4. Monthly Cell Moisture Check: Electrolytic cells become desensitized with use. A desensitized

cell will always give a false (low) moisture content reading, but may pass the Cell Check. Perform the following Cell moisture Check once a month to ensure that the cell has not become desensitized.

4.3.4.1. Use a moisture check gas of 5-50 ppm moisture gas. 4.3.4.2. Note: The check gas is NOT a calibration gas. It is simply a gas with a 5-50 ppm

moisture. 4.3.4.3. Following the steps in the General Test Procedure, run a moisture test using the 5-50

ppm moisture check gas as a sample source. 4.3.4.4. Check for a positive moisture indication. 4.3.4.5. If there is no positive indication, the cell is bad and must be replaced. 4.3.4.6. Record the results on the Equipment Calibration Log. 4.3.4.7. At Packaged Gases locations a test cylinder that reads above 5 ppm moisture may be

used for the monthly cell check if the results are recorded on the Equipment Calibration Log.

5. REFERENCES

GENERAL DESCRIPTION The MEECO Aquamatic Plus Moisture Analyzer is an automatic analyzer used to read moisture content of gases directly in ppm. Its operation is based on the principle of electrolytic hygrometry.

THEORY The heart of all electrolytic hygrometers is a cell in which water from a sample stream is continuously absorbed and electrolyzed – dissociated into hydrogen and oxygen. The cell consists of a hygroscopic material deposited on inert electrodes. A dc potential applied to each of the electrodes causes the electrolysis; the resulting hydrogen and oxygen gases are carried off by the sample stream. The electric current resulting from the dissociation is a measure of the moisture concentration in the sample stream. In practical use, the electrical circuitry, sample flow rate, and temperature are so chosen that the moisture concentration can be read in sub-parts per million by volume, directly on a readout meter.

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 5.21 MEECO Model W Moisture Analyzer

1. OBJECTIVE

This procedure establishes the MEECO Model W Moisture Analyzer.




4.1.1. Use only small diameter (1/8 in. ODA), stainless steel tubing for sample lines. 4.1.1.1. This reduces purge time and provides a fast, stable response.

4.1.2. Warning: Pressure regulation and suitable pressure relief devices must be provided when high-pressure cylinders are used for sampling.

4.1.3. Always use a metal diaphragm regulator for pressure regulation. 4.1.3.1. Do not use a composition diaphragm regulator. 4.1.4. Use an all-metal sampling system. 4.1.5. Keep sampling lines as short as possible. Eliminate all unnecessary fittings and dead legs. 4.1.6. Avoid drastic temperature changes that may influence absorption and desorption of moisture. 4.1.7. Do not operate the analyzer at temperatures below 32°F. 4.1.8. Continuously purge the sampling system and analyzer with dry gas, i.e., house nitrogen,

when they are not in use, or cap the lines so as not to expose the system to atmospheric air. 4.2. TEST PROCEDURES

4.2.1. There are two test procedures: the Single-Flow Test Method and the Delta-Flow Test Method. 4.2.2. Procedure for Packaged Gases 4.2.3. Packaged gases personnel are to use the Delta-Flow Test Method when testing samples of the

following gases: • Air • Hydrogen • Oxygen

4.2.4. Packaged gases personnel are to use the Single-Flow Test Method for all other samples. 4.2.5. Procedure for Bulk Gases 4.2.6. Bulk gases personnel are to use the Single-Flow Test Method when testing samples of the

following gases: • Argon • Nitrogen • Oxygen – when using a MEECO in dedicated oxygen service with an O cell • Hydrogen – when using a MEECO in dedicated hydrogen service with an

RHS cell • Note: Proper functioning of the O or RMS cell should be verified by testing a

sample using both the Single and Delta-Flow methods. The results should be identical.

• Oxygen or Hydrogen – when testing the product to meet specifications and the value obtained is less than the required specification.

• Note: The actual moisture value is less than the value determined by the Single-Flow Method.

• Bulk gases personnel are to use the Delta-Flow Method when moisture values in oxygen or hydrogen do not meet specifications using the Single-Flow Method or to obtain a more accurate moisture value when testing oxygen or hydrogen.

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4.3. Single-Flow Test Method (NEP-1, NEP-PL-FPM, NEP-1 BRAVO) 4.3.1. Connect the sample line to the sample inlet. 4.3.2. Insert the battery or connect the analyzer to ac power. Select AC or BATT on the panel as

appropriate. 4.3.3. Warning: Pressure regulation and suitable pressure relief devices must be provided when high-

pressure cylinders are used for sampling. 4.3.4. Introduce the sample to the analyzer. 4.3.5. Adjust the Bypass Valve to indicate mid-scale on the Bypass Flow indicator. 4.3.6. Adjust the Sample Vale for proper flow rate, using Table 1. 4.3.7. Select the proper range switch position to bring the indicator meter on-scale. 4.3.8. Note: The Range Switch is calibrated in ranges of 10, 30, 100, 300, and 1000ppm viv. Use the

lower meter scale for the 30 and 300 positions and the upper scale for the 10, 100, and 1000 positions (applies to units with the analog meter only).

(Table 1 – Sample Flowrates for Analyzers with Flowmeters) Gas Indicated Flowrate 100

cc/min Air Equivalent Flowrate, Delta-Flow Method A 50 cc/min Air Equivalent

Flowrate, Delta-Flow Method B 200 cc/min Air Equivalent

Air 100.0 50 (preferred) 200 Argon 117.5 --- --- Butane 142.0 --- --- Carbon Dioxide 124.0 --- --- Carbon Monoxide 98.5 --- --- Chlorine 157.0 --- --- Ethane 102.0 --- --- Ethylene 99.0 --- --- Halocarbon 12 205.0 --- --- Halocarbon 22 173.0 --- --- Helium 37.0 --- --- Hydrogen 46.0 23 92 (preferred) Methane 74.5 --- --- Nitrogen 98.5 --- --- Oxygen 102.0 51 (preferred) 204 Propane 123.0 --- --- Propylene 121.0 --- --- Sulfur Dioxide 149.0 --- --- Note: The values listed in Table 1 are approximate. They apply only to Brooks flowmeters installed in the analyzer by the manufacturer. The analyzer is calibrated for air at 14.7 psig and 70°F with a 100-cc/min flowrate. For more accurate results: 1. Set the flowrate of the Sample Gas to 100 cc/min using a soapfilm flowmeter or an analog flow check. 2. Note the reading of the flowmeter on the analyzer. 3. Post this reading on the analyzer and use it in adjusting flowrate during subsequent tests.

4.3.9. Read the meter when it has stabilized. 4.3.10. Note: on analog meter units the Range Switch setting selected in Step 6 always gives the full

scale value of the meter reading. For example, with the Range Switch on 10 and the meter indicating full scale, the reading is 10ppm moisture. A few old analyzers have a meter that reads 0-1 ppm instead of 0-10 ppm. Multiply the meter reading by the Range Switch setting only when using an analyzer having a 0-1ppm meter.

4.4. Delta-Flow Test – Method A (NEP-1, NEP-PL-FPM, NEP-1 BRAVO) 4.4.1. Perform Steps 1 through 4 under the Single-Flow Test Method. 4.4.2. Perform Step 5 under the Single-Flow Test Method, using the 100 cc/min air equivalent flow

rate from Table 1. 4.4.3. Continue with Steps 6 and 7 under the Single-Flow Test Method. 4.4.4. Write down the reading obtained in Step 7 under the Single-Flow Test Method. 4.4.5. Repeat Step 5 under the Single-flow Test Method again, this time setting flow rate to the value

given for Delta Flow Method A in Table 1. 4.4.6. Repeat Steps 6 and 7 under the Single-Flow Test Method. 4.4.7. Subtract the second reading (Step 6) from the first (Step 3).

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4.4.8. Multiply the difference obtained in Step 7 by 2. The result is the true moisture content of the Sample Gas.

4.5. Delta-Flow Test – Method B (NEP-1, NEP-PL-FPM, NEP-1 BRAVO) 4.5.1. Perform Steps 1 through 4 under the Single-Flow Test Method. 4.5.2. Perform Step 5 under the Single-Flow Test Method, using the 100 cc/min air equivalent flow

rate from Table 1. 4.5.3. Continue with Steps 6 and 7 under the Single-Flow Test Method. 4.5.4. Write down the reading obtained in Step 7 under the Single-Flow Test Method. 4.5.5. Repeat Step 5 under the Single-flow Test Method again, this time setting flow rate to the value

given for Delta Flow Method B in Table 1. 4.5.6. Repeat Steps 6 and 7 under the Single-Flow Test Method. 4.5.7. Subtract the first (Step 3) from the second reading (Step 6).

4.6. Single-Flow Test Method (Aquamatic) 4.6.1.1. Close all valves on the analyzer. 4.6.1.2. Connect the sample line to the sample inlet. 4.6.1.3. Turn the power on. 4.6.1.4. Purge the inlet system for about 2 minutes by opening the bypass flow control to a flow

setting between 500 and 1000 sccm. 4.6.1.5. Warning: Pressure regulation and suitable pressure relief devices must be provided when

high-pressure cylinders are used for sampling. 4.6.1.6. Introduce the sample to the analyzer by opening the sample flow control valve slowly and

permit a minimum quantity (50 sccm or less) of gas to flow through the cell. 4.6.1.7. Note: The flow should be increased to allow the meter to maintain an on-scale (less than

19.99 ppm or 199.9 ppm) reading. 4.6.1.8. Adjust the Sample Valve for proper flow rate, using Table 1 or Table 2. Table 2 – Sample Flowrates for Aquamatic Analyzers Equipped with a Mass Flow Controller

Gas Flow Controller Setting (cc/min) Argon 69 Helium 69

Hydrogen 100 Nitrogen 100 Oxygen 100

4.6.1.9. Read the meter when it has stabilized. 4.7. Delta-Flow Test Method A (Aquamatic)

4.7.1. Perform Steps 1 through 5 under the Single-Flow Test Method. 4.7.2. Perform Step 6 under the Single-Flow Test method, using the 100 cc/min air equivalent flow

rate from Table 1 or Table 2. 4.7.3. Continue with Step 7 under the Single-flow Test Method. 4.7.4. Write down the reading obtained in Step 7 under the Single-flow Test Method. 4.7.5. Repeat Step 6 under the Single-Flow Test Method again, this time setting flow rate to the value

given for Delta Flow Method A in Table 1 or by halving the flow controller rate specified in Table 2.

4.7.6. Repeat Step 7 under the Single-Flow Test Method. 4.7.7. Multiply the difference obtained in Step 7 by 2. The result is the true moisture content of the

Sample Gas. 4.8. Delta-Flow Test Method B (Aquamatic)

4.8.1. Perform Steps 1 through 5 under the Single-Flow Test Method. 4.8.2. Perform Step 6 under the Single-Flow Test method, using the 100 cc/min air equivalent flow

rate from Table 1 or Table 2. 4.8.3. Continue with Step 7 under the Single-flow Test Method. 4.8.4. Write down the reading obtained in Step 7 under the Single-flow Test Method. 4.8.5. Repeat Step 6 under the Single-Flow Test Method again, this time setting flow rate to the value

given for Delta Flow Method B in Table 1 or by halving the flow controller rate specified in Table 2.

4.8.6. Repeat Step 7 under the Single-Flow Test Method. 4.8.7. Subtract the first reading (Step 3) from the second (Step 6). The result is the true moisture

content of the Sample Gas.

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4.9. EQUIPMENT CALIBRATION 4.9.1. Air Separation Plants and Bulk Gas Customer Service Centers are required to perform a Cell

Check, DC Power Check (not applicable for the Aquamatic), and a Cell Moisture Check monthly.

4.9.2. Packaged Gases Plants are required to perform a Cell Check and DC Power Check daily prior to use (not applicable for the Aquamatic), and a Cell Moisture Check monthly.

4.9.3. Cell Check 4.9.3.1. When the Cell Check button is depressed, the analyzer meter becomes a voltmeter. 4.9.3.2. Push the Cell Check button. 4.9.3.3. Read the meter.

For NEP-1, NEP-PL-FPM (Analog Meter) • An off-scale reading indicates the

cell is dry and the analyzer is ready for use.

• A reading of 2 to 10 v indicates the cell may be wet.

• A reading of less than 2.0 v indicates the cell may be shorted or contaminated.

For Aquamatic, NEP-1 Bravo (Digital Meter) • A reading of less than 67.5 indicates that

cell may be shorted or contaminated. The meter must not read below 67.5 or 6.75. Note that the placement of the decimal point makes no difference.

4.10. DC Power Check 4.10.1. Note: The DC power check does not apply to the Aquamatic. 4.10.2. When the DC Power Check button is depressed, the analyzer meter becomes a 0-100 v

voltmeter. 4.10.3. Set the Range Switch to the X1000 position. 4.10.4. Push the DC Power Check button. 4.10.5. read the meter

4.10.5.1. A reading of 70 + 5 v indicates the cell is dry and the analyzer is ready for use. 4.10.5.2. Note: a reading of more than 75 v may indicate a malfunctioning voltage regulator.

Have it check by a qualified servicer. 4.10.5.3. A reading between 20 and 65 v indicates the cell is good, but wet. Dry it using the

procedure given later in this item. 4.10.5.4. A reading of less than 2.0 v indicates that the cell may be shorted or contaminated.

Check it for these conditions using the procedure given later in this item 4.11. Drying a Wet Cell

4.11.1. Turn the analyzer power on. 4.11.1.1. Note: a wet cell with result in incorrect reading. The cell will not dry unless current is

applied to it. 4.11.2. Purge the cell with dry gas.

4.12. Checking for a Shorted or Contaminated Cell 4.12.1. Note: This procedure is not applicable for the Aquamatic. 4.12.2. Turn the analyzer power off. 4.12.3. Unplug the analyzer (if using ac power). 4.12.4. Measure the resistance across the cell with a volt-ohm meter.

4.12.4.1. A reading of 1000 ohms to 1 megohm indicates a good cell. 4.12.4.2. A reading of less than 1000 ohms indicates a shorted or contaminated cell. If the

reading is 70 ohms or less, the cell is definitely bad and must be replaced. 4.13. Monthly Cell Moisture Check

4.13.1. Electrolytic cells become desensitized with use. A desensitized cell will always give a false (low) moisture content reading, but may pass the daily Cell Check.

4.13.2. Perform the following Cell Moisture Check once a month to ensure that the cell has not become desensitized:

4.13.3. Use a moisture check gas of 5-50 ppm moisture gas. 4.13.3.1. Note: the check gas is NOT a calibration gas. It is simply a gas with 5-50 ppm

moisture. 4.13.4. Following the steps in the General Test Procedure, run a moisture test using the 5-50ppm

moisture check gas as a sample source. 4.13.5. Check for a positive meter deflection.

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4.13.5.1. If there is no positive meter deflection, the cell is bad a must be replaced. 4.13.6. Record the results in the Equipment Calibration Log. 4.13.7. Note: In Packaged Gases Plants, a test cylinder that reads above 5 ppm moisture may be

used for the monthly Cell Check if the results are recorded on the Equipment Calibration Log. 5. REFERENCES GENERAL DESCRIPTION

The MEECO Moisture Analyzer is a portable, automatic analyzer used to read moisture content of gases directly in ppm. Its operation is based on the principle of electrolytic hygrometry.

THEORY The heart of all electrolytic hygrometers is a cell in which water from a sample stream is continuously absorbed and electrolyzed – dissociated into hydrogen and oxygen. The cell consists of a thin film of partially hydrated phosphorous pentoxide between two spirally wound platinum electrodes. A dc potential applied to each of the electrodes causes the electrolysis; the resulting hydrogen and oxygen gases are carried off by the sample stream. The electric current resulting from the dissociation is a measure of the moisture concentration in the sample stream. In practical use, the electrical circuitry, sample flow rate, and temperature are so chosen that the moisture concentration can be read in parts per million (ppm) by volume, directly on a readout meter. Samples of air, hydrogen, and oxygen may produce exaggerated reading on MEECO Moisture Analyzers. This occurs because the free oxygen or hydrogen atoms from the electrolysis of water (moisture) tend to recombine with gas in the sample stream. The re-formed water is electrolyzed again, producing a false higher reading of sample moisture content. (This recombination effect may result in extended purge times during testing of oxygen or hydrogen.) • This effect is present with all hydrogen samples. • In air or oxygen samples, this effect is significant only when the true moisture content is 20 ppm

or less. For sample flowrates in the ranges we use, the re-formation of water is constant. This fact allows us to correct the exaggerated reading and obtain the true moisture content of the sample. The Delta-Flow Test Method consists of running the test procedure twice, changing the prescribed flowrate on the second run. Since the excess moisture from re-formation is constant on both test runs, it cancels out in the subtraction giving a true moisture content reading.

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 5.22 F310-1 Supplier Assessment Questionnaire

1. OBJECTIVE

This procedure establishes the Supplier Assessment Questionnaire


It is the responsibility of all purchasing and laboratory personnel to ensure that this procedure is performed as described, that this procedure is reviewed and updated as necessary, and that proper support documentation is maintained.

4. PROCEDURE 4.1. Complete the attached questionnaire.

5. REFERENCES

5.1. The questionnaire follows: Your organization has been identified as a potential supplier of parts/services for our future procurement needs for the following products or services: This Preliminary Supplier Qualification Survey contains pertinent questions applicable to the qualification process. Please answer those questions of the survey that pertain to and are applicable to your company, as thoroughly as possible and attach any and all additional documentation/information, which you feel would be helpful in our assessment. All information supplied will be treated as confidential. To assist us in completing our assessment in a timely manner, it is requested that you provide us with the following documentation: If not ISO Certified:

1. Completed Survey 2. A copy of your current Quality Systems Manual 3. An organization chart

If ISO Certified:

1. Completed Survey 2. A copy of your ISO Certification 3. An organization chart

Upon completion of this survey, please return it in its entirety to:

Company Name Company Address

Please provide any additional comments on the last page of this survey. We would like to say “thank you” in advance for taking the time to complete our survey.

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Company Name: Company Address: Company Phone: Company Fax: E-mail Address: Web Page Address: Survey Completed by: (Name) (Title) (Date) Type of Business: Business Classification:

□ Corporation □ Distributor

□ Partnership □ Manufacturer (components/sub-assemblies)

□ Proprietorship □ Manufacturer (finished devices)

□ Other: (specify) □ Consulting Main Services: Number of years in business: Annual Sales:

Do you have other service locations?: □ Yes □ No If yes, please list locations:

Department Manager’s Name Title # of Employees

President/CEO President/CEO

Quality Assurance

Manufacturing/Operations

Marketing/Sales

Research & Development

Materials

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Total Plant Area (sq ft): Total number of employees: Government related sales: %

Is Annual Report Available?: □ Yes □ No

Is a Dunn & Bradstreet available?: □ Yes □ No

Are you receptive to an on-site survey? □ Yes □ No

Total Production Area (sq ft): Is your company union organized?: Name of Union: Expiration of current contract: Last work stoppage: How long?

Are you at the capacity of your plant operations? □ Yes □ No How many shifts do you run? What Calibration Services do you subcontract?

Do you anticipate expanding your facility within the next two (2) years? □ Yes □ No

Do you anticipate relocating your facility within the next two (2) years? □ Yes □ No Please list five (5) customers you are currently doing business with and include the name of a person we may contact as a reference for your company.

Company Contact Phone Number Comments

Do you supply calibration services or products to manufacturers of medical device equipment?

□ Yes □ No

Do you have processes that are proprietary? □ Yes □ No

Will you be available for on-site audits? □ Yes □ No

Will you confirm specification revisions when issued? □ Yes □ No What type of MRP sales system do you use?

Do you have Video Conferencing Capability? □ Yes □ No

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THE FOLLOWING QUESTIONS PERTAIN TO YOUR OVERALL QUALITY SYSTEM. PLEASE ANSWER ALL APPLICABLE QUESTIONS (include document references where possible), AND WRITE “N/A” NEXT TO QUESTIONS THAT DO NOT APPLY. THANK YOU. ** Please attach any reference documents needed to explain your responses. Question Response How is the Quality philosophy communicated and implemented throughout your organization? Are there clearly defined quality objectives?

How are the responsibilities, authorities, and interrelationships between personnel defined within your organization?

Do you have a Quality System Management representative? If so, list his/her name and title.

Do you hold periodic reviews with executive management to ensure implementation of quality objectives and adequacy of your quality system?

What programs do you have in place for continuous improvement?

Do you have a quality manual? Do you have a quality policy? Describe your organization’s quality planning activities. How do you plan for quality?

Describe your DESIGN CONTROL system. Describe your design/process change control system. What is the mechanism for communicating changes or issues in your product to your customers?

Do you have procedures to control and maintain documents and data?

Do you have a procedure to remove obsolete documents?

Do you have a procedure to change documents? How do you validate document changes? Are documents and specifications approved before use to assure compliance with contract requirements?

Describe how procedures are made available to employees for use.

Describe your suppliers/vendor controls. Do you audit your suppliers/vendors?

Can your customers audit your suppliers, if needed? Do you have an approved supplier/vendor listing? How do you ensure proper product identification and traceability? Do you lot code, date stamp, or trace materials, components or devices? Do you serialize products?

