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7090 Series Nitrogen / Sulfur GC Detectors Installation/Operation/Service Manual Rev E P/N MAN 7090 8824 Fallbrook Dr. • HOUSTON, TEXAS 77064 USA TELEPHONE: 800-444-TEST or 281-580-0339 • FAX: 281-580-0719 [email protected] • www.paclp.com

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Page 1: 7090 Operation/Service Manualpaclp.tech/lab_instruments/7090 detector with gc/7090... · 2017-06-17 · PAC 7090 Series IOS Manual Rev E MAN 7090 Page iii In This Manual The 7090

7090 Series Nitrogen / Sulfur

GC Detectors

Installation/Operation/Service Manual

Rev E

P/N MAN 7090

8824 Fallbrook Dr. • HOUSTON, TEXAS 77064 USA

TELEPHONE: 800-444-TEST or 281-580-0339 • FAX: 281-580-0719

[email protected] • www.paclp.com

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PAC 7090 Series IOS Manual

Rev E MAN 7090 Page i

Copyright © 2015 by Petroleum Analyzer Company, L.P.

All text, graphics, design, and other works contained herein are the copyrighted works of

Petroleum Analyzer Company, L.P (PAC).

All rights reserved. Any redistribution or reproduction of any materials contained

herein is strictly prohibited without the express written permission of the copyright

holder.

The PAC trademark, the PAC service mark, PAC’s logo trademark, the Antek trademark,

and Petroleum Analyzer Company, L.P.’s distinctive color trademark as used on its

instruments and in these materials, are trademarks, service marks, registered trademarks,

and/or registered service marks of Petroleum Analyzer Company, L.P. in the U.S. and

other countries and are its sole and exclusive property.

Microsoft® Windows®, Microsoft Windows XP®, and Windows Professional operating

systems are registered trademarks of Microsoft Corporation. Windows is a registered

trademark of Microsoft Corporation in the United States and other countries.

Other trademarks contained within these materials are the property of their respective

owners.

INFORMATION

The information contained within these materials is subject to change without notice.

PAC makes no warranties or guarantees, either expressed or implied in these materials,

including the warranty of merchantability or fitness for a particular purpose. At any time,

PAC may modify these materials, its instruments or its programs without notice and

subsequent versions of these materials may contain different information. These

materials could contain technical inaccuracies and/or typographical errors.

PAC does not assume responsibility for the accuracy of any translation of these materials.

About PAC

PAC is an international manufacturing and service organization with a portfolio that

spans petroleum, petrochemical, biofuels, environmental, food and beverage,

pharmaceutical and industrial analysis solutions. PAC provides advanced testing

equipment for laboratory, process on-line and field use for entities ranging from the

smallest to the largest enterprise businesses. PAC offers analytical solutions for a wide

variety of applications, including chromatographic systems and detectors, elemental,

laboratory, and on-line process analyzers, software applications, and spectroscopy.

More information about PAC is available at http://www.paclp.com.

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PAC 7090 Series IOS Manual

Page ii MAN 7090 Rev E

Revision History

Revision Description Date

A First Edition Release October, 2002

B Update Chapter 7 October, 2002

C Update October, 2012

D Ozone updates, 9.3.1 and 9.3.2, new drawing January 2014

E Added MSDS’s and Sulfur or Nitrogen/Sulfur Simultaneous Setup, removed DWG

June 2015

THIS MANUAL CONTAINS CONFIDENTIAL AND PROPRIETARY INFORMATION…

…which is the property of PAC, L.P. The information contained in this document is subject to

change without notice.

This document is for information only. The manufacturer accepts no liability for errors contained

herein or for incidental or consequential damages arising from the furnishing, performance, or use

of this material.

Unless otherwise specified, each reference to names or individual trademarks and service marks

has the sole purpose of illustrating the product described here. Contents of this publication may

not be reproduced in any form or by any means (including electronic storage and retrieval or

translation into a foreign language) without prior agreement and written consent from the

copyright owner.

All rights reserved.

Copyright ©2015, by PAC, LP Houston, Texas.

Printed in the United States of America All rights reserved.

Contents of this publication may not be reproduced in any form without permission of the copyright owner.

01.18.2015

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PAC 7090 Series IOS Manual

Rev E MAN 7090 Page iii

In This Manual

The 7090 SERIES Operation Manual contains the following sections:

Chapter 1 – General Information: Warranty and compliance information

concerning the 7090 Series detector.

Chapter 2 – Safety Notices and cautions specifically for the 7090 Series.

Chapter 3 – Introduction A general introduction to the 7090 Series detailing

the basic theory of operation.

Chapter 4 – Installation Steps to unpack, inspect and prepare the

7090 Series for use. This Chapter details the

optional equipment available.

Chapter 5 – System Overview An overview of the controls, connections and

general layout of the 7090 Series detector.

Chapter 6 – Primary tests General tests to ensure the integrity of the gas flows

and vacuums.

Chapter 7 – Start up basics The minimal conditions needed to start up the

detector.

Chapter 8 – Applications and Analytical Procedures Describes the general operation of the system.

Includes information on controls, connections,

functional tests and basic operating parameters.

Chapter 9 – Service Information (Programming and Troubleshooting) Details on servicing the 7090 Series of analyzers,

general and preventative maintenance

schedules, as well as removal and replacement

procedures.

Chapter 10 – Data Sheets Data Sheets

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TABLE OF CONTENTS

1. GENERAL INFORMATION ................................................................................................1

1.1 FCC NOTICE ......................................................................................................................... 1

1.2 DISPOSAL ............................................................................................................................. 1

1.3 CE NOTICE ........................................................................................................................... 2

1.4 WARRANTY .......................................................................................................................... 3

1.5 RETURN POLICY .................................................................................................................... 5

1.6 CONTACT US ........................................................................................................................ 7

2. SAFETY ......................................................................................................................... 10

2.1 PROPER USE AND SAFETY ...................................................................................................... 10

2.2 CERTIFICATIONS .................................................................................................................. 11

2.3 SYMBOLS ........................................................................................................................... 12

2.4 ENVIRONMENTAL PROTECTION .............................................................................................. 13

PERSONAL PROTECTIVE EQUIPMENT (PPE) ......................................................................................... 11

3. INTRODUCTION ............................................................................................................ 14

3.1 INTENDED AUDIENCE ........................................................................................................... 14

3.2 PRINCIPLE OF OPERATION ..................................................................................................... 14

3.2.1 Principle of Operation: Nitrogen .............................................................................. 14

3.2.2 Principle of Operation: Sulfur ................................................................................... 15

4. INSTALLATION .............................................................................................................. 18

4.1 PRE-INSTALLATION REQUIREMENTS ........................................................................................ 18

4.1.1 Electrical Requirements: .......................................................................................... 18

4.1.2 Environmental and space requirements: ................................................................. 19

4.1.3 Materials Requirements ........................................................................................... 20

4.1.4 Materials Supplied by PAC: ...................................................................................... 20

4.1.5 Gas Requirements: ................................................................................................... 21

4.1.6 Plumbing Requirements: .......................................................................................... 22

4.2 INSTALLATION PROCEDURES .................................................................................................. 25

4.2.1 Unpacking and inspection ........................................................................................ 25

4.2.2 Shipping damage reports ......................................................................................... 25

4.3 PHYSICAL INSTALLATION ....................................................................................................... 27

4.3.1 Gases ........................................................................................................................ 27

4.3.2 Furnace Base ............................................................................................................ 28

4.3.3 Pyrotubes and furnace ............................................................................................. 29

4.3.4 Inlet adapter ............................................................................................................. 30

4.3.5 Gas transfer lines ...................................................................................................... 32

4.3.6 Signal output cables ................................................................................................. 32

4.3.7 Vents ........................................................................................................................ 33

4.3.8 Injection systems ...................................................................................................... 33

4.3.9 Vacuum Pump .......................................................................................................... 33

5. SYSTEM OVERVIEW ...................................................................................................... 34

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5.1 FRONT PANEL CONTROLS ...................................................................................................... 34

5.2 REAR PANEL ....................................................................................................................... 36

5.3 INTERNAL COMPONENTS ....................................................................................................... 39

5.3.1 Vacuum pump .......................................................................................................... 41

5.4 FURNACE ........................................................................................................................... 42

6. PRIMARY TESTS ............................................................................................................ 44

6.1 PRESSURE TESTS ................................................................................................................. 44

6.1.1 Gas supply (External) leak check .............................................................................. 44

6.1.2 Vacuum internal leak check ..................................................................................... 45

6.1.3 7090 pressure leak check procedure ....................................................................... 46

6.1.4 Resetting system to factory defaults ....................................................................... 48

6.2 GC POWER-UP ................................................................................................................... 48

6.3 MODEL 7090 POWER-UP ..................................................................................................... 48

6.3.1 Check list .................................................................................................................. 48

6.3.2 Power-up and functional tests ................................................................................. 49

6.3.3 Furnace power-up .................................................................................................... 50

7. START-UP BASICS ......................................................................................................... 54

7.1 BASELINE ADJUSTMENTS ....................................................................................................... 54

7.2 HIGH VOLTAGE .................................................................................................................... 54

7.3 OZONE GENERATOR ............................................................................................................. 54

8. APPLICATIONS AND ANALYTICAL PROCEDURES ............................................................. 56

8.1 IMPORTANT BASICS .............................................................................................................. 56

8.1.1 Gas and carrier flows ................................................................................................ 56

8.1.2 System flow considerations ..................................................................................... 58

8.1.3 System gas flow adjustments ................................................................................... 58

8.2 OPTIMIZING SULFUR DETECTION ............................................................................................ 59

