ts tvs tfs protocols

Revision Date:Effective Date: 5/22/02Author: Mojisola AjayiSOP#: WCA005R0

SOP for Analyzing Total, Volatile and Fixed Solids

Laboratory Section of the Division of Water Quality, N.C. Department of Environment and Natural Resources of 16

D:\My Documents\SOPs\WCA005R0.doc

Total Solids Dried at 103-105oCTotal Volatile and Fixed Matter in Total Residue Ignited at 550oC

Reference: APHA, AWWA, WEF. 1992. Standard Methods for the Examination of Water and Wastewater, 18th

Edition, Method 2540B. American Public Health Association, American Water Works Association andWater Environment Federation, Washington D.C.

Reference: APHA, AWWA, WEF. 1975. Standard Methods for the Examination of Water and Wastewater, 14th

Edition, Method 208 E. American Public Health Association, American Water Works Association andWater Environment Federation, Washington D.C.

NC Division of Water Quality Laboratory Section4405 Reedy Creek Road1623 Mail Service CenterRaleigh, NC 27699-1623

(t)(919) 733-3908(f)(919) 733-6241

The mention of trade names or commercial products does not constitute endorsement or recommendation for use.

5/22/2002

Lead Chemist Approval Date

5/22/2002

Branch Head Approval Date

5/22/2002

QA/QC Officer Approval Date





Section Title Page1.0 Scope and Application 32.0 Summary of Method 33.0 Safety and Waste Handling 3-44.0 Definitions 45.0 Interferences 4-56.0 Apparatus and Equipment 5-67.0 Reagents and chemicals 68.0 Sample Collection, Preservation, Shipment and Storage 69.0 Calibration and Standardization 6-710.0 Sample preparation 711.0 Procedure 7-912.0 Calculations 9-1013.0 Quality Control 10-1114.0 Data validation procedures 11-1215.0 Preventative Maintenance 1216.0 Troubleshooting and Corrective Actions 1217.0 References 1318.0 Miscellaneous notes and precautions 1319.0 Personnel qualifications 1320.0 Attachments 1321.0 Revision History 13Attachment 1 Total, Volatile and Fixed Solids benchsheet 14Attachment 2 Sartorius Analytical Balance Calibration Log 15Attachment 3 Microbiology unit - Residue Oven Temperature log 16





1.0 Scope and Application

1.1 This method is used to determine total, volatile and fixed residue in potable, surface, ground andsaline water and domestic and industrial wastewater.

1.2 The applicable range of the determination is 1 mg/L to 200 mg/L (when a 1L sample is used).

2.0 Summary of Method

2.1 Method 2540 B-A well-mixed sample is evaporated in a pre-weighed dish and the residue is dried toa constant weight at 103°C to 105°C. The increase in weight of the dish represents the total solids.

2.2 Method 208 E- The residue from Method 2540 B is ignited to a constant weight at 550+ 50 oC. Theremaining solids represent the fixed solids while the weight loss on ignition represents the volatilesolids.

2.3 For current practical quantitation limits, see “DWQ: Laboratory Section-Practical QuantitationLimits (PQL)” posted quarterly on the Laboratory Section web site at:http://www.esb.enr.state.nc.us/lab/qa/pqlinorg.htm.

3.0 Safety and Waste Handling

3.1 Wear long-sleeve laboratory coat, gloves, and safety glasses to minimize contact with sample whenperforming analysis. Wear high temperature protective gloves (e.g., Zetex® wool-lined) whenhandling hot dishes or working with the drying oven or muffle furnace.

3.2 Retain unused sample in Microbiology cooler (G088) until the sample has been reviewed andreported.

3.3 After sample has been reviewed and reported, transfer sample to receiving room for disposal.

3.4 Refer to the Laboratory’s Chemical Hygiene Plan (CHP) for further information on safety within theunit and the laboratory.