Do you use bar coding? □ Yes □ No If yes, what standard?

Describe your manufacturing process from receipt through installation. Also, discuss documentation required at each step.

What type of process data do you collect? How are your manufacturing instructions documented?

How do you control and measure process performance?

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Is product performance and reliability data available to your customers?

If Yes, list the type of data.

How is Statistical Process Control used in your operation?

What environmental controls are implemented in your facility?

Describe your procedures for process validation. If sterile product, how do you ensure sterility of product?

Describe your Equipment Maintenance program. How do you distinguish status of product throughout the manufacturing process?

Describe your system for controlling non-conforming product.

Describe your overall corrective and preventative action system. How do you ensure timely corrective actions?

Describe your process for handling, storage, packaging, preservation, and delivery of product.

Do you have a documented FIFO procedure? Describe your system for proper recordkeeping and retention.

Describe your Device/Batch History records. Describe your internal auditing system. Describe your employee-training program. Do your employees receive job specific training? How is training documented?

If applicable, describe your systems that address servicing of your product.

What statistical techniques do you employ in the design or manufacture of your product?

Do you verify incoming products? Do inspectors have procedures or standards covering sampling plan criteria? If so, which one?

Do you hold the product until required tests or inspections are complete?

Do your incoming inspection records contain: lot size, sample size, quantity inspected, quantity rejected, inspector and date?

Do you have a Material Review Board (MRB) for reviewing of non-conforming material?

Is the Quality Department represented during the MRB?

Do you have a final inspection and test area? Do you maintain records of all inspections and tests? Do you perform incoming product evaluation and qualification testing?

Is this testing documented in a controlled procedure? Do you have documented procedure on how to handle problems and failures?

Do you allow deviations to specifications? Do you have an in-house calibration system? Is your calibration system traceable to NIST standards?

Are there controlled procedures for calibration? Do calibration records contain: equipment identification number and name, frequency of

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calibration, procedure number, date of calibration, due date for next calibration, person performing calibration, “Standard” used in calibration, and calibration results? If calibration is not required, is the equipment marked as such?

If a piece of equipment is out of calibration, is there a system to assess the product which was manufactured using the equipment to determine the effect of the out of calibration?

Do you comply with FDA Quality System Requirements?

What other regulations do you comply with? Do you hold any other registrations/certifications? Please list.

List companies from which you have received Quality Award(s) or special recognition.

For PurityPlus Use Only Pre-Assessment Review PurityPlus Plant Reviewed by/Date:

AsteRisk Reviewed by/Date:

PurityPlus Operations Committee Reviewed by/Date:

Other Reviewed by/Date:

Approved (and Comments)

□ Yes □ No Supplier On-Site Assessment Required:

□ Yes □ No

Rationale for Decision:

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 5.23 COCs and COAs

1. OBJECTIVE

This procedure establishes the guidelines for certificates of conformance, certificates of analysis and certificates of calibration.



4. PROCEDURE 4.1. Standardized Certificates of Conformance (COCs) and Certificates of Analysis (COAs) provide our

customers with information about product specifications, certification, and analysis. Order entry personnel should specify which COC or COA the customer requires. Any optional requirements should also be included.

4.2. GENERAL GUIDELINES FOR COCs AND COAs 4.2.1. All COCs and COAs must bear the following:

Full name and address of the customer Date the document was prepared. Lot number Authorized signature

4.2.2. The smallest value of analytical results that may be reported for impurities is the Limit of Detection (LoD) of the analyzer used. When the analyzer reads at or below this LoD, report the LoD, not the meter or display reading. Typical LoDs are listed below by analyzer in the column headed Limit of Detections.

4.2.2.1. When reporting an LoD instead of the actual analyzer reading, write the initials LoD after the figure – for example “<0.5 ppm LoD”

4.2.2.2. If the analytical value represents a concentration of impurities by weight, write “wt” after the value, for example, “9 ppm wt.”

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Quality Assurance Analyzer Certification Method Moisture Analyzers:

MEECO Model W MEECO Aquamatic MEECO Aquamatic + Beckman DuPont 5700 Aquatest (Karl Fisher)

Typical Limit of Detection LoD * 0.5ppm 0.10ppm 0.01ppm 0.5ppm 0.02 ppm 0.5ppm

Trace Oxygen Analyzers: Teledyne 316 RA Teledyne 306 W Teledyne 306 WAM Teledyne 306 WADX Teledyne 306 WAMX Teledyne 315 Research Incorporated Delphi Electrochemical

1.0ppm 0.2ppm 0.2ppm 0.02ppm 0.02ppm 0.5ppm 0.5ppm 0.2ppm

Percent Oxygen Analyzers Biomarine Oxygen Analyzer OA288 Taylor 244 (0-100% Range) Teledyne 320 (0-5% Range)

(0-25% Range) (0-100% Range)

Teledyne 320 D (0-100% Range)

1% 1% 0.2% 0.5% 2.0% 0.1%

Total Hydrocarbon Analyzers GOW-MAC THA Beckman 400A

0.1ppm 0.1ppm

Carbon Dioxide Plus Carbon Monoxide Analyzers

Beckman 865-X4 Horiba

0.1ppm 0.1ppm (depending on specific model)

Nitrogen in Argon Analyzer Linde Nitrospec Delphi Model D

0.1ppm 0.1ppm

Gas Chromatographs As determined by specific analysis and detection method

Gas Master – Gow-Mac 0.1%

Scales Sauter Mettler

As determined by COA reporting limits.

* Do not report analytical results to more significant figures than specified.

4.2.3. All body labels for mixtures must show the certified value of the mixture components. The neck tags, body label, and COA must show the same concentration values.

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4.2.4. All COCs and COAs should have a disclaimer statement on the bottom of the page; typical wording follows:

IMPORTANT: While we believe that the information is accurate within the limits of the analytical methods employed and is complete to the extent of the specific analyses performed, we make no warranty or representation as to the suitability of the use of the information for any particular purpose. The information is offered with the understanding that any use of the information is at the sole discretion and risk of the user. In no event shall the liability arising out of the use of the information contained herein exceed the fee established for providing such information.

4.2.5. A copy of each COC and COA must be kept on file for a minimum of one year plus the current year.

4.2.6. Calculate the desired and actual uncertainty of the mixture. Report significant figures based upon the desired and actual uncertainty or use the following list for the reporting of significant figures:

1-19ppm Report the actual concentration as limited by the Certification Method (from the list of analyzers and methods earlier in this item) but not less than 0.1ppm

20-499 ppm Report to nearest whole ppm value 500-4999ppm Report to nearest 10ppm value. When reporting in

percent form always use a zero to the left of the decimal point.

0.50%-4.99% Report to nearest hundredth place (two places to the right of the decimal point). When reporting values less than 1.00%, always use a zero to the left of the decimal point.

5.0%-50.0% Report to nearest tenth place; one place to the right of the decimal point

4.2.7. Report the following information on each CoA: Cylinder number, Mixture Components,

Requested Composition, Certified Composition, Certification Accuracy and specific items requested by the customer.

5. REFERENCES

5.1. None

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Quality Assurance Program Rev. 17 December 2012 Rev #: 6 Document Title: 5.24 Calibration Standards

1. OBJECTIVE

This procedure establishes the guidelines for calibration cylinders



4. PROCEDURE 4.1. All calibration cylinders used to calibrate quality assurance instrumentation must be accompanied by

a Certificate of Analysis (test report). A Certificate of Analysis must be requested when ordering a calibration cylinder from a Packaged Gases plant, Specialty Gas plant, or a distributor.

4.2. All calibration cylinders should have the appropriate analysis indicated on the label or tag attached to the cylinder.

4.3. All Certificates of Analysis for calibration cylinders must be retained in a quality assurance file for three years plus the current year after the last usage of the calibration cylinder.

4.4. Calibration cylinders are considered empty and must be replaced when their pressure falls below 100 psig.

4.5. Cylinders used to calibrate instruments for PurityPlus products must meet PurityPlus Primary Standard specifications, even if purchased from a non-PurityPlus supplier.

4.6. Cylinders used to calibrate instruments for PurityPlus products must be traceable to NIST, or other national meteorological institute. See references below for typical meteorological institutes.

4.7. Weights – The weights used to verify and/or calibrate gravimetric scales shall be NIST traceable weights (ASTM E 617 Class 3 or better). The weights shall be recalibrated every 2 to 5 years according to NIST 105-1. If the weights are used daily or weekly, they should be recertified every two years. If the weights are used on a monthly, or longer, interval, and they are maintained in excellent cleanliness and condition, they may be recertified not longer than five years.

4.7.1. Order a 1 kg mass for daily and monthly scale verifications… e.g. Rice Lake Weighing Systems Part Number 13193, approximately $109 in 2011. http://www.ricelake.com/product.aspx?CatID=3647

4.7.2. Order a NIST traceable weight kit. Consider http://www.ricelake.com/products/test-weights/precision-laboratory-weights-astm-classification/sets/metric/2kg-3kg-5kg/class-3/view/parts/id/12078 or other set of weights in the ranges you are measuring.

4.8. Weight Certifications – The facility you use to recertify the weights must provide documented evidence of traceability to NIST at the weight level they are certifying. Consider using the South Carolina Department of Agriculture to calibrate your weights. They are Traceable to NIST at all three levels. One agency which is acceptable is: South Carolina Department of Agriculture Metrology Laboratory 237 Catawba Street Columbia, SC 29201 Robert McGee 803-253-4052.

5. REFERENCES

5.1. PurityPlus Catalog for Primary Standard specifications 5.2. Selected National Meteorological institutes. See following page

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Selected National Meteorological institutes United States of America National Institute of Standards and Technology Standard Reference Materials® Program NIST 100 Bureau Drive, Stop 2300 Gaithersburg, MD 20899-2300 Phone: (301) 975-2200 Fax: (301) 948-3730 Canada National Research Council Canada Institute for National Measurement Standards 1200 Montreal Road, Building M-36 Ottawa, Ontario K1A 0R6 Phone: (613) 998 7018 Fax: (613) 954 1473 E-mail: [email protected] Mexico Centro Nacional de Metrología (CENAM) km 4,5 Carretera a Los Cués Apdo Postal 1-100 Centro, Querétaro 76900 Phone: (52 442) 211 0510 Fax: (52 442) 215 5332 E-mail: [email protected] Netherlands Nederlands Meetinstituut (NMi) Schoemakerstraat 97 P.O. Box 654 NL 2600 AR Delft Phone: (31 15) 269 1500 Fax: (31 15) 261 2971 E-mail: [email protected]

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Quality Assurance Program Rev. 23 July 2010 Rev #: 1 Document Title: 5.25 Calibration Intervals

1. OBJECTIVE

This procedure establishes the guidelines for the calibration intervals of instruments.



4. PROCEDURE 4.1. For instruments not mentioned below, follow the manufacturer’s recommended calibration interval

until another appropriate interval can be documented. 4.2. Default calibration intervals:

4.2.1. Trace oxygen analyzers are calibrated on a weekly basis. 4.2.2. Trace moisture analyzers are verified monthly using “intermediate testing”. Intermediate

testing is conducted by analyzing a stable wet cylinder (>20 ppm) monthly. The monthly tests are compared to each other to verify that the instrument produces consistent results over the long term. When readings vary more than the expected accuracy/stability of the cylinder, have the instrument recalibrated, repaired or replace the intermediate testing cylinder.

4.2.3. Total hydrocarbon analyzers are recalibrated before each use. The balance gas of the calibration zero and calibration span cylinders should match the sample gas unless documented studies or manufacturers’ instructions prove the acceptability of alternate balance gases.

4.2.4. Gas chromatographs are recalibrated before each use. The balance gas of the calibration span cylinders should match the sample gas if a micro gas chromatograph is used (e.g. Varian 4900 or MTI 200).

4.2.5. Percent level oxygen analyzers are recalibrated before each use or according to the frequency recommended by the manufacturer.

4.2.6. Infrared trace gas analyzers are recalibrated before each use or according to the frequency recommended by the manufacturer.

4.2.7. Plasma ionization trace nitrogen analyzers are recalibrated before each use or according to the frequency recommended by the manufacturer.

4.2.8. Gas detector tubes are not calibrated in the field. Detector tube accuracy is guaranteed by the manufacturer as long as the expiration date of the tube has not passed.

4.2.9. NIST traceable weights (ASTM E 617 Class 3 or better) shall be recalibrated every 2 to 5 years according to NIST 105-1.

4.3. Adjusting the calibration interval. The manufacturers’ recommended calibration interval/default calibration interval may not be appropriate in all installations and as instruments age. In some cases the optimum calibration interval may be increased and, in other cases, the optimum calibration interval may need to be decreased. The following steps describe “Method 1: Automatic adjustment or “staircase” (calendar-time)” of ILAC-G24:2007.

4.3.1. Each time an instrument is calibrated on a routine basis, the next interval is extended if it is found to be within e.g. 80 % of the maximum permissible error that is required for measurement, or reduced if it is found to be outside this maximum permissible error.

4.3.2. When the calibration interval is increased, the new calibration interval shall not exceed 200% of the prior interval.

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4.3.3. For example, consider the case of a trace oxygen analyzer which is routinely calibrated with a 10.0 ppm oxygen in nitrogen standard and the desired accuracy of the analysis is 10% relative (or +/- 1.0 ppm absolute). The beginning calibration interval is one week. Following is a description of the calibration interval evaluation: As As Error Comments Found Adjusted Installation - 10.0 10.0 0 Initial calibration Week 1 10.2 10.0 0.2 0.2 is 20% of the permissible error - OK Increase interval to 2 weeks Week 3 9.5 10.0 0.5 0.5 is 50% of the permissible error - OK Increase interval to 3 weeks Week 6 10.7 10.0 0.7 0.7 is 70% of the permissible error - OK Increase interval to 4 weeks Week 10 10.9 10.0 0.9 0.9 is 90% of the permissible error – Excessive error Decrease interval to 3 weeks Week 13 9.4 10.0 0.6 0.6 is 60% of the permissible error - OK Maintain interval at 3 weeks until further evaluation

5. REFERENCES

5.1. Instrument manufacturers’ operating manuals 5.2. Calibration Records

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Quality Assurance Program Rev. 2 Feb. 2010 Rev #: 1 Document Title: 5.26 Calibration Records

1. OBJECTIVE

This procedure establishes the guidelines for recording instrument calibrations.



4. PROCEDURE 4.1. Use the calibration records referenced below to document the calibration of laboratory instruments.

5. REFERENCES 5.1. Instrument manufacturers’ operating manuals 5.2. Intermediate Testing Record 5.3. Fixed Interval Calibration Record 5.4. Adjustable Interval Calibration Record

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Intermediate Testing Record

Instrument Being Tested

Serial Number/ID

Test Method

Intermediate Test Cylinder Serial Number

Description (e.g. 22.0 ppm H2O in N2)

Tolerance Minimum

Tolerance Maximum

Date Tester Instrument Response

Pass or Fail Comments

q Pass q Fail

q Pass q Fail

q Pass q Fail

q Pass q Fail

q Pass q Fail

q Pass q Fail

q Pass q Fail

q Pass q Fail

q Pass q Fail

q Pass q Fail

q Pass q Fail

q Pass q Fail

q Pass q Fail

q Pass q Fail

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Fixed Interval Calibration Record (Daily, Weekly, Monthly, Etc.) Instrument Being Calibrated

Serial Number/ID

Test Method

Calibration Interval

“Zero Gas” Cylinder Serial Number (if any)

Description (e.g. 0.05 ppm CH4 in N2)

“Span Gas” Cylinder Serial Number


Date Tester Type As Found

As Adjusted

Pass or Fail Comments

q Zero q Span

q Pass q Fail

q Zero q Span

q Pass q Fail

q Zero q Span

q Pass q Fail

q Zero q Span

q Pass q Fail

q Zero q Span

q Pass q Fail

q Zero q Span

q Pass q Fail

q Zero q Span

q Pass q Fail

q Zero q Span

q Pass q Fail

q Zero q Span

q Pass q Fail

q Zero q Span

q Pass q Fail

q Zero q Span

q Pass q Fail

q Zero q Span

q Pass q Fail

q Zero q Span

q Pass q Fail

q Zero q Span

q Pass q Fail

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Adjustable Interval Calibration Record (ILAC-G24:2007, Method 1) Instrument Being Calibrated Serial Number/ID Test Method Calibration Interval

“Zero Gas” Cylinder Serial Number (if any)

Tolerance (Permissible Error) Min. Max. 80% Min. 80% Max.


“Span Gas” Cylinder Serial Number

Tolerance (Permissible Error) Min. Max. 80% Min. 80% Max.


Date Tester Type As Found

As Adjusted

Pass or Fail

Within 80% of

Permissible Error?

Increase or Decrease Interval

Next Calibration Interval / Comments

q Zero q Span q Pass

q Fail q Yes q No

q Increase q Decrease q Same


q Fail q Yes q No



q Fail q Yes q No



q Fail q Yes q No



q Fail q Yes q No



q Fail q Yes q No



q Fail q Yes q No



q Fail q Yes q No



q Fail q Yes q No



q Fail q Yes q No



q Fail q Yes q No


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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 5.27 Breathing Mixtures

1. OBJECTIVE

This procedure establishes breathing mixtures.



4. PROCEDURE 4.1. REQUIREMENTS

4.1.1.1. Each plant must have an approved Gas Mixture Data Sheet for each mixture the plant is authorized to fill.

4.1.1.2. All requests for mixtures with Balance Air will be made having a concentration of 21% oxygen.

4.1.1.3. To assure that the listed breathing mixtures are released with the specified quantity of oxygen, the following procedures must be followed if the mixtures are filled in cylinders, clusters, tube trailers, etc., regardless of equipment ownership.

4.1.2. Once a cylinder is connected for filling, it must be product labeled prior to disconnection. This labeling requirement is mandatory, even if the cylinder is never actually filled.

4.1.3. all cluster cylinders with individual cylinder valves must have a product decal on every cylinder. This will assure the product’s identification in the event of the cluster’s disassembly.

4.1.4. All cluster cylinders without individual cylinder valves must have a cylinder product decal at each outlet.

4.1.5. All cylinder valves and manifold connections on a cluster must be identical and these valves must be the specified CGA product connection.

4.1.6. All cylinders must leave the fill area either: 4.1.6.1. Full – containing all specified components and at full rated pressure and temperature or, 4.1.6.2. Empty – at atmosphere pressure with the valve open

4.1.7. Each full breathing mixture cylinder or tube having an oxygen content of < 50% must be tested for oxygen content and for all other purity specifications. The cylinder must meet all specifications prior to release. A positive connection to the analyzer is required for all oxygen assays. Analysis of any breathing mixture, including air, with an oxygen concentration of 17%-25% requires introduction of nitrogen into the analyzer between analyses until it reads 15% or less of oxygen. A positive connection to the analyzer is not required for this purge.

4.1.8. Note: The nitrogen purge is not required for the Orsat. 4.1.9. Analysis of any breathing mixture with an oxygen content of less than 17% or between 25%-

50% requires introduction of atmospheric or compressed air into the analyzer between analyses until it reads 19.5%-23.5% oxygen.

4.1.10. Note: The atmospheric or compressed air purge is not required for the Orsat. 4.1.11. Each full breathing mixture cylinder or tube having an oxygen content of greater than 50%

must be qualitatively (product identified) tested for oxygen in addition to all other tests. The cylinder must meet all specifications prior to release. A positive connection to the analyzer is required for all qualitative tests.

4.1.12. In the qualitative test, the mixture is analyzed to assure that it contains a minimum of 21% oxygen. A Biomarine OA288, Teledyne 320, Taylor OA244, or equivalent analyzer is used. Refer to the Medical Gas Mixture Data Sheet for the appropriate analyzer. An indication on the meter that the oxygen content in the test cylinder is greater than 21% oxygen is all that is required to satisfy the test. As soon as the meter reads 21% oxygen, the test is terminated.

4.1.13. The analyzer must be purged with nitrogen between analyses until it reads 15% or less of oxygen. A positive connection to the analyzer is not required for this purge.

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4.1.14. Each individually-valved cylinder of a cluster and each individually-valved tube of a tube trailer must be tested for oxygen. This test must be conducted by opening the valve of only one cylinder or tube at a time. When the proper purity reading is obtained, the valve of that cylinder or tube must be closed and the manifold blown down to zero psig before the next cylinder or tube is tested. The analyzer must also be purged with nitrogen or air, as applicable, before the next test. See paragraph 6 or 7 above for the proper purge procedures.

4.1.15. One oxygen test is sufficient for cluster cylinders without individual cylinder valves. 5. REFERENCES

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Quality Assurance Program Rev. 7 June 2010 Rev #: 3 Document Title: 5.28 Compressed Air

1. OBJECTIVE

This procedure established compressed air.



4. PROCEDURE 4.1. GENERAL REQUIREMENTS

4.1.1. The quality assurance requirements in this item must be followed by all plants filling compressed air cylinders whether USP, Standard or diving grade. These procedures are applicable to air filled in cylinders, clusters, tube trailers, etc., no matter who owns the equipment.