8.3 OPTIMIZING NITROGEN DETECTION ........................................................................................ 64

9. SERVICE INFORMATION ................................................................................................ 66

9.1 FURNACE TEMPERATURE CONTROLLER PROGRAMMING PROCEDURE ............................................ 66

9.1.1 Initial power up ........................................................................................................ 66

9.1.2 Temperature Set Procedure ..................................................................................... 68

9.1.3 Auto Tune Procedure ............................................................................................... 68

9.2 THERMAL ELECTRIC COOLER (TEC) TEMPERATURE CONTROLLER PROGRAMMING PROCEDURE ........ 70

9.2.1 Initial Power up ........................................................................................................ 70

9.2.2 Temperature Set Procedure (see following text) ..................................................... 73

9.2.3 Auto Tune Procedure ............................................................................................... 73

9.3 BOARD ALIGNMENT PROCEDURES .......................................................................................... 74

9.3.1 Printed Circuit Boards Overview .............................................................................. 75

9.3.2 Ozone Generator Board – p/n 103603 ..................................................................... 76

9.3.3 Signal Processing (58141R3 Alignment Procedure) ................................................. 77

9.3.4 High Voltage Power supply voltage (58160) Adjustment ........................................ 79

9.3.5 Display Select Adjustment Procedure (58183) ........................................................ 80

9.4 FUSE REQUIREMENTS ........................................................................................................... 83

9.5 LEAK CHECK PROCEDURES .................................................................................................... 83

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9.5.1 Mass Flow Controller Scaling Procedure and Vacuum Test ..................................... 83

9.5.2 Pressure Test (With Furnace) ................................................................................... 85

9.6 START-UP & SHUTDOWN PROCEDURES ................................................................................... 85

9.6.1 Start-up Procedure ................................................................................................... 85

9.6.2 Shutdown Procedure................................................................................................ 86

9.7 ROUTINE MAINTENANCE ...................................................................................................... 86

9.7.1 Daily .......................................................................................................................... 87

9.7.2 As Needed ................................................................................................................ 87

9.7.3 Reaction Chamber Cleaning Procedures .................................................................. 87

9.8 PRACTICAL TROUBLESHOOTING CHECKLIST .............................................................................. 88

9.8.1 Gases ........................................................................................................................ 88

9.8.2 Instrument Conditions ............................................................................................. 89

9.8.3 Vacuum Pump .......................................................................................................... 89

9.8.4 Furnace ..................................................................................................................... 89

9.8.5 Gas Chromatograph Conditions ............................................................................... 89

9.8.6 Proper Integrator Channel selected ......................................................................... 90

9.8.7 Detection Problems .................................................................................................. 90

9.8.8 Noise Problems ........................................................................................................ 90

9.8.9 Practical Troubleshooting Hints ............................................................................... 90

9.9 ANALYTICAL TROUBLESHOOTING ............................................................................................ 91

10. DATA SHEETS ............................................................................................................. 104

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Left Blank

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PAC 7090 Series IOS Manual

7090 Series User Manual • Rev D MAN 7090 Page 1

1. GENERAL INFORMATION

1.1 FCC Notice

This equipment has been tested and found to comply with the limits for a Class A digital device, pursuant to Part 15 of the FCC Rules. These limits are designed to provide reasonable protection against harmful interference when the equipment is operated in a commercial environment. This equipment generates, uses, and can radiate radio frequency energy and, if not installed and used in accordance with the instruction manual, may cause harmful interference to radio communications. Operation of this equipment in a residential area is likely to cause harmful interference in which case the user will be required to correct the interference at his expense.

1.2 Disposal

Correct disposal of Waste Electrical and Electronic Equipment in the end-of life Applicable in the European Union and other European countries with separate collection systems

This product is designed for exclusive professional use by commercial companies. This marking shown on the product or its literature, indicates that it should not be disposed with other household wastes at the end of its working life. To prevent possible harm to the environment or human health from uncontrolled waste disposal, please separate this from other types of wastes and recycle it responsibly to promote the sustainable reuse of material resources. Business users should contact the producer or the importer and check the terms and conditions of the purchase contract. If you have a separate agreement with your producer or importer such that you will take care of end-of-life disposal on your own, please ensure an environmentally sound disposal according to the legal regulations for electric and electronic waste equipment in your country. This product should not be mixed with other commercial wastes for disposal. The above WEEE-symbol is the official marking for equipment under the WEEE-scope. In some EC-Member states, "pure B2B equipment" is not necessarily marked with the waste bin-symbol. To provide a homogenous EC-wide procedure, PAC uses the marking in all EC-Member states.

NOTE:

User changes or modifications not expressly approved by PAC, L.P. could void the

user’s authority to operate the equipment. Use only accessories provided with the

7090 Series or PAC approved options for continued FCC compliance.

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1.3 CE Notice

CE Notice

The symbol indicates the 7090 Series’ compliance with the European Union (EU)

directives and standards listed below:

The symbol indicates PAC’s compliance with the European Union (EU) directives

and standards listed below:

EMC Directive 89/336/EEC

EN 55011: 1998 “Electrical equipment for measurement, control and

laboratory use. EMC requirements. Particular requirements. Test

configurations, operational conditions and performance criteria for

sensitive test and measurement equipment for EMC unprotected

applications”

This system contains devices classified for use in a typical Class A commercial

environment and is not designed or intended for use in other EMC environments. The

user of this system is obliged to properly use and install the system and to take all

steps necessary to remove sources of interference to telecommunications or other

devices.

Issued 2012

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7090 Series User Manual • Rev D MAN 7090 Page 3

1.4 Warranty

STANDARD LIMITED WARRANTY OF

PETROLEUM ANALYZER COMPANY, L.P.

I. Limited Warranty

1. Limited Warranty. For each product sold, PAC offers to the original owner (“BUYER”) a limited warranty against failure to conform to the product specifications or any defects in material and workmanship for a period of twelve (12) months

from the date of installation of the product or eighteen (18) months from date of invoice, whichever is less (the “Initial Warranty”). If

a failure to conform to specifications or a defect in materials or workmanship is discovered within the Initial Warranty period, BUYER must promptly notify PAC in writing, which notification, in any event must be received no later than 14 months from the date

of installation of the product. Within a reasonable time after such notification, PAC will correct any failure to conform to

specifications or any defect in materials or workmanship, or in lieu of such repair, and at its sole option, shall replace the product, F.O.B. PAC’s city of shipment or refund the purchase price, less a reasonable reduction in such purchase price as determined by PAC.

In no event shall PAC be liable for consequential or special damages, or for transportation, installation, adjustment or other expenses,

which may arise in connection with such products or warranty claim. Products and parts sold by authorized PAC Distributors are covered by the Distributor’s terms and conditions.

During the Initial Warranty period, PAC offers a limited warranty on each part or product repaired or replaced by a PAC

service person for a period ending the later of (a) the remaining term of the product’s Initial Warranty or (b) ninety (90) days from the date of repair or replacement whichever is longer. After expiration of the Initial Warranty period, PAC offers a ninety (90) day

limited warranty on each part or product repaired or replaced by a PAC service person. PAC further warrants that the products and

parts it sells will conform to PAC’s written specifications therefor. The foregoing limited warranties cover parts and labor only and PAC does not warrant and will not reimburse the BUYER for any other costs relating repairing or replacing the product at issue. The

foregoing limited warranties apply only to the repair or replacement of defective parts and/or products and such determination will be in the sole discretion of PAC. The limited warranties of this Section I.1 are further subject to those warranty exclusions set forth

below.

2. Aftermarket. The use of third party parts in the operation or maintenance of the product or repairs or servicing by unauthorized service personnel immediately voids all further warranty obligations of PAC. PAC genuine consumables are sold on

an as-is basis and have no warranty beyond being shipped in good working order.

3. Limited Warranty Exclusions. Other than the warranties set forth in Section I.1., PAC disclaims any and all

express or implied warranties, including but not limited to the warranty of merchantability, fitness for a particular purpose and non-

infringement of the intellectual property of others. Provided, however, this Intellectual Property Warranty shall apply to the product

only so long as BUYER (i) does not modify the product, combine the product with other elements or use the product in a practice or a process, and such modification, combination or practice of which the product forms a part is the subject of such claim or allegation of

infringement and (ii) uses the product under ordinary conditions and for their intended purposes. PAC makes no warranty, express or

implied, as to the design, sale, installation or use of its products. PAC’s warranties will not be enlarged by, nor will any obligation or liability of PAC arise due to PAC providing technical advice, facilities or service in connection with any product. PAC disclaims any

and all other warranties and representations and PAC provides no warranty on the oral representations made by its personnel while

they are undertaking Services for BUYER. There is no warranty by PAC with respect to any product’s: (i) uninterrupted or error-free operation; (ii) actual

performance, other than the product’s capability to meet PAC’s specifications therefor; (iii) removal or installation from a worksite or

process; (iv) electronic components or associated accessories (including without limitation circuit boards and integrated circuits); (v) maintenance (including without limitation gasket and seal replacements, adjustments, minor repairs and other inspection

requirements, preventative or otherwise); (vi) use under inappropriate conditions or not in accordance with operating instructions; or

(vii) use in connection with the operation of a nuclear facility. There is no warranty for products determined to be, in PAC’s sole discretion, damaged or impaired as a result of (a) misuse, neglect or accident; (b) improper application, installation, storage or use;

(c) improper or inadequate maintenance or calibration; (d) operation outside of the published environmental specification;

(e) improper site preparation or maintenance; (f) unauthorized repairs or replacements; (g) modifications negligently or otherwise improperly made or performed by persons other than PAC; (h) BUYER-supplied software or supplies; (i) use in conjunction with or

interfacing with unapproved accessory equipment; (j) use of ABC-style or dry powder fire suppression agents; or (k) leaked sample

materials. To the extent a PAC product is used in connection with the operation of a nuclear power facility, BUYER agrees to indemnify and hold PAC harmless from any and all actions, claims, suits, damages and expenses arising from such use. PAC provides

no warranty on the oral representations made by its personnel while they are attempting to assist BUYER in the operation of a

product. This Standard Limited Warranty does not apply to items consumed by the products during their ordinary use, including but not limited to fuses, batteries, paper, septa, fittings, screws, fuses, pyrolysis, dryer or scrubber tubes, sample boats, furnaces or lamps.