3.5 Muffle furnace contains ceramic fibers that can result in the following:

3.5.1 May be irritating to skin, eyes, and respiratory tract.

3.5.2 May be harmful if inhaled.

3.5.3 May form cristobalite (crystalline silica) when used at high temperature (above 870ºC).

3.6 Follow these precautions when working with the muffle furnace to avoid exposure to ceramic fibers:

3.6.1 Use a good vacuum to clean equipment. Do not use compressed air.

3.6.2 Wear long sleeve laboratory coat, gloves, and eye protection to minimize skin and eyecontact. Contact lenses should not be worn.

3.6.3 Wash hands immediately following maintenance work on the furnace.





3.6.4 Place worn ceramic fiber in plastic bags and dispose of properly.

4.0 Definitions

4.1 Planchet- A steel tray designed to carry porcelain dishes to and from the oven and/or the mufflefurnace.

4.2 Total Solids (TS)-This is the term applied to the material residue left in the vessel after evaporationof a sample and its subsequent drying in an oven at 103-105o C. Total solids includes “totalsuspended solids,” the portion of total solids retained by a filter, and “total dissolved solids,” theportion that passes through the filter.

4.3 Fixed Solids (FS): This is the term applied to the residue of total solids retained after igniting at550°C + 50°C for approximately 15 to 20 minutes.

4.4 Volatile Solids (VS): This is the term applied to the weight loss of total solids upon ignition at 550°C+ 50°C.

4.5 LRB-This is the acronym for Laboratory Reagent Blank. An aliquot of reagent water is takenthrough the entire sample preparation and sample analysis including exposure to all glassware,equipment and reagents.

4.6 MDL-This is the acronym for Method Detection Limit. The constituent concentration that, whenprocessed through the complete method, produces a signal with a 99% probability that it is differentfrom the blank. For seven replicates of the sample, the mean must be 3.14s above the blank where sis the standard deviation of the seven replicates.

4.7 IDOC- This is the acronym for Initial Demonstration of Capability. An initial, one-time,demonstration of the ability to generate acceptable accuracy and precision with a specific method.Make a minimum of four replicate analyses of an independently prepared check sample having aconcentration between 5 and 50 times the method detection limit (MDL) for the analysis in thelaboratory.

4.8 PQL-This is the acronym for Practical Quantitation Limit. The PQL is about five times the MDLand represents a practical and routinely achievable detection limit with a relatively good certaintythat any reported value is reliable.

4.9 MSDS-This is the acronym for Material Safety Data Sheet- Written information provided by vendorsconcerning a chemical’s toxicity, health hazards, physical properties, fire and reactivity dataincluding storage, spill and handling precautions.

4.10 QCS-This is the acronym for Quality Control Sample. A solution of the method analyte of knownconcentration that is used to fortify an aliquot of LRB matrix. The QCS is obtained from a sourceexternal to the laboratory and is used to check laboratory performance.

4.11 DWQSTAR- Sample Tracking and Reporting system used by the Laboratory Section to track andreport samples.

5.0 Interferences

5.1 Large floating particles or submerged agglomerates of non-homogeneous material should beexcluded from the sample if it is determined that their inclusion is not desired in the final result.





Floating oil and grease; if present, should be included in the sample and dispersed by a blenderdevice before taking an aliquot for processing.

5.2 Excessive residue on the filter may form a water-entrapping crust. Limit sample size to that yieldingno more than 200 mg residue.

5.3 For samples high in dissolved solids, thoroughly wash the filter with deionized water to ensureremoval of dissolved material.

5.4 Prolonged filtration times resulting from filter clogging may produce high results owing to increasedcolloidal materials captured on the clogged filter. In this case, a smaller sample aliquot may bemeasured and the PQL adjusted accordingly.

5.5 Negative errors in the volatile solids may be produced by a loss of volatile matter during drying.Determination of low concentrations of volatile solids in the presence of high fixed solidsconcentration may be subject to considerable error. In such cases, measure for suspect volatilecomponents by another test.