4.1.2. Cylinders Require Test – Every compressed air cylinder filled must be tested for and must meet oxygen content and all other purity specifications prior to release.

4.1.3. Rack Requirements – All compressed air cylinders must be filled on a common rack. This rack must have a positive disconnect so that only oxygen or nitrogen can be supplied and connected to the rack at one time.

4.1.4. Required Log – Each individual filling compressed air cylinders must fill out an “Air and Medical Gas Filling Log,”. The serial number of every cylinder tested must be listed. A new log sheet must be started for each shift on which the cylinders are filled and for each change of pampers. The air standard used to verify the accuracy of the test equipment must be entered on the “Equipment Calibration Log,”.

4.2. APPROVED TEST EQUIPMENT 4.2.1. Servomex Oxygen Analzer with readability in the 19.5% Oxygen to 23.5% Oxygen range. (e.g.

OA-244 Digital Readout, 570, 572, 575, 5200, etc. 4.2.2. Teledyne 320B Portable Oxygen Analyzer

4.3. PILLING AND TEST PROCEDURES 4.3.1. Cylinder filling and quality assurance testing must be done on the same shift by the same

individual. Steps 1 through 3 must be done before the cylinders are connected to the rack. 4.3.2. Conduct the mandatory pre-filling inspections required by 4.1, High Pressure Cylinder Pre-Fill

Inspection. 4.3.3. For standard and diving grade air, remove old Warranted for Breathing labels. 4.3.4. Note: Once a cylinder is connected for filling, it must be product labeled prior to disconnection.

This labeling requirement is mandatory even if the cylinder is never actually filled. 4.3.5. Blow cylinders down. 4.3.6. Evacuate the cylinders to 27in of Hg, then fill them using 4.2, High Pressure Oxygen Cylinder

Filling. 4.3.7. Standardize the approved test equipment.

4.3.7.1. Standardization is accomplished by testing an approved analyzer with an air standard. 4.3.8. Note: the approved analyzer must read within + 0.1% of the oxygen concentration of the air

standard. 4.3.9. The air standard must be:

4.3.9.1. A Primary Standard. 4.3.9.2. In addition, each air standard cylinder must be marked as a standard cylinder, showing

the concentrations of oxygen and nitrogen. 4.3.9.3. All Primary Standards must be ordered by specifying the intended use. 4.3.9.4. The procedures listed below must be followed during preparation of the Air Primary

Standard.

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4.3.9.4.1. The air standard must be made by weight. 4.3.9.4.2. The air standard must be rolled to assure complete mixing. 4.3.9.4.3. The air standard must be cross-checked analytically on a gas chromatograph to

ensure the proper oxygen-nitrogen concentration. 4.3.10. Introduce nitrogen into the analyzer until the analyzer reads 15% or less of oxygen. (A

positive connection to the analyzer is not required for this step.) 4.3.11. Immediately connect the air sampling assembly to the cylinder. A positive connection of the

analyzer to the cylinder is required for all oxygen tests of compressed air. 4.3.12. If the oxygen content is not 19.5 to 23.5% for USP or OSHA Grade D Air, or 20 to 22% for

diving grade air, reject the cylinder. 4.3.13. Record the serial number and test results of all cylinders tested. 4.3.14. Repeat analytical steps for each cylinder tested. EVERY CYLINDER FILLED MUST BE

TESTED FOR OXYGEN CONTENT. Be sure to sample nitrogen between each test to assure the regulator is purged.

4.3.15. All cylinders must leave the fill area either: 4.3.15.1. Full – containing all specified components and at full rated pressure and temperature

or, 4.3.16. Empty – at atmospheric pressure with the valve open.

4.4. ADDITIONAL CLUSTER AND TRAILER REQIUREMENTS 4.4.1. Each individually valved cylinder of a cluster and each individually valved tube of a tube trailer

must be tested for oxygen purity. This test must be conducted by opening the valve of only one cylinder or tube at a time. When the proper oxygen purity reading is obtained, the valve of that cylinder or tube must be closed and the manifold blown down to zero psig before the next cylinder or tube is tested. The analyzer must also be purged with nitrogen before the next test.

4.4.2. One oxygen purity test is sufficient for cluster cylinders without individual cylinder valves. 4.4.3. All cluster cylinders with individual cylinder valves must have a product decal on every cylinder.

This will assure the product’s identification in the even of the cluster’s disassembly. 4.4.4. All cluster cylinders without individual cylinder valves must have a cylinder product decal at

each outlet. 4.4.5. All cylinder valves and manifold connections on a cluster must be identical and these valves

must be the specified CGA product connections. 4.5. FILLING SELF-CONTAINED BREATHING APPARATUS FOR PLANT USE

4.5.1. Self-contained breathing apparatuses used in plants may be filled from Standard Grade Air cylinders if the cylinders have been properly tested and labeled.

4.5.2. Test air cylinder for the proper oxygen concentration. 4.5.3. After transfilling to the apparatus, enter the lot number form the air cylinder on a second sticker

and apply it to the apparatus. 4.5.4. Note: Apply a new lot number to the apparatus after each filling. 4.5.5. Each self-contained breathing apparatus filled by an outside vendor must either bear a lot

number traceable to the vendor or be accompanied by a certification that air in the unit is suitable for breathing. The certification must be kept on file during the lifetime of the air in the apparatus.

5. REFERENCES

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 5.29 Beckman CO2/CO Analyzer System

1. OBJECTIVE

This procedure establishes the Beckman CO2/CO Analyzer System.




4.1.1. The following gases must be supplied to the instrument: 4.1.1.1. Sample 4.1.1.2. Zero – less than 0.1 ppm carbon dioxide in argon or nitrogen. 4.1.1.3. Span – 8-10 ppm carbon dioxide in argon or nitrogen 4.1.1.4. Check - 5-10 ppm carbon monoxide in nitrogen or argon gas having less than 0.5ppm

carbon dioxide content. 4.1.2. Warning: Pressure regulation and suitable pressure relief devices must be provided if the above

gases are supplied in the high-pressure cylinders. 4.1.3. Allow sufficient time for the analyzer circuitry to warm up before operating the analyzer.

4.2. TEST PROCEDURE 4.2.1. Close the Sample On-Off Valve.

4.2.1.1. This isolates the CO2 sample selection valve located at the lower left corner of the panel from the three calibration gas valves.

4.2.2. Place the Furnace Mode Valve in the BY-PASS FURNACE position. 4.2.3. Introduce the zero gas by opening the Zero Gas Toggle Valve and adjust the sample flow

through the analyzer to 2 cfh. 4.2.4. Adjust the Zero Pot on the analyzer to about 1% of scale. 4.2.5. When a constant reading is obtained, close the Zero Gas Valve and introduce the span gas at 2

cfh. 4.2.6. When the reading is again constant, adjust the Gain (span) Pot on the analyzer to match the

carbon dioxide content in the span mixture for 10 ppm full scale sensitivity. 4.2.7. Recheck the Zero Pot and Gain Pot adjustments (step 3 through 6) to ensure proper calibration

of the analyzer. 4.2.8. Open the check Gas Toggle Valve. 4.2.9. Switch the Furnace Mode Valve to the THRU FURNACE position. 4.2.10. Note: This causes the check gas (5 to 10 ppm carbon monoxide in nitrogen) to flow through

the hot copper oxide furnace unit (set at 325°C to 350°C) where it undergoes combustion and is converted to carbon dioxide. After combustion all carbon monoxide is measure as carbon dioxide.

4.2.11. To obtain the actual carbon monoxide concentration: 4.2.11.1. Note the meter reading. The reading obtained represents CO + CO2 4.2.11.2. Switch the Furnace Mode Valve to the BY=PASS FURNACE position 4.2.11.3. Take a second meter reading and subtract it from the one obtained above. 4.2.11.4. The difference in the readings represents the actual carbon monoxide concentration

in the check gas, which should compare to the stated concentration. 4.2.11.5. To Summarize: 4.2.11.6. The BY-PASS FURNACE position measure carbon dioxide (CO2).

4.2.11.6.1. The THRU FURNACE mode position measures carbon dioxide plus carbon monoxide (CO2 + CO)

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4.2.11.7. The actual carbon monoxide concentration (CO) is the difference between these two readings.

4.2.12. Close the Zero and Span Toggle Valves. 4.2.13. Open the Sample Selection Valve and turn it to allow selection of the desired sample gas, for

example, NITROGEN. 4.2.14. Adjust the sample flow to the analyzer to 2 cfh. 4.2.15. With the Furnace Mode Valve in the BY-PASS FURNACE position, measure and record the

concentration of carbon dioxide in the sample. 4.2.16. With the Furnace Mode Valve in the THRU FURNACE position, measure the concentration of

carbon dioxide plus carbon monoxide. Subtract the reading obtained in Step 14 to obtain the concentration of carbon monoxide.

4.3. EQUIPMENT CALIBRATION 4.3.1. The accuracy of this instrument depends on the ability to repeat the conditions of the zero and

span gases. The calibration is checked prior to use. 4.4. REFERENCE TO STANDARDS

4.4.1. The zero, span and check gas cylinders are prepared and analyzed under laboratory conditions using accepted industry practices and standards, traceable to the National Institute of Standards and Technology (NIST), formerly the National Bureau of Standards.

5. REFERENCES GENERAL DESCRIPTION

Non-dispersive infrared analyzers measure the concentration of one specific component in a gas mixture. They rely on the principle – true for most compounds of two or more different atoms – that each compound absorbs energy in a different part of the spectrum from the others. By design the Beckman Model 865-X4 gives readings in that part of the infrared spectrum absorbed by carbon dioxide. The Beckman CO2/CO Analyzer System add the Catalytic Combustion Unit to the Beckman Model 865-X4 so that concentrations of carbon monoxide as well as of carbon dioxide can be measured. To do this the added unit first converts the carbon monoxide to carbon dioxide, which the Beckman Model 865-X4 can then measure directly.

THEORY The infrared absorption of a compound is characteristic of the type and arrangement of the atoms composing its molecules. The Beckman Model 865-X4 non-dispersive infrared analyzer produces infrared radiation from two separate energy sources of nichrome wire. A DC voltage applied to the two similar helices of nichrome wire heats the wires to the point where they emit infrared energy. This energy is channeled alternately via a rotating interrupter through parallel optical paths – the sample cell and the comarion cell – to a sensing element, the detector. The optical paths are selected to eliminate interference from other infrared absorbing components. During operation, a portion of the infrared radiation passing through the sample gas is absorbed by the carbon dioxide in the sample cell. A different amount of infrared radiation is absorbed by the reference cell, resulting in a difference in the amount of infrared radiation that emerges from the two cells. The detector converts this difference to a capacitance change. This capacitance change, equivalent to component concentration, is amplified and indicated on the meter.

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 5.30 Gaseous Product Odor Test

1. OBJECTIVE

This procedure establishes the gaseous product odor test.




4.1.1. Insure that room deodorizers are of the types that suppress odors, not the sense of smell. 4.1.2. Temporarily reassign personnel from odor testing duties when they have a cold or hay fever. 4.1.3. Odor testing of tank trucks is conducted on a manifold connected to the truck. The odor test port

is usually located inside a building and should be at a height convenient for the tester. 4.1.4. If the product sample is taken from the liquid phase, vaporization must be complete, and then

issuing gas should be at near ambient temperature. 4.2. TEST PRCEDURE

4.2.1. Stand at arms length from the test port. Position yourself so that the flow of gas will be directed 90° away from your face.

4.2.2. Warning: Odor test only those gases for which an odor test is specified in the “Products” section. Never allow valve to point toward your face during test. Cold vapor can cause frostbite if it comes into contact with your skin. High pressure gas streams can propel particles at dangerous velocities. If you detect an odor at any time during the test, immediately shut off the gas supply and stop the test. Go to step 5.

4.2.3. Slowly open valve until gas flows. Stay at arms length, cup your hand and fan the gas toward your nose. Smell cautiously. If you do not detect an odor, go on the step 3.

4.2.4. Continue fanning motion while moving closer to test port. If you do not detect and odor, go on to step 4.

4.2.5. Cup hand around valve outlet and move your head in close. Smell the gas issuing from test port into your cupped hand.

4.2.6. The gas must be odor free. Any odor is cause for rejection. 4.3. EQUIPMENT RECALIBRATION

4.3.1. The results of this test are determined by the sensitivity of the olefactory nerves; therefore, no equipment calibration is applicable.


To meet USP requirements, an odor test of certain gaseous products is required prior to shipment of these products. This odor test is a part of the quality assurance testing of applicable cylinders, containers, and tank trucks, and is not the same as the test required of empty cylinders and containers received at the plant. This outgoing odor test must be performed during the quality assurance testing, by the individual performing the other quality assurance tests. THEORY The odor test uses the sense of smell to detect impurities in the gas. Human smell has been found to be a most sensitive and effective means of detecting many odors. Proper testing will confirm compliance with USP requirements.

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 5.31 MSA Infrared Analyzer

1. OBJECTIVE

This procedure establishes the MSA Infrared Analyzer.




4.1.1. an external sampling manifold is required to introduce the Sample, Span and Zero gases. The manifold also measures flow and safety exhausts all gases. This system must be free of all leaks.

4.1.2. the following gases must be supplied to the instrument: 4.1.2.1. Sample 4.1.2.2. Zero – a gas containing essentially none (less than 0.1 ppm) of the compound being

measured. 4.1.2.3. Span – a mixture containing more of the compound than the sample gas is expected to

contain. 4.1.3. Warning: Pressure regulation and suitable pressure relief devices must be provided if the above

gases are supplied in high-pressure cylinders. 4.1.4. Only regulators with metal diaphragms may be used. 4.1.5. Sufficient time must be allowed for the analyzer circuitry to warm up before the analyzer can be

operated. 4.1.6. The meter dumping shunt is for shipping purposes only. It must be removed prior to operation. 4.1.7. The analyzer should be protected from vibration and the elements.

4.2. TEST PROCEDURE 4.2.1. Introduce the Zero Gas to the analyzer. Set the flow rate according to the sheet posted inside

the analyzer front door. 4.2.2. Lock the control panel in a closed position. To do this, set the panel controls as follows: 4.2.3. Power OFF. 4.2.4. Zero to the factory setting listed on the data sheet inside the front door. 4.2.5. Span to the factory setting listed on the date sheet inside the front door. 4.2.6. The meter pointer should be on zero. If not, turn the Meter Adjust Screw until the pointer is on

zero. 4.2.7. Turn the Power Switch ON. The power light should come on. If not,

4.2.7.1. Check the wiring 4.2.7.2. Check the fuse on the front panel. The fuse holder will glow if the fuse is blown. If

necessary, install a fuse of the same type as the original. 4.2.8. When the power switch is first turned on, the heater will begin to warm up and the fan will

circulate air. Check to see that air is circulating in the analyzer. 4.2.9. Depress the Span Check Switch. The meter pointer must move upscale. 4.2.10. Release the Span Check Switch. 4.2.11. Let the analyzer warm up for at least 30 minutes. 4.2.12. Turn the Zero Knob until the meter reads 50 to 75% of full scale. 4.2.13. If you are using a recorder, check its reading. The recorder reading must agree with the

meter reading to + 1% of scale. 4.2.14. Turn the Zero Knob until the meter reads zero.

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4.2.15. Turn the Zero Knob counterclockwise. The meter pointer should go downscale past zero. Reset the meter to zero by slowly rotating the Zero Knob clockwise.

4.2.16. Introduce the Span Gas to the analyzer. 4.2.17. Turn the Span Knob until the meter indicates the known concentration of the Span Gas as

indicated on the cylinder. 4.2.18. Introduce the Zero Gas to the analyzer and recheck the zero setting. 4.2.19. The analyze is now ready for operation. Introduce the Sample Gas to the analyzer and use

the meter reading or the recorder chart reading in conjunction with the calibration curve to obtain the desired information.

4.3. EQUIPMENT CALIBRATION 4.3.1. The accuracy of this instrument depends on the ability to repeat the conditions of the zero and

span gases. This calibration is check prior to use. 4.4. REFERENCE TO STANDARDS

4.4.1. The zero and span gas cylinders are prepared and analyzed under laboratory conditions using accepted industry practices and standards, traceable to the National Bureau of Standards.

5. REFERENCES

GENERAL DESCRIPTION The MSA Model 202 LIRA Infrared Analyzer is a solid state, Luft type infrared analyzer used to determine the concentration of dissimilar compounds in a gas mixture. THEORY The infrared absorption of a compound is a characteristic of the type and arrangement of the atoms composing its molecules. Dissimilar compounds absorb in widely different spectral regions. For instance, carbon monoxide, carbon dioxide, water vapor, ammonia, and methane differ greatly in their absorption patterns. On the other hand, similar compounds have similar spectra. The absorption of ethane, propane, and butane is quite similar although there are regions of absorption difference. Fortunately, these differences are sufficiently marked so that it is possible to determine a small percentage of one of these gases in the presence of a much high concentration of the others. The analyzer is of the non-dispersive type, i.e., it is calibrated to monitor one specific component as opposed to the dispersive type, which scans the infrared spectrum to determine the presence of any infrared absorbing materials. Certain gases such as hydrogen, argon, oxygen and nitrogen do not absorb infrared energy and therefore their presence has no effect on this analyzer. The Model 202 LIRA Analyzer has two similar helices of nichrome wire to which a small d-c voltage is applied heating them to a point where they emit infrared energy. This energy is channeled through parallel optical paths, the sample cell and comparison cell, to a sensing element, the detector. The detector transforms the optical signal to an electrical signal which is then amplified so that is can be read on the meter or an external recorder.

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 5.32 Gas Detector Tubes

1. OBJECTIVE

This establishes the procedures for using gas detector tubes.




4.1.1. Only Draeger detector tubes can be used with the Draeger pump. 4.1.2. All detector tubes are ready for use, without prior mixing. 4.1.3. Both tips of each detector tube must be broken off to allow the sample to pass through the tube. 4.1.4. Warning: Use safety glasses and gloves for protection when breaking off the tube tips. 4.1.5. Install detector tubes as follows:

4.1.5.1. Unico tubes: the tip with the red dot must be nearest the pump inlet. 4.1.5.2. Gastec and Draeger tubes: the arrow must point toward the pump inlet. 4.1.5.3. Unico and Gastec tubes: the pump handle must be all the way in.

4.1.6. Detector tubes must not be used after the expiration date printed on the detector tube box. 4.2. TEST PROCEDURE

4.2.1. Connect one arm of a tee to the sample line using a gum rubber hose. Connect the other arm to the detector tube. Use of the tee allows the hand pump to pull a specified quantity of gas through the detector tube and prevents over pressurizing the tube.

4.2.2. Using the pump, pull the desired quantity of sample gas through the detector tube. 4.2.2.1. Unico and Gastec Pumps. Pull the handle all the way out for a 100 cc sample, halfway for

a 50 cc sample. After drawing the sample, lock the pump handle with a half turn. The required volume is specified in the detector tube instructions.

4.2.2.2. Draeger Pumps. To draw the correct quantity of sample gas using the Draeger pump, compress the bellows fully, then release it slowly until the arrestor chain is fully tensioned. The release (opening) period must last from 10 to 20 seconds or erroneous readings will result. The required number of compressions is specified in the detector tube instructions.

4.2.3. After waiting the prescribed amount of time, read the detector tube to determine the quantity of the impurity being tested for.

4.2.3.1. Unico and Gastec tubes. Read the length of the color stain on the tube and determine the ppm impurity directly or from a calibration chart, as appropriate.

4.2.3.2. Draeger tubes. Read the ppm impurity directly from the calibration scale on the tube. 4.2.4. Remove and discard the detector tube.

4.2.4.1. Unico and Gastec pumps. Release the handle with a half turn. If the handle moves backward by more than 1/4 –inch, reject the tube and retest. The proper volume was not obtained. Push the plunger in fully to discard the tube.

4.2.4.2. Draeger pumps. If steps 3 and 4 were performed properly, the reading is correct. Remove the tube from the pump and discard the tube.

4.2.5. Record the test results. 4.3. EQUIPMENT CALIBRATION

4.3.1. No field equipment calibration is required. Detector tubes are supplied sealed by the manufacturer and are discarded after use. All charts and scales used for measurement are also supplied. Calibration of detector tubes is valid until the expiration date.

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Precision gas detectors are portable, easy to operate instruments kits which allow rapid determination of gas and vapor concentrations.

THEORY Gas detector tubes determine the presence and quantities of impurities in a gas or vapor through a chemical reaction between each impurity and a specific reagent for the impurity. The chemical reagents are contained in glass detector tubes where they absorb and react with a measured volume of the sample being analyzed. The reaction between the reagent and the impurity produces a constant color stain the varies in length with the concentration of the impurity. The length of this stain can be read directly as quantity of impurity by volume.