This warranty is valid only if genuine PAC parts, consumables and standards are used in PAC products.

4. Resale products are goods (that are sold with PAC’s products) which are not manufactured by PAC and which are supplied as an accommodation to BUYER. PAC MAKES NO WARRANTY FOR RESALE PRODUCTS, EITHER EXPRESS

OR IMPLIED, INCLUDING WARRANTIES OF MERCHANTABILITY AND FITNESS FOR A PARTICULAR PURPOSE. THE

SOLE WARRANTY SHALL BE THAT OF THE RESALE PRODUCT MANUFACTURER. BUYER agrees that PAC has no liability for resale products beyond the services within PAC’s direct control necessary to

reasonably discharge the above stated responsibility and that PAC shall not be liable for delays caused by resale product manufacturer.

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PAC does not warrant products it does not manufacture except to the extent the warranty of the manufacturer of the product at issue

passes through or is otherwise assigned to PAC. BUYER further agrees that BUYER’s SOLE AND EXCLUSIVE REMEDY for PAC’s breach of the stated responsibility shall be limited to the difference between the resale product manufacturer’s price to PAC

and PAC’s price to BUYER for resale products.

5. Expenses for Non-Warranty Work. All repairs or replacements by PAC after the expiration of any applicable limited warranty period will be performed in accordance with PAC’s standard rate for parts and labor. Further, if upon PAC’s

inspection and review, PAC determines the condition of the product for which a warranty claim is submitted is not caused by a defect

in PAC’s material and workmanship, but is the result of some other condition, including but not limited to damage caused by any of the events or conditions set forth in Section I.3., BUYER shall be liable for all expenses incurred by PAC to conduct the inspection

and review of the product.

6. Exclusive Remedy. The limited warranty contained herein constitutes BUYER’s exclusive remedy with respect to products sold by PAC and PAC’s liability shall be exclusively limited to the written limited warranty specified herein. No

employee, representative or agent of PAC is authorized to either expressly or impliedly modify, extend, alter or change any of the

limited warranties expressed herein to BUYER. 7. Procedure and Costs. All limited warranty claims must be made in writing promptly following discovery of any

failure to conform to specifications or any defect in materials or workmanship. BUYER must hold products for inspection by PAC. If

requested by PAC, BUYER must send the product to PAC for inspection. Any such returns by BUYER will be at BUYER’s expense and BUYER will remain liable for any loss of or damage to the product during such product’s transportation to PAC. No products

will be sent to PAC for inspection unless PAC has authorized BUYER to do so.

8. Terms and Conditions. PAC’s General Terms and Conditions are incorporated herein by reference and BUYER accordingly agrees to be bound by the terms thereof.

II. Limitations on PAC Liability

1. In General. BUYER agrees that in no case shall PAC be liable for any special, incidental, consequential, or punitive

damages based upon any legal theory whether or not such damages are foreseeable. such damages include, but are not limited to, loss

of profits, loss of savings or revenue, loss of use of the product or any associated equipment, cost of capital, cost of any substitute equipment, facilities or services, downtime, the claims of third parties including customers, injury to property and, unless precluded

under applicable state law, bodily and personal injury. PAC’s total liability for any and all losses and damages arising out of any and

all causes whatsoever including, without limitation, defects in the product(s), services, software, or documentation supplied or breach of this agreement, shall in no event exceed the purchase price of the applicable product(s). BUYER agrees these limitations on PAC’s

liability are reasonable and reflected in the amounts charged by PAC for its products.

2. BUYER Data. If any data supplied by BUYER, whether in the form of BUYER specifications or pursuant to any purchase order or other documentation, proves to be inaccurate, any warranties or other related obligations of PAC relying thereon will be void.

3. Force Majeure. This Standard Limited Warranty does not cover and PAC shall not be liable for either direct or

consequential damage caused, either directly or indirectly, as a result of: (i) any act of God, including but not limited to natural disaster, such as floods, earthquakes, or tornadoes; (ii) damages resulting from or under the conditions of labor disputes, strikes or

riots, insurrection, civil commotion or war; (iii) damages or improper operation due to intermittent power line voltage, frequency,

electrical spikes or surges, unusual shock or electrical damage; (iv) accident, fire or water damage, neglect, corrosive atmosphere or causes other than ordinary use; (v) failure of supplies or transportation, or governmental action or; or (vi) any other causes beyond

Seller’s reasonable control.

4. Limitation on Warranty Claims. Prior to any obligation of PAC to perform any limited warranty service as set forth herein, BUYER must have: (i) paid all invoices to PAC in full, whether or not they are specifically related to the product at issue; and

(ii) notified PAC of the limited warranty claim within sixty (60) days from the date BUYER knew or had reason to know of the defect.

III. Compliance

1. In General. These Warranty Terms are subject to change without notice. PAC also retains the right to modify these

warranty terms in order to comply with policy or laws governing warranty issues in states or countries having specific remedies differing or additional to those described within this document.

2. Severability. If any one or more of the provisions or subjects contained in the Agreement shall for any reason be held

invalid, illegal, or unenforceable, it shall not affect the validity and enforceability of any other provisions or subjects.

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7090 Series User Manual • Rev D MAN 7090 Page 5

1.5 Return Policy

No product may be returned, whether in warranty or out of warranty, without first

obtaining approval from PAC, L.P. No replacements will be provided nor repairs be

made for products returned without such approval. A return authorization number must

accompany any returned product. The buyer will pay for the expense of returning the

unit to PAC, L.P. for service. The status of any product returned later than 30 days after

the issuance of a return authorization number will be subject to review.

Products may not be returned that are contaminated by radioactive materials, infectious

agents, or other materials constituting health hazards to PAC, L.P.'s employees.

RETURNED PRODUCT WARRANTY DETERMINATION

After PAC, L.P.’s examination, warranty or out-of-warranty status will be determined.

If a warranted defect exists, the product will be repaired at no charge and shipped pre-

paid back to the buyer. Warranty repairs do not extend the original warranty period.

If an out-of-warranty defect exists, the buyer shall be notified of the repair cost. At such

time, the buyer must issue a valid purchase order to cover the cost of the repair and

freight, or authorize the product to be shipped back as is, at the buyer’s expense. Failure

to obtain a purchase order number approval within fifteen days of notification will result

in the product being returned as is, at the buyer’s expense.

ON-SITE REPAIR

If a PAC L.P. product cannot be made functional by telephone assistance or by

installing replacement parts, and cannot be returned to PAC L.P. for repair, the

following policy applies:

PAC L.P. will provide an on-site field service representative in a reasonable amount of

time, provided that the customer issues a valid purchase order to PAC L.P. covering all

transportation, subsistence, and prevailing labor costs, including travel time, necessary

to complete the repair. For warranty field repairs, the customer will not be charged for

the cost of transportation, labor, or materials. Special service rates may apply when

service is rendered at times other than normal work periods.

Inspection

This instrument was thoroughly inspected and carefully packed before leaving our

factory. Responsibility for its safe delivery was assumed by the carrier upon acceptance

of the shipment. Claims for loss or damage sustained in transit must be made to the

carrier by the recipient as follows:

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Visible Loss or Damage

Note any external evidence of loss or damage on the freight bill or express receipt, and

have it signed by the carrier’s agent. Failure to adequately describe such external

evidence of loss or damage may result in the carrier’s refusing to honor your damage

claim. The form required to file such a claim will be supplied by the carrier.

Concealed Loss or Damage

Concealed loss or damage means loss or damage which becomes apparent when the

merchandise is unpacked and inspected. Should concealed loss or damage occur, make a

written request for inspection by the carrier’s agent within 15 days of the delivery date,

then file a claim with the carrier since the damage is the carrier’s responsibility.

By following these instructions carefully, we guarantee our full support of your claim to

be compensated for loss from shipping damage.

DO NOT - for any reason - return the instrument without first obtaining

authorization. In any correspondence to PAC, please supply the nameplate data,

including catalog number and serial number. The nameplate is located on the rear of the

instrument housing.

Record of Serial Number and Purchase Date

Catalog Number: ________________________

Serial Number: ________________________

Purchase Date: _________________________

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7090 Series User Manual • Rev D MAN 7090 Page 7

1.6 Contact Us

If you have any questions about your “7090 Series Nitrogen / Sulfur GC Detector”

contact us using the information below:

PAC L.P.

8824 Fallbrook Drive

Houston, TX 77064

WEB: http://www.paclp.com

Main Number: 281 940-1803

Service: 800 444-TEST (8378) or 281 580-0339

Fax Number: 281 580-0719

Email Support: [email protected]

[email protected]

Additional contact information for our regional offices is on the next page.