6.0 Apparatus and Equipment

6.1 Planchet – stainless steel or aluminum, 65 mm diameter plates affixed to desiccant trays withindividually numbered filter compartments

6.2 Muffle Furnace for operation at 550 ± 50oC

6.3 Desiccator – stainless steel w/glass, Fisher Scientific

6.4 Drying Oven for operation at 103°C to 105°C

6.5 Sartorius Analytical Balance, 200 g capacity with desiccant can, capable of weighing to 0.1 mg S/N# 37100120.

6.6 Magnetic Stirrer with TFE stirring bar

6.7 Wide-bore pipettes

6.8 Evaporating dishes, porcelain, 90mm, 150ml capacity.

6.9 Graduated Cylinders, 25 ml and 100 ml

6.10 Forceps – blunt and smooth with inner non-corrugated tips

6.11 Zetex® wool – lined gloves

6.12 Beaker Tongs

6.13 4 L borosilicate bottles with tubes attached for dispensing deionized water.

6.14 Class S or equivalent weights, 0.5 g, 50.0 g, and 100 g

6.15 Dish tongs for transfer of dishes to/from oven.





6.16 Sponge for washing evaporating dishes.

7.0 Reagents and Chemicals

7.1 Deionized Water - obtained from the Laboratory's reverse-osmosis system. Use 200 ml for the LRBand treat same as samples.

7.2 QCS- Follow the manufacturer’s instructions for preparation and acceptance limits.

7.3 Desiccant- Drierite color indicating, Fisherbrand catalog #07-578-4A.

8.0 Sample Collection, Preservation, Shipment and Storage

8.1 For groundwater samples, see http://www.esb.enr.state.nc.us/lab/qa/collpresgw.htm for latestinformation on preservation and holding times.

8.2 For water quality samples, see http://www.esb.enr.state.nc.us/lab/qa/collpreswq.htm for latestinformation on preservation and holding times.

8.3 Samples should be collected in plastic or glass bottles. The volume collected should be sufficient toinsure a representative sample and allow for replicate analysis, if required.

8.4 Cool sample to 4°C upon collection in order to minimize microbiological decomposition of solids.

8.5 Analyze the sample as soon as possible. If storage is required, samples maintained at 4°C may beheld for seven days.

8.6 After analysis, samples are stored at 4°C in the Microbiology Unit cooler (G088) until all data hasbeen reviewed and reported in DWQSTAR.

8.7 Samples are then delivered to the Receiving Room (G098) for disposal.

9.0 Calibration and Standardization

9.1 Calibration of the Sartorius A1205 Analytical Balance

9.1.1 Level the analytical balance by centering the bubble inside the level indicator located on thebalance.

9.1.2 To perform an internal calibration on the Sartorius A1205 analytical balance: Press theON/OFF pad to turn the balance on; "0.0000g" will appear on the digital display.

9.1.3 Press the CAL pad to begin internal calibrations. “C” will appear. A few seconds later“CC” will appear and a deep sound will follow. "0.0000g" will appear once again,signaling the internal calibration is complete.

9.1.4 Check the balance with three different Class S or equivalent weights (100 g, 50 g, 0.5 g arecurrently used) and record each measurement in the Balance Calibration Verificationlogbook. The measured values should adhere to ASTM tolerances or corrective action mustbe taken. If the calibration verification attempt does not seem to function properly, inform





the Lead Chemist immediately. Do not use this balance until the calibration problem hasbeen corrected.

10.0 Sample preparation

10.1 Bring samples and QCS to room temperature before beginning analysis.

11.0 Procedure

NOTE: If volatile residue is to be measured, turn muffle furnace on and allow temperature to reach 550oC.Prepare evaporating dishes early in the work-day at least one day before analysis using the followingprocedure:

11.1 Preparation of evaporating dishes

11.1.1 Total Solids evaporating dish preparation

11.1.1.1 Wash dishes in tap water with Alconox® detergent using a sponge.

11.1.1.2 Rinse thoroughly with deionized water.

11.1.1.3 Towel or air-dry dishes on a surface cleaned with 70% isopropyl alcohol.

11.1.1.4 Place evaporating dishes in a 103 to 105 oC oven for at least one hour.

11.1.1.5 Cool and store evaporating dishes in a desiccator until needed.

11.1.1.6 Weigh evaporating dishes immediately before use.

11.1.2 Total Volatile/Fixed Solids evaporating dish preparation:

11.1.2.1 If volatile solids are to be measured, place dishes on planchets and place theplanchets into a preheated muffle furnace set at 550oC + 50o C.