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 5.33 Gow Mac Series 550 Gas Chromatograph

1. OBJECTIVE

This procedure establishes the Gow-Mac Series 550 Gas Chromatograph


3. RESPONSIBILITIES



4.1.1. If the gas chromatograph has been shut down for a times, as when the carrier gas cylinder is changed, follow the start-up procedures below:

4.1.2. Attach the regulator to the carrier gas cylinder. 4.1.3. Purge the regulator by pressurizing it and then slowly releasing the pressure 10 to 15 times to

remove any air. 4.1.4. Hook up the line from the regulator to the carrier gas inlet at the rear of the gas chromatograph. 4.1.5. Set the regulator to an outlet pressure of 30 psig. 4.1.6. Leak check the line and regulator with leak test solution. 4.1.7. Open the column oven and leak check the column connections. 4.1.8. Balance the flow through the columns to 10 cc/ 15 seconds by adjusting the two regulatory

valves on the front of the analyzer and measuring the carrier (helium) flow through the detector outlet with gas bubble meter.

4.1.9. Maintain these balance flows for 15 minutes to purge any air from the analyzer lines. 4.1.10. Turn the Current knobs completely counterclockwise. 4.1.11. Turn the analyzer Power ON. 4.1.12. Place the meter Function switch to BRIDGE CURRENT and raise the current slowly (by

increments of 20 mA every few minutes) with the Current knob until the meter indicates 120 mA. 4.1.13. Set the Function switch to DETECTOR TEMPERATURE and turn the Detector knob slowly

until the meter indicates 100 °C detector temperature. 4.1.14. Set the Function switch to COLUMN TEMPERATURE and check to see that the column

temperature is at ambient (slightly above 20 °C). 4.1.15. Let the analyzer come to equilibrium overnight. 4.1.16. Note: In most operations, once the above conditions have been established, the Gas

Chromatograph is left on with the carrier gas flowing. 4.2. TEST PROCEDURE:

4.2.1. Caution: The carrier gas must be flowing at all times while the analyzer power is on, or the detector filaments will be damaged. The only time the carrier gas may be turned off is during a system shutdown.

4.2.2. Set the Attenuation to “X 4” and the polarity to “+.” 4.2.3. Turn on the recorder and set the Range to 1.0 mV. 4.2.4. Turn the chart to cm/minute, set the chart speed to 2 cm/minute, and adjust the recorder zero

with the Gas Chromatograph Zero Control to just above zero on the chart (ten divisions). (A straight base line indicates good equilibrium.)

4.2.5. Hook up the regulator to the primary standard. Purge out the regulator 10 to 15 times. 4.2.6. Hook up the regulator to the calibration inlet on the side of the analyzer. Set the 3-way Gas

Sampling valve to the CAL position. 4.2.7. Set a flow of approximately 100 cc/minute through the sample loop and leak-check the lines and

regulators with leak detection solution. 4.2.8. Let the standard gas flow through the system for at least two minutes.

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4.2.9. Turn the Gas Sampling valve to the INJECT position, simultaneously marking the inject point on the recorder.

4.2.10. Note: If the peaks on the chart are negative, reverse the polarity of the Gas Chromatograph. 4.2.11. After the initial run, adjust the attenuation parameters to obtain the maximum sensitivity

required, ensuring that the peaks remain on-scale. 4.2.12. Re-inject the primary standard and make repeated runs until you obtain reproducible results.

Reproducible results are defined as results differing by + 1% between two or more successive runs.

4.2.13. Hook up the sample gas and repeat steps 4 through 9 to set up the exact conditions under which the standard gas was run.

4.2.14. Run the sample until you obtain reproducible results. (See step 10) 4.2.15. Calculate the concentration of the sample. 4.2.16. Turn the recorder power off, but leave the Gas Chromatograph power on.

4.3. EQUIPMENT CALIBRATION 4.3.1. The instrument is calibrated against a known primary standard reference gas prior to use.

Reproducibility of + 1% is required. 4.4. REFERENCE TO STANDARDS

4.4.1. The standards used are reference gases prepared and analyzed under laboratory conditions using accepted industry practices and standards traceable to the National Bureau of Standards.

4.5. EQUIVALENCY TO USP/NP TEST METHOD 4.5.1. This test method is equal in accuracy and reliability to the USP/NF method.

5. REFERENCES

GENERAL DESCRIPTION The Gow Mac Series 550 is a thermal conductivity gas chromatograph. It indicates the presence of and measures the quantity of components in the column effluent. The quantity of known gas components can be determined by reference to known standards. The gas chromatograph is connected to a linear strip chart recorder or equivalent device that provides a graph or numerical presentation of the output. THEORY The heart of a thermal conductivity gas chromatograph is a thermal conductivity detector, which measures the change in resistance of heated filaments exposed to a gas stream. A carrier gas flows through a cavity, which is generally contained in a metal block. Within the cavity are hot filaments that sustain heat losses to the block at a rate that depends upon the thermal conductivity of the gas. When the current passing through the filament remains constant, heat transfer is also constant as long as the gas or its flow rate are not changed. Equilibrium is established in the detector with the carrier gas. Then, when another gas, i.e., the sample or standard gas, is introduced into the cavity, the thermal conductivity of the gas changes the rate of heat transfer from the filaments to the block, which in turn changes the temperature of the filaments. The change in filament temperature causes a change in the filament resistance creating a voltage change across the filaments. The filaments form an electrical bridge circuit in which the change in voltage creates an imbalance. This imbalance causes a current to flow through the read-out device. The current acts as an analog signal, deflecting the recording pin, etc. in proportion to the difference in thermal conductivity between the carrier gas and the sample or standard gas.

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 5.34 Gow-Mac Thermal Conductivity Analyzer

1. OBJECTIVE

This procedure establishes the Gow-Mac Thermal Conductivity Analyzer.




4.1.1. Since this is a comparative test, a standard or calibration gas is necessary to establish the range of the sample gas. The quantities and components of the calibration gas should be the same as those of the desired mixture.

4.1.2. If cylinders with eductor tubes are being tested, vent a small quantity of the gas to purge the eductor tube. This is necessary to obtain a representative sample of the cylinder mixture.

4.1.3. A high detector current can burn out the filaments. 4.1.4. Recommended Bridge Currents of Binary Mixtures: Mixture: Bridge Current: All mixtures with Balance Air 130 mA All mixtures with Balance Argon 100 mA All mixtures with Balance Carbon Dioxide 100 mA All mixtures with Balance Nitrogen 130 mA All mixtures with > 95% Helium 250 mA All mixtures with > Hydrogen 250 mA

Note: For mixtures with < 95% Helium or Hydrogen, set the Bridge Current 20 mA greater than the minimum current setting required to obtain the desired meter span calibration reading.

4.2. TEST PROCEDURE: 4.2.1. Connect both the Zero Gas and Calibration Gas cylinders to the Reference Inlet and the

Sample Inlet. Set the Gas Selector Valve to the ZERO position. 4.2.2. Warning: Pressure regulation and suitable pressure-relief devices must be provided when high-

pressure cylinders are used. 4.2.3. Adjust both rotameter valves until both the Reference Flow and Sample Flow rotameters

indicate 1.0cfh gas flow through both the Sample and Reference Flow System. 4.2.4. Turn the Current Control Knob fully counterclockwise. 4.2.5. Turn the analyzer ON. 4.2.6. Adjust the Current Control Knob until the current is at the proper setting as indicated on the

milliameter. 4.2.7. Caution: An excessive current will damage the detector filaments. 4.2.8. allow 15 minutes for the instrument to stabilize. 4.2.9. Adjust the Zero Control until the readout meter indicates “0.” 4.2.10. Turn the Gas Selector Valve to SAMPLE. Adjust both rotameters to a flow of 1.0 cfh. 4.2.11. Set the Polarity Switch to the position that causes the readout meter to deflect upscale. 4.2.12. Adjust the Calibration Control until the meter readout agrees with the value of the Calibration

Gas Cylinder. 4.2.13. Turn the Gas Selector Valve to the ZERO position and repeat Steps 7-10. 4.2.14. Turn the Gas Selector Valve to the ZERO position. Disconnect the Calibration Gas cylinder

and connect the Sample Gas cylinder to the Sample Inlet. 4.2.15. Turn the Gas Selector Valve to the SAMPLE position. Adjust the SAMPLE rotameter for a

flow of 1.0 cfh. 4.2.16. Allow five minutes for the instrument to stabilize.

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4.2.17. read the analysis of the Sample Gas directly from the meter scale. 4.2.18. Repeat Steps 13-15 until you obtain reproducible results (1% precision).

4.3. EQUIPMENT CALIBRATION 4.3.1. The instrument is calibrated against a Primary Standard Calibration Gas prior to use.

Reproducibility of the + 1% is required. 4.4. REFERENCES TO STANDARDS

4.4.1. Zero and Calibration Gas cylinders are prepared and analyzed under laboratory conditions using accepted industry practices and standards, traceable to the National Bureau of Standards.

5. REFERENCES

GENERAL DESCRIPTION: The Gow-Mac Thermal Conductivity Analyzer is a panel or shelf mounted analyzer used for non-continuous sampling and quantitative analysis of binary gas mixtures and gas purity measurements.

THEORY The Gow-Mac Gas Master is a thermal conductivity analyzer, the heart of which is a thermal conductivity cell that measures the change in the resistance of heated filaments exposed to a gas stream. The cell is made up of four helical sensing elements or filaments, electrically-heated, and arranged in a balanced Wheatstone bridge circuit.

The detector cell is balanced by passing a reference gas through both the sample and reference flow systems. Then, when a sample gas of difference composition from the reference gas is introduced to the sample system, the electrical resistance of the sensing elements increases or decreases according to the thermal conductivity of the gas. This change in the rate of heat loss from the filaments causes the Wheatstone bridge circuit to become unbalanced. The output voltage created by this imbalance is fed into a calibrated analog meter and the gas analysis can be read directly from the meter scale.

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 5.35 Beckman Hydrocarbon Analyzer – Model 400

1. OBJECTIVE

This procedure establishes the Beckman Hydrocarbon Analyzer – Model 400.


3. RESPONSIBILITIES



4.1.1. Warning: This analyzer can explode if not properly configured and installed. Proper ventilation (item 1), automatic fuel and sample shutdown systems (item 2), a spring-back fuel shutdown switch (item 3), and the flow restrictor (item 11) must be installed as indicated to assure safe operation.

4.1.2. The analyzer must be properly vented to prevent build-up of flammable gas. 4.1.2.1. Either the top must be louvered or the case vented. 4.1.2.2. Gas from the vents must exhaust to the outside of the building.

4.1.3. An automatic, solenoid-activated Fuel Shut-Off System must be installed and working. 4.1.4. Note: At Packaged Gases locations, an automatic, solenoid-activated shut-off system is

required for the Sample Gas as well as the Fuel Gas. Dual shut-off systems are also required for Bulk Gases applications if the Sample Gas is flammable. The Fuel Shut-Off Assembly and Fuel Shut-Off Solenoid must be ordered for the Model 400. They are standard on the Model 400A.

4.1.5. The analyzer start-up fuel shutdown override system must have a spring-back override switch. 4.1.6. the required switch is standard equipment on the Model 400A. It must be installed on the Model

400. 4.1.7. Only small-diameter (1/8 inch O.D.) stainless steel, seamless tubing may be used for the

sample lines. 4.1.8. Gas flow systems must be leak tight. 4.1.9. Quick disconnects must not be used at pressures above 30 psig. 4.1.10. Sample flow for flammable gas samples must not exceed 500 cc/min. 4.1.11. The analyzer must be installed in a clean area, not subject to excessive vibration or extreme

temperature. 4.1.12. Warning: High pressure gases pose a hazard to personnel and equipment. Pressure

regulation and suitable pressure relief devices must be provided when high-pressure cylinders are used.

4.1.13. Inlet pressure to the analyzer must not exceed 200 psig. 4.1.14. Only metal diaphragm regulators may be used for pressure regulation. Do NOT use

composition diaphragm regulators. 4.1.15. The following gases must be supplied to the analyzer. 4.1.16. Caution: If 100% hydrogen is supplied to the analyzer as fuel, an adequate flow of sample or

other diluent gas must enter the Sample Inlet at all times while the flame is burning. If not, the tip of the burner will overheat and be damaged. The proper flow restrictor specified in the instruction manual must also be installed.

4.1.17. Note: A Fuel Restrictor is required for all applications. A Sample Restrictor is also required for ALL Packaged Gases applications and for Bulk Gases applications involving flammable samples.

4.1.18. Fuel gas – pure H2, zero or 40/60 H2/N2 Flame Ionization Detector (FID) mixture – see instruction manual

4.1.19. Air – Hydrocarbon Free Grade

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4.1.20. Zero Gas – a cylinder certified to be < 0.2 ppm Total Hydrocarbons (THC) 4.1.21. Span gas – a cylinder certified to be between 5.0ppm and 10.0m ppm THC 4.1.22. Sample gas. 4.1.23. The analyzer may show baseline drift immediately after a start-up. This drift is evidence that

the circuitry has not warmed up. 4.1.23.1. To obtain accurate sample readings, allow sufficient warm-up time: ensure the meter

is steady before taking sample readings. 4.1.24. To minimize system response time, gas discharge from the By-pass Outlet must be at 2.0 to

3.0 liters/min. 4.1.25. For safety the system must be shut down properly. 4.1.26. Always turn the fuel gas off first, then the air and sample gases.

4.2. TEST PROCEDURES 4.2.1. With all gases turned off, set the Range Multiplier to “1000” and turn the Power Switch ON. The

indicator lamp should light. 4.2.2. Set the regulators on the air and fuel gas cylinders for suitable output pressures (25 psig to 200

psig maximum). 4.2.3. Set the analyzer internal Air Pressure Regulator to 5 psig (6 psig if 100% H2 fuel is used). 4.2.4. Place the Fuel Shut-Off Override Switch in the OVERRIDE position. Hold the switch in this

position during flam ignition. 4.2.5. Set the analyzer internal Fuel Pressure Regulator to 25 psig (30 psig if 100% H2 fuel is used). 4.2.6. Wait about one minute for the fuel gas to purge the flow system. During this period, rotate the

Fuel Pressure Regulator alternately clockwise and counterclockwise several times, then return it to the setting specified in step 5.

4.2.7. Set the Range Multiplier Switch to “1.” 4.2.8. Hold the ignite switch on for about five seconds, then release it. The Flame Out Meter will

indicate that the flame is burning. 4.2.9. If the Flame Out Meter does not indicate flame ignition, repeat Step 8. If the flame still fails to

light, it may be necessary to increase air pressure to 7 psig (step 3) and fuel pressure to 30 psig (step 5).

4.2.10. When the flame ignites, increase the setting of the internal Air Pressure Regulator to at least 15 psig. The recommended operating settings for the internal pressure regulators are as follows:

4.2.10.1. Air Pressure Regulator – 15 to 30 psig. 4.2.10.2. Fuel Pressure Regulator – 25 to 30 psig.

4.2.11. Note: the Flame Out Meter should still indicate flame ignition. 4.2.12. Release the Fuel Shut-Off Override Switch to the NORMAL position. 4.2.13. Supply the Zero Gas to the Sample Inlet. Adjust the external flow controller so that the flow

discharged from the By-Pass Outlet is between 2.0 and 3.0 liters/min. Set the internal Sample Pressure Regulator to approximately 5 psig.

4.2.14. Set the Range Multiplier Switch to “10” and the Span control to “1000.” 4.2.15. By rotating the Zero Adjust, set the meter to read the hydrocarbon content of the Zero Gas. 4.2.16. Close the Zero Gas supply and supply Span Gas to the sample inlet. Adjust the external flow

controller so that flow discharged from the By-Pass Outlet is between 2.0 and 3.0 liters/min. Verify that the reading on the internal Sample Pressure Gauge is 5 psig; if not, adjust the internal Sample Pressure Regulator to obtain 5 psig.

4.2.17. Set the Range Multiplier Switch to the appropriate position. 4.2.18. Adjust the Span Control so that the meter indicates the hydrocarbon content of the Span

Gas. Lock the Span Control by pushing the lever down. 4.2.19. Recheck the Zero setting following Steps 12 and 14. Lock the Zero Control by pushing the

lever down. 4.2.20. Supply the Sample Gas to the Sample Inlet. Adjust the external flow controller so that the

flow discharged from the By-Pass Outlet is between 2.0 and 3.0 liters/min. The Sample Pressure Gauge should read 5 psig.

4.2.21. Set the Range Multiplier Switch to the appropriate position. After the meter has stabilized, read the hydrocarbon content of the sample as methane.

4.2.22. Note: for analysis of fuel-type gases (hydrogen, its isotopes, and its non-carbon-based compounds) sample pressures below 5 psig may be required to achieve correct Zero and Span settings

4.3. EQUIPMENT CALIBRATION

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4.3.1. The accuracy of this instrument depends on the ability to repeat the conditions of the zero and span gases. This check, which is performed as part of the “Test Procedure” prior to reading the hydrocarbon content of the sample, is recorded on an Equipment Calibration Log. Please note that the balance gas of the zero and span gas should be the same gas as the sample being tested.

4.3.2. To ensure accuracy of the low range ( < 10 ppm) hydrocarbon analyses, the battery must be tested every six months as described under “Battery Check.”

4.4. BATTERY CHECK (MODEL 400 ONLY) 4.4.1. The Model 400 analyzer has an Eveready 90 VDC 205 NEDA 490 polarizing battery located

inside the case. Improper low range hydrocarbon analysis readings may result if the battery is not fully operational at 90 VDC. Every six months, check the battery as follows.

4.4.2. Shut off all gas flow to the analyzer. 4.4.3. Turn the POWER switch to OFF, and disconnect the analyzer from its power source. 4.4.4. Permit the analyzer to cool down to 70°F, then remove the connections from the positive (+)

and negative (-) battery terminals. 4.4.5. Using a suitable voltmeter, check the battery voltage. Replace the battery if the meter indicates

less than 90 VDC. 4.4.6. Tag the battery, indicating the test/replacement date, and record this information on the

Equipment Calibration Log. 4.4.7. Note: Replacement batteries may be purchased locally.

4.5. REFERENCE TO STANDARDS 4.5.1. Reference gases are prepared and analyzed under laboratory conditions using accepted

industry practices and standards traceable to the National Institute of Standards and Technology (NIST).

5. REFERENCES

GENERAL DESCRIPTION The Beckman Model 400/400A Hydrocarbon Analyzer is an automatic, continuous analyzer that measures the concentration of hydrocarbons in a gas stream.

THEORY The Beckman Model 400 Hydrocarbon Analyzer uses a flame ionization detector to determine the concentration of hydrocarbons in a sample gas stream. The flame ionization detector consists of a manifold containing a gas jet burner and an ion collector. The burner and the collector are oppositely polarized by a 90-volt power source: the gas jet receives a positive charge; the collector, a negative charge. The detector manifold funnels regulated flows of the sample and a fuel gas (hydrogen, or a mixture of hydrogen and another gas) through the gas jet. Emerging from the jet, the gases ignite and are burned, sustaining a flame. Oxygen, the other necessary ingredient of the flame, is supplied by a stream of regulated air directed around it. In the combustion process, the flame dissociates hydrocarbons in the sample gas stream into electrons and positive ions. In the electrostatic field created by the 90-volt potential between the collector and the burner jet, the negative electrons migrate to the positively charged jet, while the positive irons migrate to the negatively charged collector. The accumulation of oppositely charged particles – positive ions on the gas jet, negative electrons on the collector – causes an electrical imbalance that creates a small “ionization” current in the meter circuit. This current, which is proportional to the rate at which carbon atoms enter the burner, is a measure of the concentration of hydrocarbons in the original sample.

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 5.36 Teledyne Trace Oxygen Analyzer Model 316

1. OBJECTIVE

This procedure establishes the Teledyne Trace Oxygen Analyzer Model 316.


3. RESPONSIBILITIES



4.1.1. The analyzer must be installed level in an area that is sheltered from the elements. Auxiliary heating must be provided if the ambient temperature is expected to drop below 32°F.

4.1.2. Because very small (trace) quantities of oxygen must be detected, the system must be free of all leaks. Sample lines must be entirely of metal.

4.1.3. WARNING: Pressure regulation and suitable pressure relief devices must be provided when high-pressure cylinders are used.

4.1.4. Only regulators with metallic diaphragms should be used for high pressure cylinder analyses. 4.1.5. Sample inlet pressure should be between 5 and 50 psig (10 psig nominal). 4.1.6. A controlled sample flowrate is required for proper operation and linearity of cell response. 4.1.7. All necessary hardware and fittings upstream of the analyzer should be leak-tested under

pressure prior to startup. 4.1.8. When stopping gas flow to the instrument, reduce the sample flowrate, close the cell shutoff

valve, and then close the throttle valve completely. This sequence minimizes diffusion of air into the instrument, maintaining the fuel cell in a low-ppm environment.

4.1.9. The fuel cell is a sealed electrochemical transducer and requires no electrolyte. 4.1.10. The fuel cell life is 80,000% hours or greater. 4.1.11. The analyzer should not be used in applications where carbon dioxide is the major

component of the sample. 4.2. TEST PROCEDURE

4.2.1. With the Power OFF and the Range Switch in any position but OFF, check alignment of the meter pointer with the zero mark on the scale. Adjust the screw on the face of the meter if necessary until the pointer and zero mark are aligned.