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Web: http://www.paclp.com

Phone: USA

France

Germany

Singapore

Netherlands

Russia & CIS

China

South Korea

Thailand

Abu Dhabi

+1 281 940 1803

+33 231 264 300

+49 9343 6400

+65 6412 0890

+31 10 462 4811

+7 495 617 10 86

+86 10 65072236

+82 2 785 3900

+66 2 627 9410

+971 2 446 9671

Fax: USA

France

Germany

Singapore

Netherlands

Russia & CIS

China

South Korea

Thailand

Abu Dhabi

+1 281 580 0719

+33 231 266 293

+49 9343 640 101

+65 6412 0899

+31 10 462 6330

+7 495 913 97 65

+86 10 65072454

+82 2 785 3977

+66 2 627 9401

+971 2 446 9672

Sales: USA

France

Germany

Singapore

Netherlands

Russia & CIS

China

South Korea

Thailand

Abu Dhabi

mailto:[email protected]

mailto:[email protected]

mailto:[email protected]

mailto:[email protected]

mailto:[email protected]

mailto:[email protected]

mailto:[email protected]

mailto:[email protected]

mailto:[email protected]

mailto:[email protected]

Service: USA

France

Germany

Singapore

Netherlands

China

South Korea

Thailand

Abu Dhabi

mailto:[email protected]

mailto:[email protected]

mailto:[email protected]

mailto:[email protected]

mailto:[email protected]

mailto:[email protected]

mailto:[email protected]

mailto:[email protected]

mailto:[email protected]

sema01
Text Box
NOTE: There is no page 9.
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2. SAFETY

2.1 Proper use and safety

The 7090 Series of Nitrogen / Sulfur GC Detectors is designed to be installed, operated and

maintained as specified below and in other parts of this manual. Failure to operate a 7090

analyzer as specified may produce erroneous data and possible equipment failure. Some of the

conditions for proper and improper use of the detector are provided as follows:

PROPER USE

Normal Use – The Model 7090 Series detectors are advanced analytical systems for the

specific determination of nitrogen and/or sulfur containing compounds in simple or complex

matrices. Operation for any other use, and the results obtained from any other use, cannot be

guaranteed.

Corrosive Environments – The standard configuration of the 7090 Series detector is not

intended for use in corrosive environments.

Direct Sunlight – The detector should not be exposed to direct sunlight or inclement

weather conditions.

Ambient Temperature – The best accuracy and precision is obtained when the detector

is located in a temperature controlled environment.

Electrical Power – The electrical power source for the detector must be capable of

delivering greater than 1200 Watts of power from either a 115-VAC or 220-VAC source. Each

7090 detector is built to be powered by either 115 VAC or 220 VAC. Care must be taken to avoid

connecting the detector to the wrong AC power supply.

Sample Analysis – To ensure the sample being analyzed is representative of the current

process status, sample to the detector must be delivered by an approved, leak-free sample

handling system. The sample handling system must eliminate or minimize “dead volumes” and

areas in the flow path where new sample can be mixed with old sample.

System Leaks – Gas leaks in the system will result in poor performance and possible

damage to the detector.

Light Leaks – Light leaks in the detector or PMT housing will increase background

noise.

Gas Quality – Air and other gases supplied to the detector must be filtered and pure as

specified.

Preventative Maintenance – In order to ensure proper performance, preventative

maintenance (PM) procedures must be performed at regular intervals.

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Personal Protective Equipment (PPE)

Wear safety glasses.

Wear nitrile gloves or equivalent type.

Wear appropriate dusk mask (when handling and cutting the RCF).

All Caution and Warning notations in this manual, on tags and in other publications pertaining to

the installation, operation and maintenance of the 7090 Series detector must be read and

observed. Failure to consider the Caution and Warning messages can lead to severe personal

injury and/or equipment damage. Operators are urged to observe standard operation and

maintenance safety practices and the specific safety warnings and labels in this manual and on the

equipment itself.

2.2 Certifications

The system and its components have been designed with safety in mind. The design applies to the

use, the conditions and the instructions described in the documentation. The system:

Meets the requirements of the European Directives concerning health, hygiene and safety. The

standards applied are listed in the “CE Declaration of Conformity”.

For a copy of the corresponding declarations, please consult PAC.

If the user makes changes or modifications that are not expressly approved by PAC, the company

reserves the right to void the user’s authority to operate the equipment.

During performance or routine maintenance, the system operator may be exposed to potentially

dangerous chemicals, temperatures, electrical voltages and/or other hazards. In order to reduce

the personal risk involved, the user must follow established guidelines and accepted standards for

general analytical laboratory operation.

For established safety requirements, government safety and disposal standards, please refer to the

corresponding Material Safety Data Sheet (MSDS) for each PAC-supplied product and also

reference the corresponding vendor supplied MSDS for each sample and standard utilized with

the product.

WARNING:

Failure to follow the instructions and procedures contained in this manual could

result in death or serious injury. The instructions and procedures must be

performed by qualified and trained personnel only. Do not perform installation

or maintenance operations or procedures outside the scope of this manual.

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2.3 Symbols

This symbol (exclamation point in a triangle) indicates a general Caution or

Warning. A Caution alerts you to information that is important for

protecting the equipment and performance. A Warning alerts you to

information that is important for protecting yourself, others and equipment

from damage.

This symbol (a lightning bolt in a triangle) indicates an electrical shock

hazard. Inside the 7090 Series are exposed live voltage circuits. The 7090

Series should be opened only by qualified service personnel. To prevent

electrical shock hazard DO NOT operate the 7090 Series in rain or wet

conditions.

This symbol (three wavy lines over a straight line in a triangle) indicates a

hot surface. During operation, the 7090 Series and associated equipment

surfaces get hot. To prevent burns exercise caution when operating the

detector.

This symbol (a fire in a triangle) indicates a fire hazard. During operation,

the 7090 Series surfaces near the furnace get hot. To prevent burns exercise

caution when operating the detector.

NOTE:

A note pictogram denotes a recommendation that, if not followed, may

result in minor damage.

TIP:

A tip pictogram denotes a recommendation that can help in understanding

how to operate or service the apparatus.

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2.4 Environmental Protection

Observe all local regulations and recommendations for the disposal and recycling of parts and

materials that have been used or replaced during installation, operation, and maintenance tasks.

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3. INTRODUCTION

As a gas chromatographic detector, the 7090 Series is the most advanced analytical system

available for the specific determination of nitrogen and/or sulfur containing compounds in simple

or complex matrices. The 7090 provides unrivaled selectivity and sensitivity to nitrogen and/or

sulfur by rendering most organic compounds transparent.

3.1 Intended Audience

The contents of this document must be read, understood and observed in all points by each person

responsible for the preparation, transport, storage, installation, operation, maintenance, and repair

of the detector, before starting work with and on the instrument.

This particularly applies to the safety instructions in this manual.

3.2 Principle of Operation

3.2.1 Principle of Operation: Nitrogen

The 7090N is capable of two distinctly different modes of operation for nitrogen determination:

1) Total Nitrogen Mode and 2) Nitrosamine Mode. The Total Nitrogen Mode can be operated

simultaneously with the Total Sulfur Mode, but the Nitrosamine Mode cannot.

The principle of operation for the Total Nitrogen Mode begins with the complete, high

temperature oxidation of the entire sample matrix as illustrated in the equation (1) below.

(1) R-N + R-H + O2 → CO2 + H2O + NO + SO2 + MOx

where R-N is any chemically bound nitrogen compound and R-H is any non-nitrogenous organic

compound.

Oxidation products include CO2, H2O, NO, SO2, and various other oxides (designated MOx

above). The conversion of all chemically bound nitrogen to NO (nitric oxide) is quantitative. The

combustion gases are routed to the detector module for quantitation.

As seen in equation (2), the NO is reacted with O3 (ozone), produced by an on-board ozone

generator, to form NO2* (nitrogen dioxide in the excited state). As the excited species decays to

the ground state, light is emitted and detected at specific wavelengths by a photomultiplier tube.

This chemiluminescent emission is specific for nitrogen and proportional to the amount of

nitrogen in the original sample. Only chemically bound nitrogen is detected; atmospheric nitrogen

(N2) is not sensed.

(2) NO + O3 → NO2* + O2 → NO2 + hν

The principle of operation for the Nitrosamine Mode begins with the selective, high temperature

cleavage of NO from nitrosamine compounds in the sample as illustrated in equation (3). As each

component elutes from the GC column, the component is combined with oxygen at a temperature

of approximately 500°C. At this temperature, only N-nitroso compounds will thermally cleave to

yield NO (nitric oxide) and the nitric oxide formation is quantitative. The furnace gases are routed

through a membrane drying system to remove all water and then to the detector module for

quantitation. The nitric oxide is quantitated according to equation (2).

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(3) R-N-NO → NO + (pyrolysis products)

Nitrogen calibration standards may be analyzed to produce calibration curves. External data

systems may be interfaced to the PAC 7090 for calculations and documentation.

Figure 3-1 Connections for gas intake on a nitrogen detector

3.2.2 Principle of Operation: Sulfur

The principle of operation for sulfur detection begins with the complete, high temperature

oxidation of the entire sample matrix as illustrated in equation (4) where R-S is any organic sulfur

compound and R-H is any non-sulfur containing organic compound. As each component elutes

from the GC column, the component is reacted with oxygen at temperatures from 700 to 1100°C.

Oxidation products include CO2, H2O, SO2, and various other oxides (designated MOx below).

The conversion of chemically bound sulfur to SO2 (sulfur dioxide) is quantitative. The oxidized

gases are then reacted with hydrogen in the reductive zone of the furnace, generating H2S and

other reduced sulfur species as illustrated in equation (5). These reduced sulfur species are then

passed through the reaction chamber where they react with ozone.