11.1.2.2 Stack planchets no more than 4 high and place no more than 24 total dishes in thefurnace at one time.

11.1.2.3 Allow dishes to remain in furnace for 90 minutes.

11.1.2.4 Wearing Zetex® wool-lined gloves, remove planchets with dishes from furnaceand place them in the 103-105ºC drying oven (this step allows the porcelain to coolslowly without breaking). (CAUTION: PLANCHETS AND DISHES WILL BEEXTREMELY HOT. HANDLE WITH CARE).

11.1.2.5 At the end of the work day, remove planchets from the 103°C drying oven usingthe Zetex® wool-lined gloves and put them into desiccators (keep desiccantrefreshed, desiccant should be blue in color). Secure desiccator tops and/or doorsand check seals to ensure there are no air leaks.

11.1.2.6 Store dried evaporating dishes in desiccator until needed for analysis. (NOTE: Ifneeded immediately, dishes must be allowed to cool completely before analysis.)





11.1.2.7 Weigh immediately before use.

11.2 Total Solids Procedure

11.2.1 Preheat drying oven to approximately 2oC below boiling.

11.2.2 Remove dishes from the desiccator one dish at a time using the beaker tongs (moisture andoil from the hands will affect the weight of the dishes) and weigh on the analytical balance.

11.2.3 Keep a desiccant can in the analytical balance to help maintain a constant weight whenweighing.

11.2.4 Record dish identification number and weight on the Total, Volatile and Fixed Solidsbenchsheet.

11.2.5 Tighten the cap of the sample container, shake sample a minimum of 25 times.

11.2.6 Pour 100 ml of sample into a graduated cylinder. (NOTE: Sample volume analyzed mustyield 10-200 mg of residue. Adjust volume analyzed accordingly).

11.2.7 Record volume used on Total, Volatile and Fixed Solids benchsheet.

11.2.8 Pour the sample from the graduated cylinder into an evaporating dish.

11.2.9 Place evaporating dishes in the pre-heated drying oven.

11.2.10 Load filled dishes from the top to bottom rack in the oven.

11.2.11 Evaporate sample at 2oC below boiling to prevent splattering.

11.2.12 Dry at 103-105oC for a minimum of one hour.

11.2.13 Remove dried dishes from the oven using dish tongs

11.2.14 Place evaporating dishes in the desiccator (DO NOT STACK DISHES INSIDE EACHOTHER).

11.2.15 Allow dishes to cool in the desiccator to balance temperature.

11.2.16 Check the calibration of the balance using three Class S or equivalent weights and documentthe process in the Balance Calibration Verification logbook.

11.2.17 Weigh evaporating dishes to the nearest 0.1 mg and record weight found on Total, Volatileand Fixed Solids benchsheet.

11.2.18 Repeat the cycle of drying, cooling, desiccating and weighing until the weight change is lessthan 4% of the previous weight or 0.5 mg, whichever is less.

11.2.19 Use the final weight determination for calculating results.





11.3 Fixed and Volatile Solids Procedure

NOTE: If total fixed and total volatile solids are to be determined, ignite the weighed dishes fromthe completed total solids procedure.

11.3.1 Preheat muffle furnace to 550ºC ± 50ºC. Furnace should be up to temperature beforeinserting samples.

11.3.2 Place dishes onto a planchet using dish tongs.

11.3.3 Using Zetex® wool-lined gloves and beaker tongs, place planchets into a preheated mufflefurnace at 550ºC ± 50ºC.

11.3.4 Record the furnace temperature on the Microbiology unit - Residue Oven Temperature log.

11.3.5 Allow residue to ignite for 90 minutes.

11.3.6 Carefully remove planchets with dishes from muffle furnace sing Zetex® wool-lined glovesand beaker tongs and place planchets with dishes into 103ºC to 105ºC oven. (Thisintermediate cooling step prevents too-rapid cooling and possible cracking of the ceramicdishes).