4.2.2. Turn the Power ON. 4.2.3. Turn the Range Switch to X100 and watch the meter until the pointer comes to rest somewhere

on the scale. 4.2.4. Establish a sample gas flow to the analyzer. 4.2.5. Open the Cell Shutoff Valve. 4.2.6. Open the Throttle Valve and adjust it until the Flowmeter indicates a flowrate of 2.0 scfh (1000

cc/min). 4.2.7. Adjust the sample pressure so the analyzer inlet pressure is nominally at 10 psig. 4.2.8. Turn the Range Switch to X1000. 4.2.9. Turn the Range Switch to the appropriate range, allow the reading to stabilize, and then read

the oxygen content directly in ppm. 4.3. EQUIPMENT CALIBRATION

4.3.1. Calibrate the Teledyne Trace Model 316 Oxygen Analyzer once a month for Bulk Gas operations and once a week for Packaged/Specialty Gas operations. Please note: A new cell cannot be calibrated for 24 hours.

4.4. Calibration with a Certification Gas

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4.4.1. The recommended method of calibration is to use a certified calibration cylinder containing 8-10 ppm oxygen, balance nitrogen.

4.4.2. Introduce the calibration gas into the analyzer. 4.4.3. Wait until the reading stabilizes. 4.4.4. Adjust the Span Adjust so that the meter reads the oxygen content contained in the calibration

gas cylinder. 4.4.5. For critical high-technology accounts, an additional 1-3 ppm oxygen, balance nitrogen standard

is required to ensure there are no leaks in the sampling system. If there are no leaks the 1-3ppm oxygen standard should read + 0.1 ppm. If it does not read correctly, check the sampling system for leaks.

4.5. Calibration with Ambient Air 4.5.1. Ambient air should be used to calibrate the analyzer only in an emergency. Such calibrations

should be followed immediately by purging with a gas containing little or no oxygen. 4.5.2. The special “CAL” range of the instrument features a mark that coincides with 209,000 ppm

oxygen concentration of air. 4.5.3. Position the Range Switch on CAL and adjust the Span Control so that the indicator pointer is

on the meter CAL mark. 4.5.4. Purge the instrument overnight with the sample gas. 4.5.5. Note: The instrument should recover to 1 ppm resolution after this purge. 4.5.6. When a cylinder is used to calibrate the instrument, use a Primary Standard Reference Gas.


industry practices and standards traceable to the National Bureau of Standards. 4.7. EQUIVALENCY TO USP/NF TEST METHOD


GENERAL DESCRIPTION: The Teledyne Analytical Instruments Model 316 is a panel-mounted, solid state trace oxygen analyzer that utilizes an electrochemical fuel cell to measure the concentration of oxygen in a gas stream.

THEORY The oxygen in the sample stream is sensed by a small fuel cell. Oxygen diffusing into the cell reacts chemically to produce an electrical current that is proportional to the oxygen concentration in the gas phase immediately adjacent to the cell’s sensing surface. The minute but linear signal produced by the cell is amplified by a two stage solid state amplifier in which power consumption per stage is less than three milliwatts. This amplified signal is read out on a precision panel meter.

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 5.37 Teledyne 320 Series Oxygen Analyzer

1. OBJECTIVE

This procedure establishes the Teledyne 320 Series Oxygen Analyzer.




4.1.1. Remove the cell-sealing cap from the measuring probe. This cap keeps oxygen from the cell when the probe is mounted in its holder and the instrument is not in use.

4.1.2. The micro-fuel cell has a life expectancy of 80,000% hours (approximately six months) or more in air at 75°F. As the cell nears the end of its life, the meter readings will first become erratic and then drop off sharply to zero.

4.1.3. Use the Axial Flow Inlet for flow rates of less than 3000 cc/min and the Radial flow Inlet for flow rates of greater than 3000 cc/min. The Axial Flow Inlet provides rapid purging of the dead volume of gas in the cell at start-up. If this inlet is used at flowrates greater than 3000 cc/min, however, erroneously high readings of oxygen content will result.

4.1.4. If the batteries in the Models 320B/RC and 320B/RCD require changing, ensure that the Selector Switch is in the OFF position before commencing charging.

4.2. TEST PROCEDURE 4.2.1. Always check the analyzer with air prior to use. It must read 21 + oxygen. 4.2.2. Introduce the sample gas to the proper inlet. 4.2.3. Turn the Range Switch to the appropriate range (not applicable to the digital model) 4.2.4. When the reading has stabilized, read directly the percent of oxygen in the sample.

4.3. EQUIPMENT CALIBRATION 4.3.1. Calibrate the instrument with air prior to use. 4.3.2. Take an air sample or use a primary standard consisting of 21% oxygen and 79% nitrogen. 4.3.3. Select the 0-25% scale on the Range Switch (not applicable to digital models). 4.3.4. Rotate the Span Control until the meter pointer coincides with the red mark that extends into the

meter scale (analog models only). 4.3.5. Read the meter or digital display. 4.3.6. For analog models, you must obtain a reading of 21 + 2% oxygen. For digital models this

reading must be 21 +%. 4.4. REFERENCE TO STANDARDS

4.4.1. Standard gases are prepared and analyzed under laboratory conditions using accepted industry practices and standards traceable to the National Institute of Standards Technology (NIST).

4.5. EQUIVALENCY TO USP/NF TEST METHOD 4.6. This test method is equal in accuracy and reliability to the USP/NF method. The digital readout

models comply with the requirements of Air, USP testing. 5. REFERENCES GENERAL DESCRIPTION

Teledyne Analytical Instruments Series 320 Oxygen Analyzers are portable instruments that continuously measure the percentage of oxygen in a gas atmosphere. The analyzer cell is specific for oxygen, has an absolute zero, produces a linear output from 0-100% oxygen, and requires no zero gas. Models 320C/D and 320B/RCD have a digital output, a feature required for compliance with the requirements for Air, USP testing.

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THEORY The oxygen in a sample stream is sensed by Teledyne Analytical Instruments’ patented micro-fuel cell, a sealed electrochemical transducer. A portion of the sample product is taken into the cell through a measuring probe. The cell consumes the oxygen from the sample, producing an electrical current proportional to the concentration of oxygen in the sample. This current is amplified and displayed on a precision meter.

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 5.38 Teledyne Trace Oxygen Analyzer Model 311

1. OBJECTIVE

This procedure establishes the Teledyne Trace Oxygen Analyzer Model 311.




4.1.1. Because very small (trace) quantities of oxygen must be detected, the system must be free of all leak. Sample lines must be entirely of metal.

4.1.2. CAUTION: Pressure regulation and suitable pressure relief devices must be provided when high pressure cylinders are analyzed.

4.1.3. Only regulators with metallic diaphragms should be used for high pressure cylinder analyses. 4.1.4. A controlled sample flowrate is required for proper operation and linearity of cell response. 4.1.5. The fuel cell is a sealed electrochemical transducer and requires no electrolyte. 4.1.6. The detector cell life is 80,000% hours or greater. 4.1.7. The differential power requirement (plus and minus 3.6 volts DC) of the instrument amplifier is

furnished by two internally-mounted, 750 milliampere-hour nickel-cadmium batteries. 4.1.8. NOTE: An Integral charging circuit and a detachable power cord are provided so that the

batteries may be recharged overnight from a 110-volt convenience outlet. Do this once a month. 4.1.9. The instrument should always be purged with the sample or an inert gas before it is taken out of

service for standby or storage. Purging extends cell life and minimizes the time required for the next analysis.

4.1.10. The analyzer should not be used in applications where carbon dioxide is the major component of the sample.

4.2. TEST PROCEDURE 4.2.1. With the Range switch in the OFF position, check the alignment of the meter pointer with the

zero mark on the scale. Adjust the screw on the face of the meter, if necessary, until the pointer and zero mark are aligned.

4.2.2. Before making any connections to the analyzer, establish a sample flowrate and allow the sample to vent to the atmosphere long enough to purge the air from the line.

4.2.3. Connect the vent fitting first and then introduce the sample via the quick-disconnect fitting on the rear of the analyzer.

4.2.4. CAUTION: If a flowing sample is connected to the manifold without the vent fitting in place, the manifold pressure will rise almost immediately to equal the sample pressure, possibly causing permanent damage to the cell.

4.2.5. Turn the Range switch to “X1000.” 4.2.6. Turn the Range switch to the appropriate range, allow the reading to stabilize, and read the

oxygen content directly in ppm. 4.3. EQUIPMENT CALIBRATION

4.3.1. Calibration should be checked once a month. Do not calibrate the instrument unless there is a trace oxygen gas readily available for purging immediately following the calibration procedure.

4.3.2. The special “CAL” range of the instrument features a mark that coincides with the 209,000 ppm oxygen concentration of air. Position the Range Switch on CAL and adjust the Span Control so that the indicating pointer is in on the meter CAL mark.

4.3.3. The instrument may be calibrated using either air or a known Primary Standard Reference Gas. After calibration, the instrument will come to equilibrium within a half hour so that low ppm readings can be taken.

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GENERAL DESCRIPTION The Teledyne Analytical Instruments Model 311 is a portable trace oxygen analyzer which can be operated without an external power source and can be reliably calibrated.

THEORY The oxygen in the sample stream is sensed by a small fuel cell. Oxygen diffusing into the cell reacts chemically to produce an electrical current that is proportional to the oxygen concentration in the gas phase immediately adjacent to the cell’s sensing surface. The minute but linear signal produced by the cell is amplified by a two stage solid state amplifier in which power consumption per stage is less than three milliwatts. This amplified signal is read out on a precision panel meter.

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 5.39 Delphi Electrochemical Oxygen Analyzer

1. OBJECTIVE

This procedure establishes the Delphi Electrochemical Oxygen Analyzer.




4.1.1. To analyze for trace quantities of oxygen, the system must be free of all leaks. Sample lines must be all metal, preferably stainless steel.

4.1.2. The analyzer must be installed level to maintain adequate fluid levels. 4.1.3. The analyzer should be located in an area free of vibration, drafts, and temperature extremes. 4.1.4. The water reservoir for the humidifier must be filled with clean, distilled water. 4.1.5. The electrolyte solution, consisting of reagent grade potassium hydroxide (KOH) and clean,

distilled water, must be freshly prepared to the manufacturer’s recommended strength. 4.1.6. WARNING: Potassium hydroxide is a strong caustic that will cause severe burns. Safety

glasses and protective clothing must be worn when handling this caustic. Have water available to wash off the chemical in case of spills.

4.1.7. The electrolyte level must be maintained as specified. 4.1.8. The analyzer is intended for continuous use. 4.1.9. CAUTION: Pressure regulation and suitable pressure relief devices must be provided when

analyzing high pressure cylinders. 4.1.10. Only regulators with metallic diaphragms should be used when analyzing high-pressure

cylinders. 4.1.11. Gas streams containing acidic anhydrides, halogens (Cl2, Br, F, or I), or sulfur compounds

(H2S, SO2, or mercaptans) must not be introduced to the analyzer. If these compounds are present in the sample, a caustic pre-scrubber must be installed.

4.1.12. The instrument should never be allowed to run with the sample flowing and the power off for any extended period. This will cause the water from the reservoir and the cell electrolyte to evaporate.

4.2. TEST PROCEDURE 4.2.1. Turn the power supply ON. 4.2.2. Visually check for proper water (reservoir) and electrolyte (cell) levels. 4.2.3. Place the Range switch in position 2. 4.2.4. Introduce the sample and adjust the flow rate to 150 cc/min. 4.2.5. When the instrument has stabilized, the trace oxygen content of the sample stream can be read

directly from the recorder or indicator. The position of the Range switch must be considered in obtaining the correct multiplier.

4.3. EQUIPMENT CALIBRATION 4.3.1. The analyzer has an internal calibration circuit, which can be adjusted to introduce a known

quantity of oxygen into the sample stream. The heart of this calibration circuit is an electrolysis cell, an electrical device that separates water into hydrogen and oxygen. Power to the calibration circuit is controlled by a separate on/off switch located next to the switch that controls power to the analyzer. When the circuit is on, current to the electrolysis cell can be adjusted with the Calibrator knob. When the current and sample flow rate are adjusted accurately, the trace quantity of oxygen added to the sample stream can be calculated as explained below.

4.3.2. The analyzer does not require a “zero” standardization because the electrochemical measuring cell has an “absolute” zero. The cell requires oxygen to produce an output current, and when no

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oxygen is present, no current flows. Only a span calibration is required to completely calibrate the analyzer within the ranges specified.

4.3.3. The analyzer is wired so the recorder or indicator used to measure oxygen concentration can also be used to measure the current applied to the electrolysis cell. This calibrator current, which is adjusted with a rheostat, can be read on the recorder or indicator when the Range switch is in the CAL position. When the desired current has been set, the ppm oxygen introduced into the sample stream can be read by switching to the appropriate range while keeping the calibrator current on.

4.3.4. At a flow rate of 150 cc/min, each milliampere of calibrator current will add 25 ppm of oxygen to the sample stream, i.e. 1 mA adds 25 ppm, 2 mA adds 50 ppm, etc.

4.3.5. To calibrate the instrument, proceed as follows: 4.3.5.1. Adjust the analyzer flow rate to 150 cc/min. Note the recorder or indicator reading (in ppm

oxygen). 4.3.5.2. Turn the Range switch to CAL position and turn the Calib switch ON. 4.3.5.3. Adjust the calibrator current to a value such that the selected current and flow rate

combination produce an amount of oxygen equivalent to at least 50% of the highest analyzer range. You can read the current directly from the recorder or indicator because the Range switch is in CAL.

4.3.5.4. Switch to RANGE 2, leaving the flow rate and calibrator current as adjusted. The calibrator is now adding the calculated ppm oxygen to the sample stream. The recorder or indicator will go upscale to indicate the ppm oxygen now in the sample stream. This should be the original reading obtained in step 1 plus the calculated amount added by the calibrator. If the proper reading is not indicated after 15 minutes, adjust the Span potentiometer dial to obtain the proper reading. Allow several more minutes after the Span adjustment before taking a final reading.

4.3.5.5. When the recorder or indicator reaches the proper reading, turn off the calibrator current. The recorder or indicator will now go downscale and indicate the amount of oxygen in the sample gas. If this reading is the same as that obtained in step 1, the instrument is calibrated. If not – and this occurs whenever a span adjustment was required in step 4 – the new value must be used as a starting point (step 1) and the calibration repeated until the readings (step 1 and step 5) coincide.

4.3.5.6. Alternately, the analyzer can be calibrated by connecting a primary standard reference gas of known oxygen content to the sample inlet and adjusting the instrument until the recorder or indicator reads the oxygen content of the standard. If the recorder or indicator reads the value recorded on the cylinder body label the instrument is calibrated. If the reading, in ppm, is not the same as the figure on the cylinder label, the recorder or indicator is adjusted to read that value with the Span potentiometer. After the adjustment, the gas flow should be turned off and the calibration procedures repeated to ensure that the correct value is obtained.

4.3.5.7. Calibrate the analyzer once a month, after each setup, or after a change of cell electrolyte. Primary Standard As the electrolyte ages, you will lose sufficient Span adjustment and will be unable to calibrate the instrument properly. When this occurs, replace the electrolyte with a freshly prepared solution and recalibrate the analyzer.



4.5.1. This test method is equal in accuracy and reliability to the USP/NF method. 5. REFERENCES GENERAL DESCRIPTION

The Delphi Electrochemical Oxygen Analyzer is a panel mounted, continuous use device that measures trace quantities of oxygen by consuming the oxygen and generating a proportional electric current. This current flows through a resistance producing a voltage which can be monitored by a self-balancing potentiometer to indicate the amount of oxygen present. THEORY Oxygen reaching a silver surface will rapidly oxidize the surface to silver oxide. The silver oxide forms a thin protective layer preventing further oxidation of the silver mass. The energy of formation of the

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silver oxide is very low and therefore the process is easily reversed by moderate temperature (300oC) or electrochemical action. In fact, a small battery may be formed using an oxidized silver plate or screen as the positive electrode, a piece of lead as the negative electrode, and an alkali metal hydroxide as the electrolyte. When the electrodes of this “battery” are connected, a short pulse of current will be produced as the silver oxide is reduced to silver metal. The oxygen reacts with the water and electrons from the circuit to form hydroxyl ions which oxidize the lead to form lead oxide, water, and electrons. This action is represented by the following equations:

Ag2O + H2O + 2e- → 2Ag + 2OH- at the silver cathode Pb + 2OH- → PbO + H2O + 2e- at the lead anode

The lead oxide is soluble in excess hydroxyl so it dissolves into the electrolyte. In effect, the oxygen has been transferred from the silver cathode to the lead anode, while electrons flow in the external circuit. As soon as all the silver oxide has been converted, the current ceases to flow until more oxygen reaches the silver and forms more silver oxide. In the Delphi Model A cell, the lead rod (the anode) is entirely immersed in the electrolyte. The cathode, a series of silver sheets supported by a silver channel in the center of the cell cavity, dips into the electrolyte. A thin electrolyte film forms on the surface of the cathode sheets, above the electrolyte. The current produced by this system is proportional to the percentage of oxygen in the gas passing over the pool and contacting the film on the sheets. The system has an absolute zero. If there is no oxygen in the sample gas, no current flows. A built-in electrolytic cell is used to set the span of the analyzer.

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 5.40 Teledyne Trace Oxygen Analyzer

1. OBJECTIVE

This procedure establishes the Teledyne Trace Oxygen Analyzer.




4.1.1. In order to analyze for trace quantities of oxygen, the system must be free of all leaks. Sample lines must be entirely metallic.

4.1.2. The analyzer must be installed level to maintain adequate fluid levels. 4.1.3. The water reservoir which supplies the humidifier must be filled with clean distilled water. 4.1.4. The electrolyte solution, consisting of reagent grade potassium hydroxide (KOH) and clean

distilled water, must be freshly prepared to the manufacturer’s recommended strength. 4.1.5. WARNING: Potassium hydroxide is a strong caustic that will cause sever burns. Safety goggles

or a face shield, and protective clothing must be worn when handling this caustic. Have water available to wash off chemical in case of accidental spills.

4.1.6. The electrolyte level must cover the bottom 3/32-inch of the silver screens of the electrochemical cell.

4.1.7. The silver screens of the electrochemical cell must be kept clean. 4.1.8. A controlled sample flow rate between 150 cc/min and 300 cc/min is required for proper

operation and linearity of cell response. 4.1.9. Only regulators with metallic diaphragms should be used when high-pressure cylinders are

being analyzed. 4.1.10. WARNING: Pressure regulation and suitable pressure relief devices must be provided when

high-pressure cylinders are used. 4.1.11. The analyzer is intended for continuous use. 4.1.12. Do not introduce gas streams containing acidic anhydrides or mercaptans to the analyzer. If

these compounds are present, and caustic pre-scrubber must be installed. 4.2. TEST PROCEDURE

4.2.1. Turn the Power switch ON. 4.2.2. Select the appropriate range on the Output Selector or Range switch. 4.2.3. Visually check for the proper water (reservoir) and electrolyte (electrochemical measuring cell)

levels. 4.2.4. Introduce the sample and adjust the flow rate to 150 cc/min. 4.2.5. When the instrument has stabilized, read the trace oxygen content, in ppm, directly from the

read-out device (recorder or digital voltmeter). 4.3. EQUIPMENT CALIBRATION

4.3.1. The analyzer has an internal calibration circuit – an electrolysis cell that electrolyzes water into hydrogen and oxygen when current is applied to the calibrator. By accurately adjusting the sample flow rate and the current applied to the calibrator using flow rate and current values obtained from a nomograph (Figure 1), the operator can produce a known quantity of oxygen for calibration.

4.3.2. The analyzer has an absolute zero and no zero adjustment is required for calibration purposes. The electrochemical measuring cell requires oxygen to produce an output current; if no oxygen is present, no current flows. Only a span calibration is required for complete calibration of the analyzer within the ranges specified.

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4.3.3. The concentration of oxygen added to the sample stream by the calibration can be determined using the following formula:

Ppm O2 = 3750* X calibrator current in milliamperes Sample flow rate in cc/min * Based on the liberation of 3/75 cc/min O2 (NTP) by a one-ampere current

4.3.4. Thus, with a sample flow rate of 150 cc/min, 1 milliamp of calibration current produces 25 ppm

of oxygen, 2 milliamperes produce 50 ppm, 20 milliamperes produces 500 ppm, etc. For simplicity, the relationships shown in the above formula have been incorporated into a nomograph (Figure 1) which may be used instead of the formula.

4.3.5. The electrical circuitry of the analyzer is arranged so that the readout device used to measure the oxygen concentration can also be used to measure the current applied to the calibrator. The Output Selector or Range switch allows the user to monitor the ppm of oxygen in various ranges or the milliampere output of the calibrator. The calibrator current is adjusted with a rheostat. The calibrator current can be read on the readout device when the Calibrator switch is ON or when the Output Selector switch is in the CAL position. When the Output Selector or Range switch is switched to the appropriate range, with the calibrator current left on, the ppm oxygen produced by the calibrator can be read on the readout device.

4.3.6. The analyzer is calibrated by adding a known amount of oxygen to the oxygen already in the sample stream. The calibration procedure is as follows:

4.3.6.1. With the Output Selector or Range switch set to the appropriate range, adjust the analyzer flow rate to 150 cc/min, or to any desired flow rate compatible with Figure 1. Note the reading in ppm of oxygen.