(4) R-S + R-H + O2 → CO2 + H2O + SO2 + MOx

(5) SO2 + H2 → H2S + Other Reduced Species

According to equation (6), the H2S and other reduced sulfur species are reacted with O3 (ozone),

produced by an onboard ozone generator to form SO2 * (sulfur dioxide in the excited state). As

the excited species decays to the ground state, light is emitted and detected, at specific

wavelengths, by a photomultiplier tube. This chemiluminescent emission is specific for sulfur and

is proportional to the amount of sulfur in the original sample.

(6) H2S + Other Reduced Species + O3 → SO2* → SO2 + hν

Sulfur calibration standards may be analyzed to produce calibration curves. External data systems

may be interfaced to the PAC 7090 Series for calculations and documentation.

NO Sample

Ozone inlet

Sample vent

Pressure

Sensor

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Figure 3-2 Connections for gas intake on a sulfur detector

H2S Sample

Ozone inlet

Sample vent

Pressure

Sensor

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Left Blank

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4. INSTALLATION

4.1 Pre-installation Requirements

Figure 4-1 Model 7090 Front view

4.1.1 Electrical Requirements:

Stable 115 VAC, 50/60 Hz, 1200 Watts or Stable 230 VAC, 50/60 Hz, 1200 Watts.

The PAC 7090 system utilizes stable 115 VAC, 50/60 Hz or 230 VAC, 50/60 Hz. A 10 amp

circuit is required for 115 VAC and 5 amp for 230 VAC. A good earth ground is necessary for

proper operation.

WARNING:

A poor ground may present a severe shock hazard. If a replacement power plug is

used, confirm that the wiring is correct and that the plug is rated to carry the

maximum current.

AC power is supplied via a three conductor power cord. This cord is fitted with a three-prong

plug rated for 12 amps. This plug will mate to most 115 VAC receptacles. For 230 VAC and

some 115 VAC operations, a different plug may be supplied. In all cases, care should be taken to

ensure that the color code, as shown in the following figure, is followed exactly.

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Figure 4-2 Follow the color code when making power connections

NOTE:

The analyzer is set for either 115VAC or 230 VAC operation.

4.1.2 Environmental and space requirements:

PAC 7090 systems can operate over a wide range of environmental conditions. However, for

optimum performance, the following conditions are recommended:

Temperature: 10 to 27°C (50 to 80°F)

Humidity: 25 to 75 % (no condensation)

NOTE:

Operation of the instrumentation outside of these conditions may result in

unsatisfactory and erratic performance.

A corrosive atmosphere will, in time, cause problems with solder joints, gold-plated contacts, and

other reactive surfaces. Likewise, dust, smoke, or other airborne particulate matter that may be

swept in by the cooling fans may collect on internal surfaces. This particulate accumulation can

retain moisture and cause short circuits or prevent thermal radiation from heat transfer surfaces

resulting in component damage.

Model 7090 Size

Height: ..................................................... 61 cm (24 inches)

Width: ...................................................... 36 cm (14 inches)

Depth: ...................................................... 59 cm (23 inches)

Weight: ................................................... 28 kg (62 pounds)

Approximately 60 cm (24 inches) of bench space is required for the PAC 7090 system. The bench

should be capable of supporting at least 28 kg (62 pounds). This weight does not include the gas

chromatograph (GC). Adequate air space should be provided at the top and behind the instrument

for proper ventilation. Allow a minimum of 15 cm (6 inches) for ventilation. Additional space

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may be required if optional equipment or accessories are attached or used in conjunction with the

7090 system.

CAUTION:

Improper ventilation of the instrument may result in overheating and damage to

system components.

WARNING:

The furnace of the Model 7090 gets extremely hot! Care must be taken to ensure

that no temperature sensitive materials (plastics, solvents, chemicals, autosamplers,

compressed gas, etc.) are exposed to the furnace. Do not touch any part of the

furnace until it is completely cool – hot metal parts can cause severe burns!

4.1.3 Materials Requirements

Additional materials may be required if optional equipment or accessories are

attached or used in conjunction with the 7090 system.

4.1.4 Materials Supplied by PAC:

The PAC 7090 system includes the following modules and accessories:

Model 7090 Detector (with 7090 Accessory Kit*)

P/N 86060 Specified Furnace, 7090

* A 7090 accessory kit includes all the components that are not installed in the

7090 instrument. These include items such as the furnace, power and

thermocouple cables, the gas lines, power cord, signal cable, pyrotube(s), filters,

etc.

Part # Description

99506N–115V Model 7090 CLND, 115 V

99506N–230V Model 7090 CLND, 230 V

99506S–115V Model 7090 SCD, 115 V

99506S–230V Model 7090 SCD, 230 V

4.1.4.1 Optional 2nd Detector (Add-on):

The Optional 2nd

Detector includes the following modules and accessories:

2nd

7090 Detector (with its own Accessory Kit)

P/N 86060 Additional Specified Furnace, 7090

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Part # Description

101757 Model 7090 SCD, 115V, Add-on

101758 Model 7090 SCD, 230V, Add-on

101759 Model 7090 CLND, 115 V , Add-on

101760 Model 7090 CLND, 230 V, Add-on

4.1.4.2 Installation Kits:

Each 7090 detector or 7090 add-on requires an installation kit* to mount the 7090

furnace on the gas chromatograph (GC).

PAC makes available kits for a wide variety of GCs. Contact PAC for supported models.

*Installation kits include all the components that are required to adapt the 7090

furnace to the specific GC. Items may include adapter plates, furnace base

assembly, heater, and GC cover with shield.

4.1.4.3 Optional Equipment:

P/N 80.24.401/402 Vacuum Pump Assembly

The vacuum pump must be capable of a vacuum of 25 torr at a flow of 100

ml/min.

P/N 100259 Oxygen Purifier, 7090

* Gas Chromatograph (capillary column injector required)

* Accessories for capillary column analysis

4.1.4.4 Required Materials Not Supplied By PAC:

* Oxygen supply, dry, regulated to 3.0 bar (40 psig)

* Helium supply, dry, regulated to 3.0 bar (40 psig)

* Hydrogen supply, dry, regulated to 3.0 bar (40 psig)

4.1.5 Gas Requirements:

Dry* oxygen: ............................. 3.0 bar (40 psig), 99.75 %, 6-25 mL/min

Dry* helium: .............................. 3.0 bar (40 psig), 99.995 %, 0-20 mL/min

Dry* hydrogen†: ....................... 3.0 bar (40 psig), 99.995 %, 0-200 mL/min

*Dry is defined as 5 ppm weight water, maximum. †Hydrogen is required only for sulfur instruments.

Each gas line must be a dedicated line or should have an independent valve to turn off gases when

the system is not in use. A pressure gauge installed after the valve will enhance the ability to

properly perform a leak test of the system.

“Chromatographic” or “Zero” grade hydrogen and helium, and 99.75% grade oxygen are

recommended to ensure trouble-free performance. Gas suppliers have different grades and

designations for gas. Care should be taken when choosing the gases to be used.

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All gas streams must be regulated at 3.0 bar (40 psig) and in-line gas purifiers are absolutely

recommended for all gas supplies. All factory adjustments and settings are performed at 3.0 bar

(40 psig). However, in certain applications, the oxygen or helium line pressure may need to be

increased to 4.5 bar (60 psig).

WARNING:

High pressure gases should be handled with extreme care. Ensure that all relevant

safety precautions are carefully followed and that all gas lines, regulators, gas

purifiers, etc. are specified for the intended use.

All supply gases should be delivered through clean, dry aluminum, copper, or stainless steel

tubing. Tubing should be carefully washed and dried to ensure contamination free gas. Use

methylene chloride or trichloroethane followed by methanol or acetone and air drying to clean

new tubing. Other solvents may be used provided they are capable of dissolving oils or greases.

All solvents should be reagent grade or better.

CAUTION:

When using a liquid leak detector, care should be taken not to wet any

electrical or electronic components, or contaminate the analytical flow system.

Severe component damage or errant results may occur.

4.1.6 Plumbing Requirements:

All threaded connections (with the exception of compression type connections) should be

assembled carefully with Teflon® tape to guard against contamination and leaks.

All gases must be dry and free of particulate matter. Filters, gas scrubbers, and dryers are

available from PAC and are recommended in all cases.

Each supply gas cylinder requires a two-stage regulator to reduce the cylinder pressure to the

desired working pressure. PAC can supply the recommended regulators. `Care should be taken to

ensure use of the proper regulator for each gas in use.

Figure 4-3 illustrates a general flow diagram for the supply gases to an PAC 7090 system. This

procedure should be followed for each gas supply used (i.e., oxygen, helium, hydrogen, etc).

Sulfur Setup

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Figure 4-3 Instrument setup for nitrogen, sulfur, or nitrogen/sulfur simultaneous

Nitrogen Setup

Sulfur Setup

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Nitrogen / Sulfur Setup

Sulfur or Nitrogen/Sulfur Simultaneous Setup

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4.2 Installation Procedures

Select a suitable location that meets the criteria as stated in Section 4.1.

CAUTION:

Only trained personnel with prior knowledge of all pertinent safety procedures and

operations should be allowed to install, operate and service the instrument.

After determining the location for the 7090 Series instrument, unpack and install the analyzer by

performing the following procedures.