11.3.7 Leave dishes in oven for approximately 2 hours.

11.3.8 Wearing Zetex® wool-lined gloves, remove dishes from oven using beaker tongs and placethem in desiccators. DO NOT STACK DISHES.

11.3.9 Allow the dishes to cool completely.

11.3.10 Check the calibration of the balance using certified weights and document in the BalanceCalibration Verification logbook.

11.3.11 Weigh evaporating dishes to the nearest 0.1 mg as soon as they are completely cool.

11.3.12 Repeat the cycle of drying, cooling, desiccating and weighing until the weight change is lessthan 4% of the previous weight or 0.5 mg, whichever is less.

11.3.13 Use the final weight determination for calculating results.

12.0 Calculations

12.1 Total Solids calculation

Where:mg TS/L = (A-B) x 1000 A= weight of dried residue + dish, mg and

sample volume, ml B=weight of dish, mg





12.2 Volatile Solids and Fixed Solids calculations:

Where: mg VS /L =(A-B) x 1000

sample volume, ml A = weight of residue + dish before ignition, mg. B = weight of residue + dish after ignition, mg and

mg FS/L =(B-C) x 1000 C = weight of dish, mgsample volume, ml

12.3 Relative Percent Difference (RPD) formula:

RPD = 2[A-B] x100 A= concentration value of first sample A+B B = concentration of duplicate sample

[A-B] = absolute difference betweendeterminations

12.4 For samples containing <100 mg/L TS, VS, FS, report results to 2 significant figures.

12.5 For samples containing >100 mg/L TS, VS, FS, report results to 3 significant figures.

13.0 Quality Control

13.1 Prior to analyzing samples by this method, the following determinations and analyses must besucessfully completed and documented.

13.1.1 Desiccant must be blue in color, replace or recharge exhausted desiccant that turns pink byheating in an oven at 218°C for 1 hour.

13.1.2 The thermometers used to check the temperature of the oven and furnace must be checkedagainst an NIST traceable thermometer annually. Any correction factor obtained must berecorded on the thermometer and considered when reading oven and/or furnacetemperatures.

13.1.3 IDOC - Each analyst must have prepared an acceptable IDOC (Initial Demonstration ofCapability) study before analyzing samples. Analyze 4 mid-range standards and submit tothe unit lead chemist for calculation.

13.2 Daily laboratory performance must be monitored by analyzing the following:

13.2.1 Check the analytical balance with at least three Class S or equivalent weights each dayanalysis is performed. The measured values must adhere to ASTM tolererances orcorrective action must be taken.

13.2.2 Analyze a blank dish by rinsing the membrane funnel with deionized water for each set up.Must be < ½ currently published PQL or corrective action must be taken.

13.2.3 Analyze a LRB daily. Must be < ½ currently published PQL or corrective action must betaken. Refer to Section 16.0.





13.2.4 Analyze a QCS sample with each analytical batch. The QCS must meet manufacturer'spublished limits or corrective action must occur. Refer to section 16.0.

13.2.5 Duplicate the first sample of an analytical batch and every 10th sample, giving priority asduplicates to Chain of Custody, split samples, and emergency samples. Record the relativepercent difference (RPD) of duplicate sample results on the laboratory benchsheet. Forsamples containing > 50 mg TS/L, the relative percent difference of duplicate samplesshould be no greater than 20%. If RPD > 20%, corrective action must occur. Samplesbelow 50 mg TS/L may not duplicate well. For samples with < 50 mg TS/L, the absolutedifference between duplicate results must be less than the PQL. Duplicate determinationsshould agree within 5% of their average. If duplicates results do not meet this requirement,corrective action must be taken. Refer to section 16.0.