4.3.6.2. Turn the Output Selector switch to the CAL position if the instrument is so equipped. Turn the Calibrator current switch ON and using Figure 1, adjust the Calibrator Current or Current Adj knob to a value that will produce a concentration of oxygen that is equip to at least 50% of the highest range. Current in milliamperes can be read directly from the readout device. Not the ppm oxygen determined from the nomograph.

4.3.6.3. Return the Output Selector or Range switch to the appropriate range, leaving the flowrate and calibrator as adjusted in steps 1 and 2. The reading should now be the sum of the oxygen values noted in steps 1 and 2. If not, wait 15 minutes, and then recheck the reading.

4.3.6.4. If the readout device does not indicate the proper oxygen content after approximately 15 minutes, adjust the Sensitivity Adjustor or Span knob to obtain the proper reading. Allow several minutes for the cell to come to equilibrium before taking a final reading.

4.3.6.5. When the readout device indicates the proper oxygen value, turn off the calibrator. The readout device will now go downscale and indicate the concentration of oxygen in the sample gas. If an adjustment was required with the Sensitivity Adjust or Span knob, this reading will be different from that obtained in step 1. If so, using this new oxygen value as a starting point, repeat the calibration procedure, making a second Span adjustment.

4.3.6.6. Alternately, the analyzer can be calibrated by connecting a primary standard reference gas of known oxygen content to the analyzer and determining the oxygen concentration on the readout device. If the oxygen reading in ppm is not the same as the value recorded on the body label of the cylinder containing the primary standard, adjust the Sensitivity Adjust or Span knob to obtain the correct value. Discontinue gas flow and repeat the above procedure to ensure that you have obtained the correct value.

4.3.6.7. The analyzer is calibrated once a month, after each startup, or following a change of electrolyte in the cell. The analyzer is calibrated using a primary standard reference gas.

4.3.6.8. As the electrolyte in the cell ages, Span adjustment will become insufficient for proper calibration. When this occurs, replace the elector lye with a freshly-prepared solution and recalibrate the analyzer.




GENERAL DESCRIPTION

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The Teledyne Trace Oxygen Analyzer is a panel-mounted, continuous use, electrochemical analyzer that measures trace quantities of oxygen by consuming oxygen from a gas stream and generating a proportional electric current. The current produced by the cell flows through a resistance and produces a voltage which can be monitored by a self-balancing potentiometer, indicating the amount of oxygen present.

THEORY The electrochemical cell consists of a cell block, a lead electrode (anode), and a silver screen assembly (cathode). The cell is filled with an electrolyte solution, consisting of potassium hydroxide (KOH), until the lower portion of the silver screens are covered. The cell of the analyzer is basically a fuel cell with the fuel being the lead electrode. The “combustion rate” of the lead is determined by the available oxygen. The silver screens serve the purpose of catalytically converting the oxygen to hydroxyl ions which are then used up on the “combustion” of the lead. The complete reaction is represented by the following equations: 1. O2 + 2 Ag = 2AgO 2. 2 AgO + 2 H2O + 4e → 2Ag + 4 (OH)- 3. 2 Pb + 4 (OH) - → 2PbO + 2 H2O + 4e

The last equation represents the “combustion” of lead to lead oxide with the resultant liberation of electrons needed to convert the oxygen to (OH)- This electron flow is read out by the instrument.

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 5.41 Beckman Moisture Analyzer

1. OBJECTIVE

This procedure establishes the Beckman Moisture Analyzer.



4. PROCEDURE 4.1. Preparation for Test

4.1.1. Install the analyzer in an area not subject to excessive vibration or extreme temperature variations.

4.1.2. Use only small diameter (1/8 inch) stainless steel capillary tubing for sample lines. 4.1.2.1. This reduces purge time and provides a fast, stable response.

4.1.3. Make sure all tubing and other components in contact with the sample are clean. 4.1.4. Always use a metal diaphragm regulator for pressure regulation.

4.1.4.1. Do not use a composition diaphragm regulator. 4.1.5. Warning: Pressure regulation and suitable pressure relief devices must be provided when high-

pressure cylinders are used. 4.1.6. Use packless valves whenever possible. 4.1.7. Use an all-stainless-steel sampling system. 4.1.8. Keep sampling lines as short as possible. Eliminate all unnecessary tubing bends, fittings, and

dead legs. 4.1.9. Dry down the sample lines and other parts of the sample system as follows:

4.1.9.1. Introduce a dry gas, e.g. house nitrogen, into the system. 4.1.9.2. Establish a considerable by-pass flow (approximately 940 cc/min). 4.1.9.3. Allow the dry gas to purge the system.

4.1.10. Continuously purge the sampling system and analyzer with dry gas when they are not in use, or cap the lines so as not to expose the system to atmospheric air.

4.1.11. NOTE: The Range Selector Switch should be left on STANDBY or a numbered position during periods of inactivity. In the standby mode, current flows continuously through the cell, keeping it dry and ready for use.

4.1.12. Keep electrical power on by leaving the Range Selector Switch on STANDBY or a numbered position whenever Sample Gas is flowing through the cell.

4.1.13. NOTE: The OFF position removes power from all circuits. It is normally used only during servicing.

4.1.14. Leak test the system using an approved solution. 4.1.15. Do not operate the analyzer at temperatures below 32oF. 4.1.16. Keep the cell sealed to minimize absorption or moisture; never leave it open to the air longer

than necessary. 4.1.17. Do not use the analyzer to test samples of ammonia, amines, alkenes higher than propylene,

alkynes, alkadienes, or hydrogen fluoride. These gases are not suitable for the analyzer. 4.2. Test Procedures:

4.2.1. There are two test procedures: the Single-Flow Test Method and the Delta-Flow Test Method. 4.2.2. Procedure for Packaged Gases: 4.2.3. Packaged gases personnel are to use the Delta-Flow Test Method when testing samples of the

following gases: 4.2.3.1. Air 4.2.3.2. Hydrogen 4.2.3.3. Oxygen

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4.2.4. Packaged gases personnel are to use the Single-Flow Test Method for all other samples. 4.2.4.1. Procedure for Bulk Gases 4.2.4.2. Bulk gases personnel are to use the Single-Flow Test Method when testing samples of

the following gases: 4.2.4.2.1. Argon 4.2.4.2.2. Nitrogen 4.2.4.2.3. Oxygen or Hydrogen – when testing the product to meet specifications and the

value obtained is less than the required specifications. 4.2.4.2.4. Note: The actual moisture value is less than the value determined by the Single-

Flow Method 4.2.5. Bulk Gases personnel are to use the Delta-Flow Method when moisture values in oxygen or

hydrogen do not meet specifications using the Single-flow Method or to obtain a more accurate moisture value when testing oxygen or hydrogen.

4.3. Single-Flow Test Method 4.3.1. Warning: Make sure that the proper pressure regulation and safety relief device are provided.

Do not operate the analyzer about 100 psig. 4.3.2. Connect the sample line to the sample inlet. 4.3.3. Close the Sample Flow Control Valve. 4.3.4. Set the Range Selector Switch to STANDBY. 4.3.5. Introduce the Sample Gas to the analyzer. 4.3.6. Adjust by-pass flow to indicate mid-scale (approximately 470 cc/min) on the By-pass Flowmeter. 4.3.7. Adjust the Sample Valve for proper flowrate using Table 1. 4.3.8. Select the proper Range Selector Switch position to bring the needle on-scale.

Gas Indicated Flowrate

100 cc/min Air Equivalent

Flowrate Delta-Flow Method A 50 cc/min

Air Equivalent

Flowrate Delta-Flow Method B 200 cc/min

Air Equivalent Air 100.0 50 200 Argon 127.0 -- -- Carbon Dioxide 86.0 -- -- Helium 103.0 -- -- Hydrogen 46.0 23 92 Nitrogen 97.0 -- -- Oxygen 115.0 57.5 230 Note: The values listed in Table 1 are approximate. They apply only to Brooks flowmeters installed in the analyzer by the manufacturer. The analyzer is calibrated for air at 14.7 psig and 70oF with a 100cc/min flowrate. For more accurate results:

1. Set the flowrate of the Sample Gas to 100 cc/min using a soap film flowmeter or an analog flow check.

2. Note the reading of the flowmeter on the analyzer. 3. Post this reading on the analyzer and use it in adjusting flowrate during subsequent tests.

Note: if the meter goes off-scale on the 1000 ppm range, the sample system is insufficiently purged. To avoid damaging the electrolytic cell, close the Sample flow Control Valve and continue purging the system. 4.3.9. When the needle has stabilized, read the meter. 4.3.10. Multiply the meter reading by the range multiplier to obtain ppm moisture by volume. 4.3.11. Close the Sample Flow Control Valve. 4.3.12. Place the Range Selector Switch on STANDBY. 4.3.13. Note: The analyzer is never turned off (Range Selector Switch on OFF) except for brief

periods of routine maintenance. 4.4. Delta-Flow Test Method A

4.4.1. Perform Steps 1 through 5 under the Single-Flow Test Method. 4.4.2. Perform Step 6 under the Single-Flow Test Method, using the 100 cc/min air equivalent flowrate

from Table 1. 4.4.3. Continue with Steps 7, 8, and 9 under the Single-Flow Test Method. 4.4.4. Write down the result of the calculation in Step 9 under the Single-Flow Test Method. 4.4.5. Perform Step 6 under the Single-Flow Test Method again, this time setting flowrate to the value

given for Delta-Flow Method A in Table 1. 4.4.6. Repeat Steps 7, 8, and 9 under the Single-Flow Test Method.

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4.4.7. Subtract the second result from the first. 4.4.8. Multiply the difference obtained in Step 7 by 2. The result is the true moisture content of the

sample. 4.4.9. End with steps 10 and 11 under the Single-Flow Test Method.

4.5. Delta-Flow Test Method B 4.5.1. Perform Steps 1 through 5 under the Single-flow Test Method. 4.5.2. Perform Step 6 under the Single-Flow Test Method, using the 100 cc/min air equivalent flowrate

from Table 1. 4.5.3. Continue with Steps 7, 8 and 9 under the Single-Flow Test Method. 4.5.4. Write down the result of the calculation in Step 9 under the Single-Flow Test Method. 4.5.5. Perform Step 6 under the Single-Flow Test Method again, this time setting flowrate to the value

given for Delta-Flow Method B in Table 1. 4.5.6. Repeat Steps 7, 8 and 9 under the Single-Flow Test Method. 4.5.7. Subtract the first result from the second. The result is the true moisture content of the sample. 4.5.8. End with steps 10 and 11 under the Single-Flow Test Method.

4.6. Monthly Cell Moisture Check 4.6.1. Electrolytic cells become desensitized with use. A desensitized cell with always give a false

(low) moisture content reading. 4.6.2. Perform the following Cell Moisture Check once a month to ensure that the cell has not become

desensitized: 4.6.3. Use a Moisture Check Gas of 10-30 ppm moisture gas. 4.6.4. Note: The Check Gas is NOT a calibration gas. It is simply a gas with 10-30 ppm moisture. 4.6.5. Following the appropriate steps under the heading “Test Procedures,” run a moisture test using

the 10-30 ppm moisture Check Gas as a sample source. 4.6.6. Check for a positive meter deflection. 4.6.7. If there is not positive meter deflection, the cell is bad and must be replaced. 4.6.8. Record the results on the Equipment Calibration Log (L 442-42). 4.6.9. Note: In Packaged Gas locations, a test cylinder that reads above 10 ppm moisture may be

used for the monthly cell check if the results are recorded on the Equipment Calibration Log. 5. REFERENCES General Description

The Beckman Model 340 Trace Moisture Analyzer is an automatic, continuous analyzer used to measure water vapor concentrations (up to 1000 ppm) in a gaseous sample stream. The analyzer operates on the principle of electrolytic hygrometry.

Theory: Trace moisture analysis is accomplished through the simultaneous absorption and electrolysis of water in an electrolytic cell. (Electrolysis is the splitting of water molecules into their component hydrogen and oxygen atoms.) Within the cell, which consists of a tube formed by two slightly separated rhodium wire helices, water vapor in the gas sample stream is absorbed by a thin film of phosphorous pentoxide (P2O5). The P2O5 film coats the inner surface of the rhodium wire electrodes. When the P2O5 film absorbs moisture, it becomes conductive, allowing a dc current to flow between the wire electrodes. It is this current that causes the electrolysis, generating hydrogen and oxygen gases and simultaneously drying the P2O5. because the current, following Faraday’s law, is directly proportional to the water vapor in the sample, the current provides a linear signal for meter indication. A steady stream of sample gas at a precisely regulated flowrate is necessary for accurate analysis. To speed results, the sampling line and instrument may be purged using a faster flowrate through the bypass system, while maintaining the prescribed sample flowrate. Samples of air, hydrogen, and oxygen may produce exaggerated readings on Beckman Moisture Analyzers. This occurs because the free oxygen or hydrogen atoms from the electrolysis of water (moisture) tend to recombine with gas in the sample stream. The re-formed water is electrolyzed again, producing a false higher reading of sample moisture content. • The effect is present with all hydrogen samples. • In air or oxygen samples, this effect is significant only when the true moisture content is 20 ppm

or less.

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For sample flow rates in the ranges we use, the re-formation of water is constant. This fact allows us to correct the exaggerated reading and obtain the true moisture content of the sample. The Delta-Flow Test Method consists of running the test procedure twice, changing the prescribed flow rate on the second run. Since the excess moisture from re-formation is constant on both test runs, it cancels out in the subtraction, giving a true moisture content reading.

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Quality Assurance Program Rev. 26 June 2008 Rev #: 2 Document Title: 5.42 Fuel Oxidizer System Self Assessment

1. OBJECTIVE

This procedure establishes the typical self assessment for making fuel oxidizer mixtures.


It is the responsibility of all laboratory personnel to ensure that this procedure is performed as described, that this procedure is reviewed and updated as necessary, and that proper support documentation is maintained. No fuel oxidizer mixtures may be filled unless approved by management.

4. PROCEDURE

Sat

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q q 1. Do we have a copy of the Bureau of Mines papers? Where are the documents? Yes q No q Location:

q q 2. What published documents are we using for the LEL and BTUs of fuels? Documents:

q q 3. Do we always segregate the fuel from the oxygen in the cylinder with an inert gas?

Yes q No q Remarks:

q q 4. Is the “Critical” component filled first? Yes q No q Remarks:

q q 5. Are our filling and supervisory personnel thoroughly qualified? Yes q No q Remarks:

q q 6. Is the training documented? Yes q No q Location:

q q 7. When was the last time each operator was observed filling a fuel/oxidizer mixture?

Operator/Date:

q q 8. When was the last time each operator was retrained? Operator/Date:

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q q 9. Do we require written authorization for each instance of a fuel/oxidizer to be filled?

Yes q No q Remarks:

q q 10. Do we use oxidizers other than Air or Oxygen? Yes q No q Remarks:

q q 11. Have we established a maximum percentage for the mixture LEL? Yes q No q Max % LEL:

q q 12. Does the maximum mixture LEL include multiple fuels in the same mixture? Yes q No q Remarks:

q q 13. Have we established a maximum BTU content for the mixture? Yes q No q Max BTUs:

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q q 14. Does the maximum mixture BTU content include multiple fuels in the same mixture?

Yes q No q Remarks:

q q 15. Have we established policies about whether fuel/oxidizer mixtures will be filled/sold in aluminum, low pressure or DOT 39 cylinders?

Yes q No q Remarks:

q q 16. Have we established procedures which define when dilution mixtures (base mixtures, premixtures, etc.) must be used?

Yes q No q Location of LWI:

q q 17. Have we defined the minimum grams of each gas which may be filled on each scale?

Yes q No q Min. grams:

q q 18. Have we defined when a micro cylinder and micro scale may/must be used… low gram & low vapor pressure components?

Yes q No q Location of LWI:

q q 19. Does our fill system contain any “dead legs”? Yes q No q Remarks:

q q 20. Do we blow down the empty fuel/oxidizers using a flammable, inert or oxidizing rack? Are the blowdown racks suitable for use with other mixtures after using for fuel/oxidizers?

Yes q No q Remarks:

q q 21. Do we put high pressure oxygen into manifolds previously containing a flammable gas?

Yes q No q Remarks:

q q 22. What is the specified and true accuracy of the fill scales (or gauges)? Accuracy:

q q 23. How often are the scale calibrations verified? Frequency: Location of LWI:

q q 24. How much error can be tolerated in the scale calibration verification?

Maximum permissible error:

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q q 25. How do we verify the scale precision? With a cylinder on the platform? With a pressurized pigtail?

Yes q No q Procedure:

q q 26. Are hoses used as pigtails for the cylinder on the scale? Yes q No q Remarks:

q q 27. Do we use automatic shut-off valves for filling fuel/oxidizer mixtures? Yes q No q Remarks:

q q 28. Do we permit fuel rich mixtures to be made? Yes q No q Remarks:

q q 29. Do the fillers/supervisors understand the chemical reactions when the calculations are performed?

Yes q No q Remarks:

q q 30. Do we permit acid and basic gases to be mixed? Yes q No q Remarks:

q q 31. Do we permit unsaturated hydrocarbons (Ethylene, Acetylene, etc.) and Hydrogen to be mixed? Limit the pressure?

Yes q No q Remarks:

5. REFERENCES

• CGA P-36 • CGA SA-15

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Quality Assurance Program Rev. 22 Oct 2010 Rev #: 4 Document Title: 5.43 Periodic Scale Verifications

1. OBJECTIVE

This procedure establishes the standard method of determining the uncertainty of the gravimetric scale used in preparing mixtures.



4. PROCEDURE 4.1. Daily Verification - Perform the following on a daily basis whenever the scale is used to make

gravimetric mixtures.

4.1.1. Using the 150 Kg scale, place a large cylinder on the scale platform

4.1.2. Select a certified 1 kg weight

4.1.3. Tare the scale

4.1.4. Place the 1 kg weight on the scale. Wait approximately three seconds. Record the indicated value on the scale display.

4.1.5. If the indicated value is within +/- 1 gram of the certified weight, the scale is acceptable for use. If the scale is outside +/- 1 gram of the certified weight, the scale needs attention. Contact your supervision.

4.2. Monthly Verification - Perform the following on a monthly basis.

4.2.1. Using the 150 Kg scale, place a large cylinder on the scale platform

4.2.2. Select a certified 1 kg weight

4.2.3. Tare the scale

4.2.4. Place the 1 kg weight on the scale. Wait approximately three seconds. Record the indicated value on the scale display.

4.2.5. Remove the weight. Do not rezero or retare the scale between each weighing.

4.2.6. Repeat the steps 4.2.4 and 4.2.5 above four more times.

4.2.7. Calculate the standard deviation for of the five replicate weight readings. Multiply the standard deviation by two. This result is assumed to be the uncertainty of the scale.

4.2.8. There may be additional scale errors: linearity, pigtail torque, loose flexures, purity of source gases, leaks, etc.

4.3. Fill Pigtail Uncertainty Error Calculation - Perform the following procedure when the fill system is installed and whenever the pigtail is replaced. This will calculate the torque/mass/volume in the pigtail and fill line

4.3.1. Place a cylinder on the scale and connect to the fill pigtail

4.3.2. Keep the cylinder valve closed

4.3.3. Evacuate to the cylinder valve

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4.3.4. Tare the scale to 0.0 grams

4.3.5. Pressurize the pigtail with Nitrogen to 2500 psi

4.3.6. Read and record the scale weight

4.3.7. Repeat the test four more times

4.3.8. Average the five torque readings and compare the repeatability

4.3.9. Acceptance Criteria: A ¼ inch SS pigtail should read ~4.0 grams. A 1/8 inch pigtail should read ~1.5 grams. This number should be very repeatable.

5. REFERENCES

• None

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Quality Assurance Program Rev. 16 Oct 2009 Rev #: 0 Document Title: 5.44 Certification Period (Shelf Life) For Calibration Gas Standards

1. OBJECTIVE

This procedure establishes guidelines for certifications periods for compressed gas calibration standards in aluminum cylinders that are properly prepared and stable


It is the responsibility of all laboratory personnel to be aware of these guidelines and apply them to the mixtures, as applicable.

4. PROCEDURE Following is the recommended certification periods for compressed gas calibration standards in

aluminum cylinders that are properly prepared and stable

Certified Components Balance Gas Applicable Certification Concentration Period (Months)

Ambient nonmethane Nitrogen > 5 ppb 24 organics

Ambient toxic organics Nitrogen > 5 ppb 24

Aromatic organic gases Nitrogen > 0.25 ppm 36

Carbon dioxide Nitrogen or air > 300 ppm 36

Carbon monoxide Nitrogen or air > 8 ppm 36

Hydrogen sulfide Nitrogen > 4 ppm 12

Methane Nitrogen or air > 1 ppm 36

Nitric oxide Oxygen-free N2 > 4 ppm 24

Nitrous oxide Air > 300 ppb 36

Oxides of nitrogen Air > 80 ppm 24 (i.e., sum of nitrogen dioxide and nitric acid)

Oxygen Nitrogen > 0.8% 36

Propane Nitrogen or air > 1 ppm 36

Sulfur dioxide Nitrogen or air 40 to 499 ppm 24

Sulfur dioxide Nitrogen or air > 500 ppm 36

Other non-reactive Non-reactive > 1% 60 mixtures not containing Oxygen When used as a balance gas, "air" is defined as a mixture of oxygen and nitrogen where the minimum concentration of oxygen is 10 percent and the concentration of nitrogen is greater than 60 percent. Oxygen-free nitrogen contains <0.5 ppm of oxygen.