4.2.1 Unpacking and inspection

1. Unpack each item listed on the packing list.

2. Inspect items for damage.

3. Inspect the exterior of the detector for damage.

4. Place the detector onto the predetermined lab bench or table.

4.2.2 Shipping damage reports

Shipments are inspected immediately prior to being packaged for transportation. Since our

packaging exceeds all freight specifications, your equipment should have arrived in perfect

condition.

Our terms of sale are through Ex Works at shipping point, meaning that title to these goods is

passed to the final receiver when the goods are transferred to the carrier at our factory. If any part

of the shipment is damaged, we suggest reporting the damage immediately to the transportation

company. The following procedures are suggested for reporting damaged equipment.

Common Carrier:

If the item is discovered at the time of delivery, have the driver note the nature and extent of the

damage on the carrier’s copy and on the delivery copy of the freight bill.

If the item is discovered after delivery, call the carrier immediately after discovering the damage

and request that an inspection be made as soon as possible. Perform the following steps when

damaged items are found after delivery.

1. Contact the carrier immediately for an inspection of the item(s).

NOTE:

It is essential that the damaged item(s) be left in the original shipping container(s).

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2. Obtain a copy of the inspection report to support your claim.

NOTE:

Claims on air shipments must be filed within 270 days. Other claims must be filed

within 9 months of the shipping date.

3. File the claim as quickly as possible, even if you have to estimate the dollar

amount of the damage.

Parcel Delivery Service (UPS, DHL, FEDEX, etc.):

NOTE:

All claims must be initiated by the receiver.

Follow the steps listed above to report damages to shipments by common carriers, and notify our

office in Houston, Texas by dialing 800-444-8378. Our Technical Service Department will help

you process your claim.

NOTE:

Do not return the system or any item to the factory without factory authorization.

United Parcel Service (UPS):

NOTE:

All claims with UPS must be initiated by the receiver.

Unless otherwise specified, UPS is the preferred primary carrier for PAC shipments. Follow the

steps listed above for reporting damages caused when items are shipped by common carriers, and

notify our Customer Service Department, which will take the necessary action for your claim.

NOTE:

Do not return the system or any item to the factory without factory authorization.

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4.3 Physical Installation

4.3.1 Gases

Refer to the figure below to locate the gas inlet and outlet fittings on the rear of the 7090 system.

Figure 4-4 Gas Connections

Compression Fittings

Using the copper gas lines supplied with the 7090 system, connect the supply gases to the proper

gas inlet fittings. Refer to the figure below for the recommended assembly procedure for the

swage-type compression fittings included in the accessory kit.

Figure 4-5 Compression Fittings

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1. Insert tubing through nut.

2. Slide ferrule over the tubing.

3. Insert tubing with ferrule into the fitting until tubing bottoms in fitting.

4. Secure nut finger tight.

5. Use a wrench to turn the nut ¾” turn. After all gas fittings are connected, the

system should be carefully checked for leaks. Do not attempt to operate the

system until all leak checks have been performed.

4.3.2 Furnace Base

Select a suitable mounting location for the Furnace Base. Ensure that the furnace will not come

into direct contact with any electrical wiring or any plastic or flammable components on the gas

chromatograph or accessory equipment. The PAC Model 7090 may be installed on many

different gas chromatographs with several configurations. PAC provides installation kits for a

variety of GCs. Contact PAC for a list of available kits.

PAC installation kits contain an exploded assembly diagram to illustrate the mounting of base

assembly, furnace, and accessories on top of the GC.

WARNING:

The furnace of the Model 7090 gets extremely hot! Make ensure no temperature

sensitive materials (plastics, solvents, chemicals, autosamplers, compressed gas,

etc.) are exposed to the furnace. Refer to Figure 4-6 for mounting locations.

Figure 4-6 Furnace mounting on a typical gas chromatograph (GC)

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4.3.3 Pyrotubes and furnace

1. Locate the outer ceramic tube (P/N 12.94.302), the outer pyrotube nut or long

nut (P/N 10.25.753), and the 1/4" graphite ferrule (P/N 10.40.012), insert the

tube into the base and secure. Tighten by hand and then one quarter to one half

turn using a 1/2" wrench.

2. Slide the furnace assembly (P/N 86060) over the ceramic tube and tighten it

until it cannot be turned any further. Connect the furnace, power, and

thermocouple cables and route them to connections on the back of the 7090.

NOTE:

Mount the appropriate installation kit on top of the GC before installing the ceramic tube.

Figure 4-7 Furnace power and thermocouple connections

For Nitrogen detectors, perform the following steps.

1. Attach the 1/8” x 6 cm long tube (P/N 10.50.043) to the treated ¼” to 1/8”

reducing union with nut (P/N 10.10.042T).

2. Attach the filter (P/N 40.50.007) to the end of the 6 cm tube.

3. Attach the ¼” end of the reducing union with nut to top of the ¼” ceramic tube

with ¼” graphite ferrule (P/N 10.40.012).

4. Attach the nitrogen detector sample line from the 7090 to the top of the filter.

For Sulfur detectors, perform the following steps.

1. Disassemble the treated Tee fitting to make sure it has a ¼” graphite ferrule on

one end and a 1/8” graphite ferrule on the other end.

2. Attach the filter (P/N 40.50.007) to the shorter 6 cm tube.

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3. To the longer 10 cm tube, attach the 1/8” to 1/16” reducing union (P/N 30057).

4. Slide the 1/8” graphite ferrule over the 1/8” ceramic tube and slide the tube into

the Tee fitting.

5. Screw the 6 cm line and tighten to swage the ferrule holding the 1/8” ceramic

tube in place.

WARNING:

Over tightening the graphite ferrule will cause the 1/8" ceramic tube to break,

and the instrument will not detect sulfur compounds.

6. Loosely re-install the larger ¼” graphite ferrule and nut. Slide the whole

assembly and attach it to the ¼” ceramic tube. Tighten the nut to secure

assembly in place making sure that the 10 cm long line (the hydrogen feed tube)

points towards the back of the GC.

7. Attach the hydrogen gas line from the reducer fitting on the 10 cm line to the

hydrogen out fitting on the back of the 7090.

8. Attach the sulfur detector sample line from the 7090 to the top of the filter.

4.3.4 Inlet adapter

1. Remove the Column Adapter Assembly components from the Adapter Kit

P/N 19119 and assemble as follows:

Detector – Column Adapter Assembly P/N 19119

Insert the glass lined tubing, seal and straight union into the Detector Adapter (P/N 30380). Screw the union on finger tight.

Glass Lined Tubing (P/N 30429)

Sealing Ring (P/N 30140)

Straight Union (P/N 30282)

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Insert the Detector Stem Adapter into

the bottom of the furnace base from the

GC oven side.

Push the Adapter up until it stops in the

furnace base.

Tighten the ¼” SS nut securely to

hold the Adapter in place.

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The capillary column installation is detailed in 6.1.3.3 after all system checks have been

performed.

4.3.5 Gas transfer lines

Route the Oxygen Transfer Line from the Base Assembly to the back of the 7090 and connect to

the Oxygen Out fitting.

4.3.6 Signal output cables

The Model 7090 is not equipped with any integration capabilities and requires some means of

interpreting data; therefore a recorder or integrator is required. Refer to the requirements for the

proper voltage input. Plug the recorder cable into the lmv, lv, or 10v connector located on the rear

panel of the 7090. See the following for info.

The color code is as follows:

RED = POSITIVE (+)

BLACK = NEGATIVE (-)

CLEAR or GREEN = SHIELD

Left Rear of 7090

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4.3.7 Vents

The Model 7090 has an Ozone Scrubber to remove all ozone produced in the system. Venting of

the gases should produce no problem under normal situations, but if your sample contains any

potentially hazardous chemicals we recommend venting the vacuum exit into a hood to reduce

safety hazards. Check your local regulations regarding venting of gaseous materials.

4.3.8 Injection systems

Due to the nature of the samples, they can be easily absorbed onto metal surfaces. Care should be

taken to avoid the use of highly absorptive metals such as brass, copper, aluminum, etc. Use of

inert tubing is recommended in any cases where there is direct contact with the sample itself, such

as when utilizing a gas or a liquid sample valve. We also caution that most injector systems are

made of stainless steel components and sample contact with these metals is possible when using a

valve or syringe injection. When using a sample valve, we recommend completely bypassing the

injector.

4.3.9 Vacuum Pump

A vacuum pump is required in the operation of the 7090. The pump must be capable of a vacuum

of 25 torr at a flow of 100 ml/min. Do not connect the column to the detector base until a

preliminary leak check has been performed. Install a capillary plug fitting to the detector base as

shown in Figure 6.1. Do not turn the instrument on until a leak check of the entire system has

been performed (see Chapter 6).

WARNING:

Removal of the vacuum pump line from the scrubber assembly while furnace

and/or detection chamber are under vacuum could allow particulates to be

pulled into the reaction chamber.

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5. SYSTEM OVERVIEW

Before continuing with the setup of the PAC 7090 system, become thoroughly familiar with the

controls, connections, and general layout of the system.

NOTE:

For specific information concerning the function or operation of controls or

connections, consult the appropriate section of this manual or its addenda.

5.1 Front panel controls

This section explains the front panel controls and indicators to manipulate and monitor most of

the 7090 system’s analytical parameters, including detector sensitivity and baseline manipulation.

Figure 5-1 identifies the major front panel components and is followed by a brief explanation of

each.

NOTE:

All controls, except auto zero, are automatically initialized to the default settings upon

power-up. For more detailed information on the specific function(s) and

operation of the detector controls, refer to Chapter 8.