13.2.6 Sample volume analyzed must yield 10.0 mg – 200 mg of residue

13.2.6.1 If < 10 mg residue remains in dish, increase sample volume (up to 1 liter) andreanalyze.

13.2.6.2 If > 200 mg residue remains in dish, dilute sample and reanalyze.

13.2.7 Record the temperatures of the drying oven and muffle furnace on the Microbiology unitResidue Oven Temperature log and Total, Volatile and Fixed Solids benchsheet.

13.2.8 The oven temperature must be monitored to ensure that it is operating within the limits of103-105°C.

13.2.8.1 If the temperature drifts < 103 °C, then re-dry filters.

13.2.8.2 If the temperature drifts > 103 °C, then the samples must be reanalyzed due to thepossible loss of volatile solids.

13.2.9 The muffle furnace must be monitored to ensure that it is within the limits of 550±50°C. Ifthe temperature drifts excessively during an analysis, the samples must be re-dried or re-ignited when the oven or furnace is brought back into control. Begin timing the drying cyclewhen the temperature equilibrates.

13.2.10 Record quality control data in the Total Solids logbook.

13.2.11 Enter standard preparation information in the Microbiology Standards logbook.

14.0 Data validation procedures

14.1 Peer review-Completed data should be submitted for peer review within 2 days of analysis. Verifythat all standards, reagents and quality control analyses have been entered into appropriate logs.Verify that all information has been transferred correctly to the benchsheet. Verify that all QCSsamples meet acceptable limits that accompany each standard. Verify that duplicate samples are <20 % RPD. Verify that results have been entered into the Excel solids spreadsheet correctly. Allstandard information should be documented on the Total, Volatile and Fixed Solids benchsheet. Ifany errors are found, return data to the analytical chemist for correction. Ensure initials and dates areon benchsheet.





14.2 Lead Chemist Review-Peer reviewed data should be submitted to the lead chemist within 4 days ofanalysis. Verify that all information has been transferred correctly to benchsheet. Verify that allQCS samples meet acceptable limits. Verify that duplicate samples are < 20 % RPD. Verify thatresults have been entered into the appropriate spreadsheet correctly. All standard information shouldbe documented on benchsheet. If any errors are found, return data to the analytical chemist forcorrection. Ensure initials and dates are on the benchsheets. After reviewing data, submit to dataentry personnel for reporting.

15.0 Preventative Maintenance

15.1 The analytical balance is serviced by a certified vendor on an annual basis.

15.2 The absorption capacity of the desiccant must be monitored closely. Once the desiccant has turnedfrom blue to pink (indicating water absorption), heat desiccant in a 218°C oven for one hour. Cooland it is ready to be reused. Desiccant may be reused up to 3 times. After 3 times, discard the olddesiccant and replace with new.

16.0 Troubleshooting and Corrective Actions

16.1 Samples are not analyzed within holding time.

16.1.1 The affected data must be qualified with “Q” (Holding time exceeded.).

16.2 LRB is greater than 1/2 the concentration of the PQL.

16.2.1 Reanalyze samples if within holding time.

16.2.2 If holding time has expired, the data must be qualified with "V".

16.3 QCS is not within manufacturer’s published acceptance range.

16.3.1 Reanalyze samples if within holding time.

16.3.2 If holding time has expired, qualify data with "J2".

16.4 RPD for duplicates is >20% (for total solid concentrations > 50 mg/L) or absolute difference exceedsPQL (for total solid concentrations <50 mg/L).

16.4.1 If the samples are within holding time, all samples following the last successful qualitycontrol sample must be reanalyzed.

16.4.2 If the problem remains unsolved or if the samples are not within holding time qualify thedata with "J2" (the reported value failed to meet the established QC criteria for eitherprecision or accuracy).

16.5 Document any errors that may occur during the analysis and corrective actions taken on the “SampleAnomaly Report” (SAR) form.





17.0 References

17.1 APHA, AWWA, WEF. 1992. Standard Methods for the Examination of Water and Wastewater, 18th

Edition, Method 2540B Control, Published by American Public Health Association, American WaterWorks Association and Water Environment Federation, Washington D.C.


Edition, Method 208E, Published by American Public Health Association, American Water WorksAssociation and Water Environment Federation, Washington D.C.