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Quality Assurance Program Rev. 3 Feb 2010 Rev #: 0 Document Title: 5.45 Reporting Significant Digits In Analytical Results

1. OBJECTIVE

This procedure establishes guidelines for determining the number of digits to report on Certificates of Analysis (CoA).



4. PROCEDURE 4.1. Do not report more digits than your data support and your customer is expecting (certification

accuracy).

4.2. Multiply your actual analytical result by the desired certification accuracy.

4.3. Starting from the left, determine the location of the first non-zero digit. This location is the location of the last reportable digit.

4.4. Example 1 If you make a certified standard (2% accuracy) and the analysis is 5.1234%, you would report 5.1%. 0.02 x 5.1234 = 0.102468 - The first non-zero digit is the one (1) in the first decimal place. This is the last place you report on the CoA

4.5. Example 2 If you make a certified standard (2% accuracy) and the analysis is 4.87654%, you would report 4.88%. 0.02 x 4.87654 = 0.0975308 - The first non-zero digit is the nine (9) in the second decimal place. This is the last place you report on the CoA.

6. REFERENCES

• None

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Quality Assurance Program Rev. 11 March 2010 Rev #: 0 Document Title: 5.46 Moisture Dewpoint Conversion Chart

1. OBJECTIVE

This procedure establishes a moisture dewpoint conversion chart.



4. PROCEDURE Use the chart on the following page to convert moisture dewpoints between ppm, %, degree F and degree C.

5. REFERENCES

• See chart on the following page.

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Moisture Dewpoint Conversion Chart

Dew Point (oF)

Dew Point (oC)

PPM H2O

Percent H2O

Dew Point (oF)

Dew Point (oC)

PPM H2O

Percent H2O

Dew Point (oF)

Dew Point (oC)

PPM H2O

Percent H2O

83 28.3 38727 3.873 19 -7.2 3376 0.338 -45 -42.8 92.0 0.0092082 27.8 37432 3.743 18 -7.8 3197 0.320 -46 -43.3 87.0 0.0087081 27.2 36138 3.614 17 -8.3 3017 0.302 -47 -43.9 82.0 0.0082080 26.7 34844 3.484 16 -8.9 2897 0.290 -48 -44.4 76.0 0.0076079 26.1 33842 3.384 15 -9.4 2776 0.278 -49 -45.0 72.0 0.0072078 25.6 32840 3.284 14 -10.0 2656 0.266 -50 -45.6 67.0 0.0067077 25.0 31838 3.184 13 -10.6 2535 0.254 -51 -46.1 62.0 0.0062076 24.4 30836 3.084 12 -11.1 2415 0.242 -52 -46.7 59.0 0.0059075 23.9 29833 2.983 11 -11.7 2294 0.229 -53 -47.2 55.0 0.0055074 23.3 28831 2.883 10 -12.2 2174 0.217 -54 -47.8 51.0 0.0051073 22.8 27829 2.783 9 -12.8 2053 0.205 -55 -48.3 48.0 0.0048072 22.2 26827 2.683 8 -13.3 1933 0.193 -56 -48.9 44.6 0.0044671 21.7 25825 2.583 7 -13.9 1854 0.185 -57 -49.4 41.8 0.0041870 21.1 25057 2.506 6 -14.4 1775 0.178 -58 -50.0 39.0 0.0039069 20.6 24290 2.429 5 -15.0 1695 0.170 -59 -50.6 36.5 0.0036568 20.0 23522 2.352 4 -15.6 1616 0.162 -60 -51.1 34.0 0.0034067 19.4 22755 2.276 3 -16.1 1537 0.154 -61 -51.7 31.7 0.0031766 18.9 21987 2.199 2 -16.7 1458 0.146 -62 -52.2 29.4 0.0029465 18.3 21220 2.122 1 -17.2 1378 0.138 -63 -52.8 27.5 0.0027564 17.8 20452 2.045 0 -17.8 1299 0.130 -64 -53.3 25.6 0.0025663 17.2 19685 1.969 -1 -18.3 1220 0.122 -65 -53.9 23.6 0.0023662 16.7 18917 1.892 -2 -18.9 1153 0.115 -66 -54.4 22.1 0.0022161 16.1 18336 1.834 -3 -19.4 1087 0.109 -67 -55.0 20.6 0.0020660 15.6 17754 1.775 -4 -20.0 1020 0.102 -68 -55.6 19.2 0.0019259 15.0 17174 1.717 -5 -20.6 970 0.0970 -69 -56.1 17.9 0.0017958 14.4 16593 1.659 -6 -21.1 920 0.0920 -70 -56.7 16.6 0.0016657 13.9 16011 1.601 -7 -21.7 870 0.0870 -71 -57.2 15.4 0.0015456 13.3 15430 1.543 -8 -22.2 820 0.0820 -72 -57.8 14.3 0.0014355 12.8 14849 1.485 -9 -22.8 780 0.0780 -73 -58.3 13.3 0.0013354 12.2 14268 1.427 -10 -23.3 740 0.0740 -74 -58.9 12.3 0.0012353 11.7 13687 1.369 -11 -23.9 700 0.0700 -75 -59.4 11.4 0.0011452 11.1 13329 1.333 -12 -24.4 660 0.0660 -76 -60.0 10.5 0.0010551 10.6 12971 1.297 -13 -25.0 630 0.0630 -77 -60.6 9.80 0.00098050 10.0 12613 1.261 -14 -25.6 590 0.0590 -78 -61.1 9.10 0.00091049 9.4 12255 1.226 -15 -26.1 560 0.0560 -79 -61.7 8.40 0.00084048 8.9 11898 1.190 -16 -26.7 530 0.0530 -80 -62.2 7.80 0.00078047 8.3 11540 1.154 -17 -27.2 500 0.0500 -81 -62.8 7.20 0.00072046 7.8 11182 1.118 -18 -27.8 475 0.0475 -82 -63.3 6.60 0.00066045 7.2 10824 1.082 -19 -28.3 448 0.0448 -83 -63.9 6.20 0.00062044 6.7 10466 1.047 -20 -28.9 422 0.0422 -84 -64.4 5.70 0.00057043 6.1 10068 1.007 -21 -29.4 400 0.0400 -85 -65.0 5.30 0.00053042 5.6 9670 0.967 -22 -30.0 378 0.0378 -86 -65.6 4.78 0.00047841 5.0 9272 0.927 -23 -30.6 359 0.0359 -87 -66.1 4.50 0.00045040 4.4 8874 0.887 -24 -31.1 330 0.0330 -88 -66.7 4.15 0.00041539 3.9 8475 0.848 -25 -31.7 317 0.0317 -89 -67.2 3.84 0.00038438 3.3 8077 0.808 -26 -32.2 300 0.0300 -90 -67.8 3.53 0.00035337 2.8 7679 0.768 -27 -32.8 283 0.0283 -91 -68.3 3.28 0.00032836 2.2 7281 0.728 -28 -33.3 265 0.0265 -92 -68.9 3.00 0.00030035 1.7 6883 0.688 -29 -33.9 250 0.0250 -93 -69.4 2.76 0.00027634 1.1 6633 0.663 -30 -34.4 235 0.0235 -94 -70.0 2.54 0.00025433 0.6 6383 0.638 -31 -35.0 222 0.0222 -95 -70.6 2.35 0.00023532 0.0 6133 0.613 -32 -35.6 210 0.0210 -96 -71.1 2.15 0.00021531 -0.6 5883 0.588 -33 -36.1 196 0.0196 -97 -71.7 1.96 0.00019630 -1.1 5633 0.563 -34 -36.7 105 0.0105 -98 -72.2 1.81 0.00018129 -1.7 5383 0.538 -35 -37.2 174 0.0174 -99 -72.8 1.66 0.00016628 -2.2 5133 0.513 -36 -37.8 164 0.0164 -100 -73.3 1.53 0.00015327 -2.8 4883 0.488 -37 -38.3 153 0.0153 -101 -73.9 1.40 0.00014026 -3.3 4633 0.463 -38 -38.9 144 0.0144 -102 -74.4 1.29 0.00012925 -3.9 4453 0.445 -39 -39.4 136 0.0136 -103 -75.0 1.18 0.00011824 -4.4 4274 0.427 -40 -40.0 128 0.0128 -104 -75.6 1.08 0.00010823 -5.0 4094 0.409 -41 -40.6 119 0.0119 -105 -76.1 1.00 0.00010022 -5.6 3915 0.392 -42 -41.1 113 0.0113 -110 -78.9 0.63 0.000063021 -6.1 3735 0.374 -43 -41.7 105 0.0105 -120 -84.4 0.25 0.000025020 -6.7 3556 0.356 -44 -42.2 98.0 0.00980 -130 -90.0 0.10 0.0000100

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Quality Assurance Program Rev. 26 August 2010 Rev #: 0 Document Title: 5.47 Portable Calibration Gas Disposal Guidelines

1. OBJECTIVE

This procedure establishes a guideline for disposal of portable calibration gas cylinders.


It is the responsibility of all laboratory personnel to be aware of these guidelines and apply them, as applicable.

4. PROCEDURE If a customer asks the following question “How do I (we) dispose of an empty or expired calibration gas cylinder?” Use the following guidelines. Remember, that the hazards posed by Purity Plus disposable cylinders include: Residual pressure, toxic, flammable, corrosive or hazardous gas. Guidelines for Disposal: The IWDC and PurityPlus recommend the following guideline for disposing of non-refillable cylinders. 1. If authorized by your supplier, return non-refillable cylinders to your supplier for proper disposal. A

qualified disposal facility should have the equipment, procedures and qualified personnel to safely dispose of the hazardous contents in non-refillable cylinders. There will typically be a fee for disposal of non-refillable cylinders.

2. If you decide to dispose of the residual contents and non-refillable cylinder, be guided by the following: a. Thoroughly understand the hazards of the gas by consulting the Material Safety Data Sheet

for the product. b. Thoroughly understand the hazards of the high pressure cylinder and equipment. c. Thoroughly understand the environmental hazards and regulations for releasing the gas to

the atmosphere. Use appropriate hood/scrubbers/disposal technology as appropriate for the gas.

d. Have a written procedure approved by competent authority before proceeding. Include potential emergency actions as needed.

e. Assure all personnel use appropriate personal protective equipment. f. Using appropriate equipment, procedures and qualified personnel, vent the pressure from the

cylinder. Evacuate the cylinder and purge with inert gas. Re-evacuate and purge as necessary to assure a safe container.

g. Using appropriate equipment, procedures and qualified personnel, remove the cylinder valve. h. Dispose of the cylinder and valve according to local regulations.

5. REFERENCES

• None

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Quality Assurance Program Rev. 12 July 2012 Rev #: 1

Document Title: 5.48 Preparing NIST Traceable Gravimetric Mixtures

1. OBJECTIVE

This procedure establishes guidelines for preparing NIST traceable gravimetric mixtures. “NIST” in this case applies not only to the National Institute of Standards and Technology (USA), but also to other National Meteorological institutes (NMI).

2. SCOPE

This procedure applies to the specialty gases lab.

3. RESPONSIBILITIES


4. PROCEDURE

4.1. Qualification procedures

4.1.1. Assure that your gravimetric scales have been calibrated with weights traceable to NIST or your NMI through an unbroken chain of comparisons to stated references. Assure that the calibration interval has not been exceeded. The maximum permissible scale calibration interval is one year.

4.1.2. Assure that the sample cylinder analysis has been confirmed by an alternate technology (secondary analysis). This alternate technology (gas chromatograph, process analyzer, wet chemistry, etc.) is also calibrated with standards traceable to NIST or your NMI. Exceptions to the secondary analysis must be justified and documented.

4.1.3. Calculate the standard uncertainties (k=1) of the gravimetric analysis and of the secondary analysis. Use the “Summary Results” worksheet in the “Gravimetric Scale Uncertainty” workbook to calculate the Compatibility Criterion. The Compatibility Criterion must be TRUE in order to confirm the gravimetric analysis against the secondary analysis. If the Compatibility Criterion is FALSE, the sample mixture is placed in quarantine until the uncertainties can be resolved. See ISO 6142:2001, Section 6, and ISO 6143 for alternate strategies and instructions about confirming the mixture.

4.1.4. Report the results from the analytical method with the least uncertainty.

4.2. Calculate the uncertainty of the gravimetric analysis by following the “Gravimetric Scale Uncertainty Calculations” procedure, 5.49.

4.3. Assure the uncertainty of the analytical result is not more than the certification accuracy of the order.

4.4. NIST Traceability - In order to support a claim of NIST traceability, you must document the analysis or references used to establish the claim and provide a description of the chain of comparisons that were used to establish a connection to a particular stated reference. There are several common elements to all valid statements or claims of traceability:

4.4.1. A clearly defined particular quantity that has been measured

4.4.1.1. This can be described in specialty gas labs as the gas mixture, ppm, percent, etc. For scales, the defined quantity is “kilogram”, “pound”, etc.

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4.4.2. A complete description of the measurement system or working standard used to perform the measurement

4.4.2.1. This is typically the analytical instrument used to do the analysis.

4.4.3. A stated measurement result or value, with a documented uncertainty

4.4.3.1. This is typically the analytical result with it’s uncertainty.

4.4.4. A complete specification of the stated reference at the time the measurement system or working standard was compared to it

4.4.4.1. This is typically a complete description of the calibration gas: serial number, lot number, concentration, etc.

4.4.5. An internal measurement assurance program for establishing the status of the measurement system or working standard at all times pertinent to the claim of traceability

4.4.5.1. Your measurement assurance program would typically include verifying that the environment (temperature, etc.) is suitable and that the instrument is handled and shipped properly.

4.4.6. An internal measurement assurance program for establishing the status of the stated reference at the time that the measurement system or working standard was compared to it

4.4.6.1. Your measurement assurance program for the calibration gases/masses would typically include verifying that the environment (temperature, etc.) is suitable and that the standards are handled and shipped properly. Also be sure any gases with expiration dates are in date and that minimum cylinders are maintained, as needed.

4.5. An internal measurement assurance program may be quite simple or very complex, the level or rigor to be determined depending on the level of uncertainty at issue and what is needed to demonstrate its credibility. Users of a measurement result are responsible for determining what is adequate to meet their needs. ISO 17025 accredited certificates of analysis are accepted as being traceable to NIST.

4.6. See below for a sample of a NIST traceable certificate of analysis.

5. REFERENCES

• ISO 6142:2001

• Gravimetric Scale Uncertainty (23 August 2010) B.xls spreadsheet

• http://ts.nist.gov/Traceability/SupplMatls/suppl_matls_for_nist_policy_rev.cfm#FAQ_General5

• See the sample Certificate of Analysis below.

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Quality Assurance Program Rev. 23 August 2010 Rev #: 0

Document Title: 5.49 Gravimetric System Uncertainty Calculations

1. OBJECTIVE

This procedure establishes the standard method of determining the uncertainty of the gravimetric scale used in preparing mixtures. This procedure is in conformance with ISO 6142:2001/ Amd.1:2009(E)

2. SCOPE


3. RESPONSIBILITIES


4. PROCEDURE

4.4. Select either “pooled experimental standard deviation” or actual uncertainty calculations. The pooled experimental standard deviation simulates the preparation of the mixture and includes the aggregate uncertainty of scale resolution, drift, etc. The actual individual uncertainty calculations consider each of these potential uncertainties individually.

4.5. Pooled Experimental Standard Deviation (A.5.2.1)

4.5.1. Simulate the actual filling of the mixture without opening the cylinder valve. When your procedure calls for adding gases, simply add approximately the same mass through calibrated weights. Be sure to do the following actions exactly as if you were making the mixture:

4.5.1.1. Move the cylinder on and off the scale. If you typically fill the cylinder on an external manifold and move the cylinder to the scale, do the same in the simulation. This allows the uncertainty of the position of the cylinder on the scale platform to be estimated, if applicable.

4.5.1.2. Valve movement – simulate turning the cylinder valve by trying to close the valve even when you procedure asks for you to open the valve. This will allow the movement of the cylinder/scale to be included in the pooled estimate of uncertainty.

4.5.1.3. Pressurized pigtail – When the procedure calls for you to add gases, pressurize the pigtail to approximately the same pressure that you would use if you were actually making the mixture. This allows the torque/mass of the pigtail to be included in the pooled estimates.

4.5.1.4. Time – allow the scale to be loaded with the cylinder/simulated masses for approximately the same time that it takes to fill the actual mixture. This allows the resolution and scale drift to be included in the pooled estimate of uncertainty.

4.5.2. Simulate filling the mixture a total of three times. Take your final weighing at the same step where you consider the mixture to be finished, but be sure to leave the cylinder on the scale with the simulated masses still on the scale. If you typically take your final weighing with the cylinder connected to the pigtail and pressurized, take your simulated

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final weighing with the pigtail connected and pressurized. If you typically take your final weighing with the pigtail disconnected, take your final weighing in the same manner.

4.5.3. Document the final scale readings in the Pooled Uncertainty Calculations (Sheet: Pooled (A.5.2.1)) on the “Gravimetric Scale Uncertainty” spreadsheet.

4.6. Option – Actual Individual Uncertainty Calculations

4.6.1. This procedure is to be written as an option to the pooled uncertainty calculations and will included calculation of drift, resolution, etc.

4.7. Uncertainty of the Weights (A.5.2.2)

4.7.1. This is typically an insignificant uncertainty. However, it should be included in the mixture uncertainty calculations.

4.7.2. If a calibrated scale is used to directly determine the readings, follow the steps below:

4.7.2.1. Preload the scale with the same cylinder style as will be used in the mixture.

4.7.2.2. Place masses on the scale with approximately the weight as the gas in the final mixture.

4.7.2.3. Remove this weight, tare the scale and repeat for a total of five readings.

4.7.2.4. Record the scale reading in the Weight Uncertainty Calculations (Sheet: Weights (A.5.2.2)) on the “Gravimetric Scale Uncertainty” spreadsheet.

4.7.2.5. If more than one scale is used in the process, follow these steps with each scale.

4.7.3. If the mixture mass is to be compared against certified masses on a beam balance, follow the steps below.

4.7.3.1. Document the masses and standard uncertainty of each mass used in making the mixture.

4.7.3.2. If a mass is used more than one time, include the mass for as many times as it is used.

4.7.3.3. This feature is not presently included in the spreadsheet. If you begin making the mixture with a beam balance, calculate the uncertainty of the weights using ISO 6142:2001.

4.8. Buoyancy Effects (A.5.2.3)

4.8.1. There are two buoyancy effects to consider: the variability of the atmospheric conditions and the increase in the cylinder size/buoyancy as it is being filled.

4.8.2. Atmospheric Conditions –

4.8.2.1. If the mixture is made when the atmospheric conditions (temperature, barometric pressure, humidity) change, you must take into account the uncertainty based on the variable buoyancy of the cylinder. Use ISO 6142:2001 to calculate the uncertainty of the buoyancy. For typical high pressure mixture cylinders, this effect is insignificant.

4.8.2.2. Alternately, assure the temperature, barometric pressure and humidity do not measurably change over the time in which the cylinder is being prepared. If ambient conditions are stable, the variability of the buoyancy need not be considered.

4.8.3. Cylinder Size/Buoyancy

4.8.3.1. A good source of the information about cylinder expansion can be found by consulting the cylinder requalification data for typical cylinders of the same style.

4.8.3.2. Determine the likely expansion of the cylinder at the final fill pressure. This will be less than the requalification pressure and can be assumed to be linear for the purposes of this calculation.

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4.8.3.3. Document the cylinder expansion and air density in the Buoyancy Calculations (Sheet: Buoyancy (A.5.2.3)) on the “Gravimetric Scale Uncertainty” spreadsheet.

4.9. Residual Gas (A.5.2.4)

4.9.1. If you begin making the mixture with the balance gas purged in the cylinder, calculate the uncertainty of the residual gas using ISO 6142:2001.

4.9.2. If you evacuate the cylinder, document the residual gas effect using the Residual Gas Calculations on the “Gravimetric Scale Uncertainty” spreadsheet.

4.10. Uncertainty in the purity of the gases (A.5.3)

4.10.1. If you are making the mixture without adjusting the grams of the ingredients based on the purity of the gases, calculate the uncertainty of the purity of the gases using ISO 6142:2001.

4.10.2. A superior method is to adjust the recipe in the Specialty Gas Manager based on the actual purities of the ingredient gases. Preload the ingredients with their own recipes and use the ingredient recipes as source gases.

4.11. Uncertainty in the molar masses of the gases (A.5.4)

4.11.1. The molar mass of the components and the related uncertainties are calculated from the atomic weights given in the IUPAC publication on the Atomic Weights of the Elements. Another source for molar masses and uncertainties is: http://www.chem4free.info/calculators/molarmass.htm

4.11.2. As stated in ISO 6142:2001, the uncertainty of the molar masses for typical gases is insignificant and certainly less that 1/10 the total uncertainty of the mixture.