Figure 5-1 Front panel displays for the nitrogen analyzer (left) and sulfur (right)

1. Displays: for either high voltage set point or signal output.

2. Switch: for display of high voltage set point or signal output.

3. Sensitivity Selector: x1, x10, x25, x50 amplification factor for the Signal

Processing printed circuit board. The gain factor is used to increase or decrease

the sensitivity of the detector electronics. This is a multiplicative factor;

therefore, a factor of x50 is 50 times more sensitive than a factor of x1. This

control affects all analog outputs.

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4. Gain: The gain switch is the primary sensitivity control for the photomultiplier

tube preamplifier. HI gain is 100 times more sensitive than LOW gain. This

control affects all analog outputs.

5. Auto Zero: The auto zero button, when pushed, will automatically zero the

baseline of the detector. This function can be activated either manually or

remotely.

6. Ozone Generator On/Off Switch: Powers the ozone generator ON or OFF.

7. High Voltage On/Off: Powers the PMT voltage ON or OFF.

8. Nitrogen PMT Temperature Controller: See Section 9.2.1 for programming

procedures.

9. Furnace Temperature Controller: See Section 9.1 for programming

procedures.

10. Display LCD: Displays the value for the selection of furnace vacuum, detector

vacuum, ozone flow rate, oxygen flow rate, hydrogen flow rate, or furnace

vacuum set point.

11. Display Select: The Display Select Switch allows the user to scroll through

each of the six displays (Figure 5-2). Possible displays:

Figure 5-2 Status Lights

Furn Vac Displays the vacuum at the base of the furnace in

torr.

Det Vac Displays the vacuum in the Reaction Chamber in

torr.

O3 Displays the flow rate of ozone into the reaction cell.

O2 Displays the flow rate of oxygen into the furnace.

H2 Displays the flow rate of hydrogen into the furnace.

Furn Vac Set Displays the vacuum set point at which the Furn Vac

status light turns green.

12. Status Lights (six): The Status Lights provide a quick

inventory of the status of the instrument. Each light will change

from red to green as that portion of the system reaches a standby

mode and is ready for standard operations. All greens indicate that

the instrument is ready for normal operation.

O2 Oxygen Pressure LED: Indicates if the oxygen pressure is 30

psi or above. If oxygen is not present, the system cannot heat and

the power to the Ozone Generator will be turned off. If supply

pressure drops when a system is at temperature, the system will

cool down and the hydrogen solenoid will immediately turn off and

all lights will turn off except for the O2 light which will be red.

O3 Ozone On/Off Status LED: Indicates the current status of the

Ozone Generator.

The Generator will not operate if the oxygen pressure drops below

30 psi.

TEMP Temperature Status LED: The temperature status light is

designed to turn green when the instrument reaches a temperature

above 750°C and below 1100 °C.

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Furn Vac Furnace Vacuum LED: Furnace Pressure Status. Indicates the vacuum at the base

of the furnace is within limits. Typically this value in a system with no leaks is less

than 180 torr with an adequate vacuum pump. The light will not turn green until the

vacuum drops below 250 torr. The system will not heat if this light is not green.

H2 Hydrogen Status LED: The power to the hydrogen solenoid is set at the factory to

automatically turn on when the furnace reaches a temperature of 750 °C. If oxygen

pressure drops, the hydrogen solenoid will be automatically turned off, and the

LED will turn red, indicating that no power is applied.

Ready System Status LED: Indicates that the system is ready for use.

13. Mass Flow Controller Adjustments: The flow controllers are located behind the

front access door and can only be adjusted with a small screwdriver. To adjust

the flow controllers, insert the screwdriver into the slotted adjustment. Turning

clockwise will increase the flow and counterclockwise will decrease the flow.

14. High Voltage Power Supply (HVPS) Adjustments: The HVPS can only be

adjusted with a small screwdriver. To adjust the HVPS, insert the screwdriver

into the slotted adjustment for the correct detector, DET A is sulfur and DET B

is nitrogen. Turning clockwise will increase the voltage and counterclockwise

will decrease the voltage supplied to the PMT.

5.2 Rear panel

The following is a brief explanation of the function and operation of the rear panel controls and

connections of the PAC 7090 system. These controls and connections are primarily used for the

manipulation of gases, electrical power, external control cables, and signal distribution.

Most electrical and electronic connections are made from the rear panel of the 7090 system.

Connectors are present for Main Power, Remote Auto Zero, Detector Output Connections, and

Pyro Furnace and Thermocouple Control. Also included on the rear panel are the cooling fan,

vent, and fuses. Some electronic connections may be located on peripheral equipment. Refer to

Figure 5-3 for location of the major components on the rear panel.

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Figure 5-3 Rear panel

1. Furnace Thermocouple Connector: Interface connector between the 7090 system and the Furnace

Assembly Thermocouple.

2. Cooling Fan: This fan provides for removal of excess heat from the 7090 system.

3. Furnace Power Connector: Interface connector between the 7090 system and the Furnace

Assembly

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4. Scrubber Tube Assembly: The Scrubber Tube contains a catalyst for the complete elimination of

ozone prior to the vacuum pump. Do NOT attempt to operate the system without a Scrubber

Tube.

5. Detector Output Connections: Interface connectors for analog outputs of detector signals. Signal

levels of 1 millivolt, 1 volt, and 10 volts are available. Each connector is keyed for proper

polarity.

6. Sample Transfer Line: The Sample Transfer Line is a direct connection from the exit of the Furnace to

the Sample In fitting of the Reaction Chamber Assembly.

7. Plumbing Connections: (Refer to Figure 4-4.)

Oxygen Connect 3.0 Bar (40 PSI) oxygen source here.

Hydrogen* Connect 3.0 Bar (40 PSI) hydrogen source here.

Helium* Connect 3.0 Bar (40 PSI) Helium “He” source here.

Hydrogen Out The “H2 Out” line connects directly to the base of the furnace.

Oxygen Out The “O2 Out” is connected via the Oxygen Transfer Line to the

makeup fitting on the Detector Inlet.

*The hydrogen and the helium are only used on the sulfur detector.

Figure 5-4 Fuses

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Fuse Description 115 VAC 230 VAC

1 & 2 Main Fuses (8 amp) (5 amp)

3 Fuse 70 VAC (transformer secondary) furnace voltage

(10 amp) (10 amp)

4 Fuse furnace transformer (8 amp) (5 amp)

5 Fuse 24 VAC (2 amp) (2 amp)

6 Fuse 24 V Transformer (2 amp) (1 amp)

7 Fuse Temperature Controller (1 amp) (1 amp)

8 Fuse 5 VDC Power Supply Ozone Generator (1 amp) (1 amp)

9 Fuse 15 V Power Supply Mass Flow Controllers (1 amp) (1 amp)

10 Fans (1 amp) (1 amp)

11 Detector Trays

(1 amp) (Slow-blo)

(1 amp) (Slow-blo)

NOTE:

The main fuses are located in the fuse drawer situated in the housing of the power

receptacle. Use a small screwdriver to release the latch and the drawer will slide out

easily.

5.3 Internal components

Below is a brief description of the major components and their functions:

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Figure 5-5 Internal Components

1. Signal Processing Board: The PMT signal is manipulated on this board by

selecting proper gains and ranges. The baseline controls are also performed by

this board.

2. Power Distribution Board: These boards contain all the fuses and provide the

main power distribution for the entire system.

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3. Display Board: The Display Board interprets all the conditions of the system

and gives the instrument user a current status at a glance. It contains all the

switches for operation and is located behind the front door access It is also

responsible for the measurement of the vacuum in the reaction chamber and at

the base of the oxidative/reductive furnace.

4. Signal Output Board: This board has the divider network to allow the signal to

be monitored as 10 volts, 1 volt, or 1 mv.

5. Ozone Generator Board: This board provides the circuitry to pulse the

transformer and produce ozone.

6. High Voltage Power Supply Board: This board provides the stable voltage to

operate the photomultiplier tube. This voltage can be monitored on the front

panel.

7. PMT Housings: The photomultiplier tubes are encapsulated here in a light free

environment. This housing should never be opened with voltage applied or

permanent damage to the PMT can occur.

8. Reaction Chamber: This is the mixing chamber for the reaction to occur by

uniformly mixing the ozone and the sample.

9. Hydrogen Solenoid: This solenoid is controlled so that it is energized only

when the furnace has reached the proper operating temperature and O2

pressure is above 30 psig.

10. Transformer: This transformer provides the 24 VAC to operate the HVPS

Board.

11. Transformer: This transformer provides the 70 VAC to operate the furnace.

12. 5V Power Supply: This provides the stable 5 VDC to operate the Ozone

Generator.

13. Ozone Generator: The Ozone Generator converts the oxygen into ozone

required for the detection of sulfur species.

14. Mass Flow Controllers: These control the flow of gases to the furnace and

ozone generator.

15. Temperature Control: This is the control for the furnace.

16. Testpoints, Sulfur (above) & Testpoints, Nitrogen (below): These are the

testpoints for ±15 VDC and 5 volt power supplies.

17. Line filter: reduces noise from random spikes from power source.

18. Nitrogen Thermoelectric Cooler and Fan: keeps PMT cool for nitrogen

detector.

19. 15V Power Supply: This provides the stable 15 VDC to operate the Mass Flow

Controllers.

5.3.1 Vacuum pump

The system requires a stable vacuum pump to operate. The pump must be capable of a vacuum of

25 torr at a flow of 100 ml/min. (See Section 4.3.9) The vacuum pump is connected directly to

the Scrubber Tube exit fitting. Refer to Figure 5-6.

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Figure 5-6 Vacuum pump connection

5.4 Furnace

The following is an explanation of the function and operation of the Furnace Module on the PAC

7090 system. Figure 5-7 illustrates the location of the main features and connections of the

furnace.