17.3 U.S. Environmental Protection Agency, 1978. Methods for Chemical Analysis of Water and Wastes,EPA-600/4-79-020, Method 160.4 Residue, Volatile (Gravimetric, Ignition at 550oC), USEPA Officeof Research and Development, Cincinnati, OH.

17.4 United States Code of Federal Regulations. Title 40 chapter I. Subchapter D. Part 136 et seq.Guidelines Establishing Test Procedures for the Analysis of Pollutants. U.S. Government PrintingOffice, Washington, D.C.

17.5 North Carolina Administrative Code Title 15, Department of Environment, Health and NaturalResources Chapter 2, Water Quality Division, Subchapter 2H, Procedures for Permits, Approvals,Section .0800 Laboratory Certification.


Edition, Section 1020 Quality Control, Published by American Public Health Association, AmericanWater Works Association and Water Environment Federation, Washington D.C.

18.0 Miscellaneous notes and precautions

N/A

19.0 Personnel qualifications

19.1 Each employee must review and sign "Employee Training and Information" for safety as required byCFR OSHA 1910.1450(f).

19.2 An acceptable IDOC study should be performed before any analysis of samples is performed.

19.3 Chemist should be familiar with Microsoft Office® Excel to ensure data is entered into computercorrectly.

20.0 Attachments

20.1 Attachment 1: Total, Volatile and Fixed Solids benchsheet

20.2 Attachment 2: Sartorius Analytical Balance Calibration Log

20.3 Attachment 3: Microbiology unit- Residue Oven Temperature Log

21.0 Revision History

Revision number Date Revised Revision Summary0 5/22/02 New SOP





Attachment 1: Benchsheet for Total, Volatile and Fixed Solids

Lab # toPage of Micro ID Sartorius Analytical Balance

Set up Read back TRUE VALUE mg/L S/N: 37100120Date FOUND mg/LAnalyst RANGE mg/LChecked by:

NOTE: Use A2 for calculation if within 4% or 0.5 mg of A1 Sample: Sample: Sample: mg total susp.solids/L = (A-B) x1000 where: Duplicate: Duplicate: Duplicate: Sample volume, ml A= weight of dried %RPD %RPD %RPDmg volatile solids/L = (A-C) x1000 residue + dish, mg Sample volume, ml B=weight of dish, mg.mg fixed solids/L =(C-B) x1000 C= weight of residue + Oven Temperature

oC Oven Temperature

oC

Sample volume, ml dish after ignit., mg Time in Time InTime out Time out

Dish Dish [A1-A2],Dish Residue Residue (g) Ignited Total Total Total Total Total Total

Dish Sample Weight (mg) Weight (mg) Weight (mg) (< 0.5 mg Weight (mg) Residue Volatile Fixed Residue Volatile fixedLab # # Vol (ml) (B) (A1) (A2) or 4 %) (C) (mg) (mg) (mg) (mg/L) (mg/L) (mg/L)

Blank dishQCS

*=Chain of Custody +=Salt deposit T=Total Residue C=Total Volatile/Total Fixed A=Averaged Value

Lab Notes:

Duplicate Information

Drying time information

Reported Values

Calculations

1st drying time 2nd drying time

Balance InformationQCS

Total, Volatile and Fixed SolidsStandard Methods 18th ed 2540 B and Standard Methods 14th ed 208 E





Attachment 2: Sartorius Analytical Balance Calibration log

Sartorius Analytical BalanceS/N: 37100120

Date Chemist 100 g 50 g 0.5 g

Balance Information

Balance Calibration

Sartorius Analytical Balance Calibration Log





Attachment 3: Microbiology unit - Residue Oven Temperature Log

D a t e C h e m i s t 1 0 3 oC - 1 0 5

oC 5 5 0

oC + 5 0

oC D a t e C h e m i s t 1 0 3

oC - 1 0 5

oC 5 5 0

oC + 5 0

oC

M i c r o b i o l o g i c a l U n i t - R e s i d u e O v e n T e m p e r a t u r e s