4.12. Other sources of errors (A.5.5)

4.12.1. Thermal effects – the buoyancy issues have been covered above

4.12.2. Adsorption/desorption phenomena – The cylinder must be passivated for reactive mixtures, particularly for low concentrations. Different ingredients have variable affinities for the materials in the cylinder, valve, lubricants, cleaning solutions, etc. In the case of potential reactions on the cylinder walls, use an appropriate protocol to demonstrate the stability of the mixture (e.g. EPA Protocol).

4.12.3. Air drafts – rather than quantify the uncertainty of air currents, we recommend the elimination of air currents to the extent that the scale reading is affected. The pooling uncertainty calculations would typically account for these effects.

4.13. Uncertainty Budget – The gravimetric mixture uncertainty budget is calculated and displayed on the “Uncertainty Budget” worksheet.

4.14. Results

4.14.1. 1% Accurate NIST Traceable Mixtures – The minimum grams necessary to achieve the 1% relative accuracy NIST traceable mixture is calculated and displayed on the “Summary Results” worksheet.

4.14.2. Other Mixtures – The minimum grams necessary to achieve the desired mixture accuracy is calculated and displayed on the “Summary Results” worksheet.

4.14.3. Cautions -

4.14.3.1. The calculated minimum grams to achieve the desired accuracies depend on no other significant uncertainties being manifest. You may want to apply an additional factor to allow for unknown uncertainties.

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4.14.3.2. The calculated results also do not take into account other factors which could render a mixture completely invalid. (e.g. contaminated cylinder walls, reactions inside the cylinder, operator error, intermittent scale failure, etc.) Any of these factors can happen during a mixture. Use great care during the mixture process and be alert to unusual events which could signal an unexpected result. See “Preparing NIST Traceable Gravimetric Mixtures” for instructions about confirming the analysis.

5. REFERENCES

• ISO 6142:2001/ Amd.1:2009(E)

• Gravimetric Scale Uncertainty (23 August 2010) B.xls spreadsheet

• Specialty Gas Manager, AsteRisk, LLC

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Quality Assurance Program Rev. 04 October 2011 Rev #: 0

Document Title: 5.50 Elements of Analytical Results

1. OBJECTIVE

This procedure establishes the standard elements of analytical results.

2. SCOPE


3. RESPONSIBILITIES


4. PROCEDURE

Declaring Analytical Results – Analytical results include the analyte, measureand, uncertainty, confidence interval, a description of the measuring system, a description of the reference material. Additional elements may also be included in the analytical results (requested concentration, etc.)

4.1. Measureand – The measureand is the instrument reading and includes the units being measured. The measureand is typically declared as a part of the analytical result. (e.g 1.80 ppm).

4.1.1. SI units are not completely implemented in many markets. If SI units are not used, assure the customer understands the units. For example, “ppm” is not a valid SI unit, but is well understood among specialty gas users. The SI equivalent would be µmol/mol or mol-6/mol, etc.

4.1.2. The measureand may be in volume units, mole units, weight units, LEL units, etc. Mole units are the default unless declared otherwise such that the customer understands the unit system.

4.1.3. There are occasions when the measureand is not explicitly declared on the certificate. For example, when we analyze non-volatile residue in a mil-spec gas analysis. We may read the milligrams of the residue and simply declare “Pass” or “Fail” for the certified analysis. In these cases, the customer must have access to the tolerance limits (e.g. have a copy of the mil-spec) and accept the abbreviated analytical result.

4.2. Uncertainty - All analytical measurements have some uncertainty around the reading. This principle is true for gas chromatographs, thermometers, gravimetric scales, trace moistures analyzers, etc. Uncertainty is usually expressed in relative terms (e.g. +/- 1 % relative). For example a meaureand with uncertainty might be declared: 1.80 µmol/mol +/- 5 % relative. “Rel.” may substiture for “Relative”.

4.2.1. If absolute uncertainty is to be used, assure the customer is aware of the uncertainty system. (E.g. 1.80 µmol/mol +/- 0.09 µmol/mol absolute.) “Abs.” may substitute for “absolute”.

4.3. Confidence Interval – when we declare the measured reading along with the measurement uncertainty, we must include a statement of the confidence we have that the true reading is within the stated uncertainty. This is typically done with a confidence interval statement. The following confidence interval statements are approximately equivalent: “95 % confidence

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interval”, “95 % CI” and k=2. All these statements indicate that the true reading will be within the stated uncertainty approximately 95 % of the time (two standard deviations).

4.3.1. For example, an analytical result might be expressed: 1.80 µmol/mol +/- 0.09 µmol/mol abs. (k=2)

4.4. Alternatives - Acceptable alternatives for declaring uncertainty and confidence intervals

4.4.1. The full result may be declared on the certificate of analysis or certificate of calibration.

4.4.2. The measureand may be declared in the certificate body and the uncertainty with confidence may be declared in the footer, notes, etc.

4.4.3. The measureand and uncertainty may be declared in the certificate body and the confidence may be declared in the footer, notes, etc.

4.4.4. The measureand may be declared in the body and the uncertainty with confidence can be declared in a customer specification, published specification, contract, etc. The customer must have access to the uncertainty and confidence information.

4.5. Description of the measuring system – The analytical results must include a description of the measurement system. This can be included in the report body near the measureand or it may be included elsewhere in the report. For example, the description of the measurement system might be included in the page footer.

4.5.1. A full description of the measurement system would include the analytical methodology, instrument description, instrument conditions and other parameters to document the analytical method at the time of execution.

4.5.2. An abbreviated description of the measurement system might be included on the certificate as long as an abbreviated description is permitted by government regulation, mil-spec, customer specification, standards specification, etc. The abbreviated description might be: “Electrochemical oxygen analyzer”, “Gas chromatograph with flame ionization detector”, etc. The abbreviation may be referenced by footnote to the footer of the report.

4.5.3. If an abbreviated description of the measurement system is used, the full description of the measurement system must be retrievable, if needed within the records retention period of the report.

4.6. Description of the reference material – The analytical results must include a description of the reference material. This can be included in the report body near the measureand or it may be included elsewhere in the report. For example, the description of the reference material might be included in the page footer.

4.6.1. A full description of the reference material would include the certificate number, lot number, serial number or other unique identifier for the reference material. In addition, include expiration date and environmental conditions, if applicable.

4.6.2. If permitted by mil-spec, customer acceptance, regulatory requirements, etc, the description of the reference material may be included on internal records and not described on the certificate.

5. REFERENCES

• ISO 6143:2001(E)

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Quality Assurance Program Rev. 04 October 2011 Rev #: 0

Document Title: 5.51 Considering Analytical Uncertainty Near Tolerance Limits

1. OBJECTIVE

This procedure establishes the standard method of considering the analytical uncertainty when the analysis results are near the tolerance limits.

2. SCOPE


3. RESPONSIBILITIES


4. PROCEDURE

4.1. Measureands - Most analytical measurements are well within the tolerance of the analyte. For example, when analyzing argon, UHP, we test for the oxygen concentration to assure that there is not more than 2 ppm oxygen in the argon. Usually, the oxygen concentration is well below 1 ppm.

4.2. Reliability - Occasionally an argon cylinder will have an oxygen reading near the tolerance limit of 2 ppm. When the reading is near the tolerance limit, we must consider the uncertainty and confidence interval of the analytical method and determine if the true oxygen concentration could actually be above the limit.

4.2.1. Example – Assume that the trace oxygen analyzer is a Delta F 510, 0 to 5 ppm range, with expanded uncertainty (k=2) of 0.063 ppm abs. at the 2 ppm level.

4.2.2. This means that if we analyze a true 2.000 ppm, we can be reasonable sure that 95% of the indicated readings will be between 1.937 and 2.063 (2.000 ppm +/-0.063 ppm, k=2).

4.2.3. Similarly, if we wanted to be confident that 95 % of instrument readings near the tolerance limit were actually within the tolerance limit, we would need to lower our Buffer Tolerance (Guard Band) limit by the expanded uncertainty (k=2) of the analytical method at that concentration.

4.2.3.1. Note: In reality, lowering the Buffer Tolerance by the expanded uncertainty (k=2) would yield a 97.5 % confidence interval since only one side of the normal distribution curve would extend over the tolerance limit.

4.3. Mixtures - Evaluation of the Buffer Tolerance should also be completed for mixtures when the analytical results are near the mixture blend tolerance (upper or lower range).

4.4. Determining the Buffer Tolerance –

4.4.1. The Buffer Tolerance is the value which will assure, to 95 % confidence interval, that the true value is below the full analytical tolerance.

4.4.1.1. In the example above, the Buffer Tolerance is 1.937 ppm and the full analytical tolerance is 2 ppm.

4.4.2. One method to determine the Buffer Tolerance is to reduce the tolerance range by the expanded uncertainty of the analytical method at the tolerance concentrations.

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4.4.2.1. For ISO 17025 accredited laboratories, the Buffer Tolerance can be quickly calculated be examining the Measurement Uncertainty Budget for the analytical method. Contact Tom Badstubner if you have any questions about establishing the Buffer Tolerance.

4.4.3. Similarly, the measurement uncertainty can be calculated using ISO 6143:2001(E) or equivalent procedures. Calculate the Buffer Tolerance by reducing the tolerance range by the expanded uncertainty of the analytical method at the tolerance concentrations.

4.4.4. Another resource for determining the Buffer Tolerance is to consult with the instrument manufacturer to assure 95 % confidence interval at the analytical tolerances required.

4.5. Action Needed – when an instrument indicates a value over the Buffer Tolerance, one of the following actions shall be taken:

4.5.1. Analyze the material three more times and average the four analytical results. This will cut the Buffer Tolerance in half (i.e. to one standard deviation, k=1) Because the uncertainty of the analysis is less, the analysis is more reliable..

4.5.2. Conduct a delta-flow leak check to evaluate if sample system contamination is contributing to the nearly out-of-specification reading.

4.5.3. Contact the Quality Manager and seek clarification about how to accept/reject this material.

4.5.4. Have customer service contact the customer to see if this material will meet their specifications.

4.5.5. Remake the mixture.

4.5.6. Reject the material being analyzed.

5. REFERENCES

• ISO 6143:2001(E)

• Sample Buffer Tolerance Record

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Quality Assurance Program Rev. 15 August 2012 Rev #: 0

Document Title: 5.52 Calibrating Electronic Scales By The Specialty Gas Lab

1. OBJECTIVE

This procedure establishes the standard method of calibrating the electronic scale by the specialty gas lab. This is intended to provide NIST traceability in cases where true NIST traceability is not practical from outside scale calibration services.

2. SCOPE

This procedure applies to the specialty gases lab. In this document, “Scale” and “Balance” are used interchangeably. This procedure is adapted from NIST Handbook 44. Adjustments to the generic principles in Handbook 44 have been made to recognize that specialty gas scales are always tared to eliminate the significant weight of the high pressure cylinder. After the large tare, small amounts of gas are added to the cylinder.

3. RESPONSIBILITIES


4. PROCEDURE

4.1. General Considerations

4.1.1. See “Calibration Standards” for specifications and calibration intervals for NIST traceable weights used in the calibration of the electronic scales. Be sure the uncertainty of each weight is documented on its calibration certificate.

4.1.2. Assure the scale, flexures and scale pit are clean and free of debris. Assure the scale is level and not touching any other objects (side of pits, cables, etc.). Use great care in handling scale components. Never open the sealed electronic sensing unit. If internal adjustments are needed, contact a qualified scale repair company.

4.1.3. Assure that air drafts are minimized during the calibration and normal operation of the scale. Likewise assure that no measurable scale influence is detected from electromagnetic fields, walkie-talkies, floor vibrations from forklifts/trucks/trains, unstable floor, magnetic effects, etc.

4.1.4. Scales should be calibrated regularly throughout their range. Where a scale is only used over a part of its capacity (as in specialty gas labs), calibration may be restricted to this range. In this case, a note on the calibration certificate stating the range that has been calibrated should be prominently displayed on the scale. Note that (although this will vary with the application and the scale) measurements made in the lowest 5% or 10% of a scale’s capacity may not be sufficiently accurate to use. In general, a different scale with a smaller capacity will make better measurements in that range.

4.1.5. Calibrations may be performed in-house in accordance with documented procedures that have been assessed as appropriate, using weights that have been traceably calibrated. Alternatively, a suitable accredited calibration laboratory, as evidenced by an appropriate calibration certificate, may undertake the calibration of scales. If a non-accredited external calibrator is used, it will be necessary to ensure that the requirement of ISO/IEC 17025 that the calibrating laboratory can demonstrate

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competence, measurement capability and traceability is met. The uncertainty of measurement should also be determined.

4.1.6. Weights used for the calibration of scales should be appropriate to the accuracy of the scale being calibrated. In any case, wherever possible they should have 95% confidence level uncertainty of calibration less than half the smallest digit size or recorded scale interval of the scale to be calibrated. If groups of weights are to be used together, then this criterion should be applied to the arithmetic sum of the uncertainties. This will ensure that the uncertainty of the weight(s) used will not give rise to an undetected error in the calibration of the scale.

4.1.7. The apparent mass of weights used will be affected by their buoyancy in the air in which they are used, and this will change with the air density. The calibration value of the weights will have been certified for air density 1.2 kg m-3. If the buoyancy effect caused by a different air density at the time of use leads to an error in the applied load that is greater than one half of the resolution of the scale being calibrated, a correction should be made.

4.1.8. Zero Tracking - Some electronic scales have a ‘zero-tracking’ facility. When a scale has been either ‘zeroed’ when unloaded, or tared to show zero when a load has been applied, zero-tracking will keep its indication locked to zero, provided that any incremental load change is not greater than a pre-set amount - often half a digit. This means that if a slow load change may occur at zero indication and would be significant to the measurement, it is important that the zero-tracking facility is disabled, either by changing the software setting or by adding a small weight that is present throughout the weighing.

4.1.9. EXERCISING - Scales of all types should be ‘exercised’ by loading to near maximum capacity or service load several times before being calibrated or used.

4.1.10. CALIBRATION AND CHECK INTERVALS

4.1.10.1. The frequency of calibration will depend on the type of scale and its use. The scale should be calibrated fully (see paragraph 4.3.3) at least once a year, unless sufficient evidence has been obtained to show that the scale has remained well within acceptance limits and that the interval can be extended.

4.1.10.2. Daily or before-use checks should be made on scales (see section 6) and the results recorded. This applies whether the scale has been calibrated in- house or by an external organization.

4.1.10.3. Other regular checks (intermediate checks) may be required between full calibrations, dependent upon use and intervals between full calibrations. In particular, regular eccentric-load indication tests can be helpful in the early detection of faults developing in the scale (see paragraph 5.3.2). Results of intermediate checks should be recorded.

4.1.10.4. Full calibrations should be performed after a significant change In the laboratory’s environmental conditions, a change in position of the scale, or following service or repairs carried out on the scale (whether carried out by the user or by a service agent). Intermediate checks, or full calibrations, should also be performed when there is any reason to believe that any other change has occurred which may affect the accuracy of the scale, or where servicing is planned that can be expected to adjust its characteristics.

4.1.10.5. If any intermediate check reveals a significant change in the accuracy of a scale a full calibration should be carried out. As a result, it may be necessary to review the validity of measurements made on the scale since the previous calibration. Consideration should also be given to repair and/or adjustment of the scale, and modification of any external factor that may have caused the change in accuracy. Where servicing work is carried out it should be followed by a further full calibration.

4.2. General Calibration Procedure

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4.2.1. Where the scale to be calibrated is electronic, and has an internal ‘calibration’ function that allows the output of the scale to be adjusted between zero and an internally or externally applied weight, it is advisable for this facility to be operated prior to the calibration, and also for it to be operated regularly before the scale is used.

4.2.2. The procedure should include tests for the following parameters, except where the construction or use of the scale renders a particular test inappropriate:

4.2.2.1. Repeatability (using a minimum of ten repeated measurements when calibrating a range up to 50 kg, and a minimum of five repeated measurements when calibrating a range exceeding 50 kg). This test should be done at or near the nominal maximum capacity of the scale or at the largest load generally weighed, returning to zero after each reading. For scales having more than one range, this test should be carried out for each range used. It is not necessary for the weight used for a repeatability test to be traceably calibrated.

4.2.2.2. Sensitivity, or the value of a scale division (should be omitted for scales with digital displays). The sensitivity of mechanical scales will generally change with load, and it is therefore necessary to measure the sensitivity at a load similar to that for which the scale is used. For a scale used across its range, it would be appropriate to measure the sensitivity with no load, loaded at half its capacity and loaded at or near its full capacity.

4.2.2.3. Departure of indication from nominal value, covering at least 10 points, evenly spread over the range; extra points may be required to make the even spread convenient, or to cover specific loadings used in the normal application. For scales that have internal weights (eg dial-up weights) each weight setting should be tested. For scales having more than one range, this test should be carried out for each range used.

4.2.2.4. Eccentric or off-center loading, using a load of between 1/4 and 1/3 of the maximum capacity, typically placed between 1/2 to 3/4 of the distance from the center of the load receptor to the edge, in a sequence of center, front, left, back, right, center, or equivalent. It is not necessary for the weight used for the eccentric-load indication test to be traceably calibrated.

4.2.2.5. Effect of tare and/or balancing mechanism (only for graduated balance/tare mechanisms).

4.2.3. The error allowed for a particular scale, for a particular test, should be set by the laboratory after considering the use to which the scale is put. Manufacturer’s specifications for scales will often be inappropriate for the application.

4.2.4. In order to comply with the requirements of ISO/IEC 17025, the laboratory needs to ensure that a suitable uncertainty of measurement is calculated for the scale calibration. A worked example that is consistent with the ISO Guide to the

4.3. USE OF CALIBRATION RESULTS

4.3.1. A typical set of certified calibration results will consist of a repeatability figure, a set of eccentric load measurement data, a set of indication error measurements across the range of interest, and a 95% confidence level uncertainty of measurement. This uncertainty figure applies only to the measured values obtained during the calibration, and should not be used as an estimate of the maximum indication error that the scale will give in use.

4.3.2. Repeatability is generally expressed as a standard deviation figure for each measuring range calibrated, based on a sample of 10 repeat readings up to and including 50 kg, and on a sample of 5 repeat readings above 50 kg. To estimate the range that will include 95% of all the indications that the scale might produce for a given load under the same conditions, multiply the repeatability standard deviation by the appropriate value for Student’s ‘t’ (see Table below). For scales up to 50 kg this is typically 2.325, and for scales with a capacity greater than 50 kg it is typically 2.87. The resulting figure is then plus or minus about a mean value. (This means that the total range of values in

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which 95% of the indicated values for a given load will fall is twice the certified standard deviation times Student’s ‘t’). Note that this figure will include the effects of normal eccentric loading in use, providing that users are trained to load reasonably precisely at the center of the platform.

Note: a coverage factor of k=2 actually relates to a level of confidence of 95.45% for a normal distribution. For convenience this is approximated to 95% which relates to a coverage factor of 1.96. However, the difference is not generally significant since, in practice, the level of confidence is based on conservative assumptions and approximations to the true probability distributions. The values given in Table 2 are for a level of confidence of 95.45%.

4.3.3. Although the ‘eccentricity’ test gives a numerical value of the indication error when the load is applied off-center, the result should not be taken as a limit on the range of eccentric load indication errors that the scale could produce. A particular load used in certain defined positions on the load receptor may not be typical of use, and will generally not be extreme. The eccentric load indication error is some function of the load applied, its distance from the center of the load receptor, and its angular position on the receptor. The calibration does not produce enough information to define this function, and so no predictions of the indication error in use can be derived. If the scale is used properly, with loads positioned near the center of the receptor, the indication errors in use are likely to be smaller than those found during the calibration. Conversely, a heavier load nearer the edge of the receptor could produce a larger indication error than that found by the calibration. Note: The main benefit of the eccentric loading test is to monitor the condition of the scale. Records should be maintained of the results, and each test carried out at the same loading and positions. It will then be possible to detect deterioration in the condition of the scale, and to monitor if it performs below acceptable limits. Repair of the scale can then be arranged before it leads to poor measurement results.

4.3.4. The measurements of indication error across the range of the scale can be used to either plot the error curve of the scale and hence make corrections for particular loadings, or to estimate the maximum indication error that is likely to affect the weighing result if no correction is made to a weighing result.

4.3.5. If no corrections are applied to indications on the scale in use, then an approximate uncertainty of the indications can be used. This is the arithmetic sum of the greatest measured indication error across the range and the certified uncertainty of measurement. Note that this is not rigorously true, being only at 95% confidence at the point of the greatest calibrated indication error and an over-estimate of uncertainty elsewhere in the range. Note also that it is only valid if the in-use weighings are made over a similar range of eccentricity to that during the repeatability calibration, and that no allowance is made for any change of behavior of the scale after the calibrations. With many electronic scales, the effects of changes in behavior can be minimized by using the ‘calibration’ function and built- in spanning weight, where is it available.

5. REFERENCES

• NIST, Handbook 44

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