Figure 5-7 Furnace

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1. Outer Pyrotube: Ceramic tube for sample oxidation

2. Inner Pyrotube: Ceramic tube for sample reduction

3. Thermocouple: Senses the furnace temperature

4. Furnace Power Cable: Supplies power to the heater element

5. Furnace Shield: Insulates the Furnace Assembly

6. Base Assembly: Mounts to the GC and connects the GC column to the furnace

7. Oxygen Transfer Tube (Sulfur Only): Supplies oxygen and helium to the

detector base of the furnace

8. Hydrogen Inlet Tee: Supplies hydrogen to the inlet

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6. PRIMARY TESTS

6.1 Pressure Tests

The gas flows for the PAC 7090 system will generally depend on the GC column(s), sensitivity

desired, and the specific application.

CAUTION:

To prevent system damage, all system components and accessories should

be properly installed and carefully checked for leaks before final gas flow

adjustments are made and the capillary column is installed. The gas supplies

should be connected as outlined in Section 4.3.1 of this manual.

Each gas line must be a dedicated line or have an independent valve to turn off gases when the

system is not in use. A pressure gauge installed after the valve will enhance the ability to properly

perform a leak test of the system.

6.1.1 Gas supply (External) leak check

1. Power off 7090 and turn off helium supply.

2. Turn on all other supply gases and set pressure to 3.0 bar (40 psi).

NOTE:

The H2 flow will display 00 until the instrument is fully installed. Record this setting

in Chapter 7.

Table 6.1

Factory Settings

Main Fuses

Oxygen Flow controller

Fuse furnace transformer

Hydrogen Flow controller

Fuse 24 VAC

Ozone Flow controller

Helium Makeup

CAUTION:

Do not over tighten shut-off valve. Turn counterclockwise only until resistance

is felt. Over tightening may damage the flow control devices.

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3. Turn off each gas at the valve located prior to the system and monitor the

pressure gauge. No noticeable pressure drop should be observed within five

minutes. If leak(s) are present, they are located prior to the system’s flow

controllers and are more than likely located in the manifolds providing gases

to the analyzer. Locate the leaks by testing each fitting with a liquid leak

detector such as SnoopTM

. Tighten the leaking fittings only enough to stop the

leak. Over tightening will damage the ferrule and fitting. Do not attempt to

operate the system or the gas lines until the leak(s) are located and

eliminated.

CAUTION:

When using a liquid leak detector care should be taken not to wet any electrical

or electronic components. Severe component damage may occur.

6.1.2 Vacuum internal leak check

1. Open supply gas valves and set regulators for 40 psi.

2. Perform a leak check of the external supply gases as described in the

previous section.

3. Ensure that there is a capillary plug fitting as shown in Figure 6-3.

4. Ensure that all plumbing connections are properly installed as described in

Section 4.3.

5. Ensure that the 7090 system is plugged into the proper power supply

(115 VAC or 230 VAC).

6. On the rear panel, turn on the Main Power.

7. Turn off ozone switch(es). Use the display select to scroll to O2 and O3 flows

and set flows to 0.

8. Turn on Helium supply.

9. On the front panel, use the display select to scroll to the FURN VAC display.

10. Ensure that the furnace temperature control is set to 25°C as described in

Section 6.3.3 so that the furnace will not heat until a proper leak check has

been performed.

11. Turn vacuum pump power on.

12. Watch the FURN VAC display to ensure that the displayed value is dropping.

CAUTION:

Do not use any liquid leak detection fluids while under vacuum.

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13. If there are no leaks, the FURN VAC and DET VAC values will read a Torr

value of less than 20. Record the value in Table 6.2 below. Record the DET

VAC value in Table 6.2. If there are no leaks, turn off vacuum and proceed to

Section 6.1.3.

Table 6.2

FURN VAC, torr _______________________

DET VAC, torr _______________________

14. If the values do not drop below 20, there is a leak that must be located prior to

operating the system or applying heat to the furnace.

15. If a leak is present, you may need to perform a more in depth leak check using

pressure to isolate the location of the leak.

16. The likely places for leaks are a break in the 1/ 4" ceramic pyrotube or the

Teflon detector sample inlet line. Carefully check these places first.

NOTE:

Internal vacuum sensors (U4 and U6) should be calibrated yearly to ensure optimal

performance.

6.1.3 7090 pressure leak check procedure

Pressure leak check preparation: Turn off ozone power, HVPS, and H2 and Helium flows. Set

furnace temperature to 0°C. Once furnace is below 200°C, turn off vacuum pump and allow

furnace vacuum reading to reach ambient pressure.

6.1.3.1 Total 7090 System leak check

1. Lower Oxygen pressure supply to 5-10 psi.

2. Adjust O2 and O3 flows to 25 ml/min.

3. Remove capillary column from base adapter and plug adapter input with the

blanking nut and ferrule provided in adapter kits.

4. Remove 1/4" Teflon line from exit of scrubber mounted at rear of 7090 and

plug the scrubber exit with 1/4" Swagelok plug.

5. Monitor both ozone and oxygen flows for several minutes.

a. If both oxygen and ozone flow readings drop to 0.0; the system has

passed the pressure leak check. Remove plugs, raise O2 pressure back to

normal (40 psi) and install column to base adapter.

b. If either oxygen or ozone flows do not drop to 0.0; a leak is present and

must be repaired. If the location of the leak is not known, use the

following section “Leak checking isolated components” to pinpoint the

leak.

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6.1.3.2 Pressure leak checking isolated components

This section will help locate a leak. Once the leak is repaired, go back to Section 6.1.3.1 and

verify that the total system is leak free.

A. Leak checking the furnace:

1. Remove 1/8" Teflon line from furnace exit and plug furnace exit with an 1/8"

Swagelok plug.

2. Monitor only the oxygen flow reading:

*If oxygen flow drops to 0.0; the furnace and connected lines are leak free. Go to step 3.

*If oxygen flow does not drop to 0.0; the leak is present at furnace or connecting lines. Reading

the oxygen flow will also indicate the size of the leak(s) you are looking for. After fixing a

furnace leak, proceed to step 3.

3. Remove plug from furnace sample vent and reconnect Teflon line back to

furnace sample vent.

B. Leak checking ozone assembly:

1. Disconnect union in Teflon line between ozone assembly and reaction

chamber.

2. Install 1/8" Swagelok plug on downstream side of union.

3. Watch for ozone flow reading.

* If ozone flow drops to 0.0, ozone assy. is leak free, go to step 4.

* If ozone flow does not drop to 0.0, leak is present in ozone generator assy.

or line to the assembly. After fixing leak, go to step 4.

4. Remove plug from union and reconnect ozone line to reaction chamber line.

C. Leak checking reaction chamber:

1. Ensure the PMT HVPS is switched off!

2. Remove 1/4" Teflon exit line from reaction chamber. Plug the exit fitting of

reaction chamber with 1/4" Swagelok plug.

3. Monitor the oxygen and ozone flow readings.

* If both flows drop to 0.0, reaction chamber, furnace and ozone assemblies are

leak free, go to step 4.

* If either flow does not drop to 0.0, leak is present in reaction chamber or

Tygon® line to detector vacuum sensor. Fix leak and go to step 4.

4. Remove 1/4 " plug from reaction chamber and reconnect 1/4" line to scrubber.

5. Leak check complete system again as in Section 6.1.3.

6. If a leak is still present, inspect the scrubber tube assembly. Tighten or reseal

the scrubber tube and check complete system again.

7. Lower oxygen pressure supply to 5-10 psi.

8. Remove capillary column from base adapter and plug adapter input with the

blanking nut and ferrule provided in adapter kit.

9. Remove 1/4" line from exit of scrubber mounted at the rear of the 7090 and

plug the scrubber exit with 1/4" Swagelok plug.

10. Monitor both ozone and oxygen flows.

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6.1.3.3 Capillary column installation

1. Remove the capillary plug.

2. Ensure that the proper flow is set on the capillary column.

NOTE:

The procedure is only necessary for fused silica columns.

3. Insert the capillary column 15 cm into the furnace. The distance is measured

from the tip of the column to the back of the nut.

6.1.4 Resetting system to factory defaults

1. Referring to Table 6.1, reset the Mass Flow Controllers on O2, H2, and O3 to

factory defaults.

NOTE:

H2 will not show any flow until the system is fully operational.

6.2 GC Power-up

Refer to your gas chromatograph manual and perform any diagnostic tests as required by the

manufacturer prior to the operation of the gas chromatographic system. Upon completion of these

tests, ensure that all gas chromatograph carrier gas flows are set, and that there is flow through

the capillary column without any leaks. Heat the capillary injector and the column oven to the

proper temperature. Refer to the column manufacturer's guidelines to establish the proper

temperatures. Heat the 7090 detector base to 280ºC.

6.3 Model 7090 Power-up

6.3.1 Check list

( ) Proper operating voltage determined? (Section 4.1.1)

( ) System located properly? (Section 4.1.2)

( ) Accessories (if any) installed?

( ) Gas line(s) installed? (Section 4.3.1)

( ) Pyrotubes and furnace installed properly? (Section 4.3)

( ) Leak check OK? (Section 6.1)

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( ) All power switches OFF?

( ) Electrical/electronic interconnections correct? (Section 4.3.6)

( ) Power cord plugged into power source? (Section 4.1.1)

( ) GC flows are set and flowing? (Section 6.2)

( ) Vacuum pump connected and turned OFF?

( ) Hydrogen Valve OFF (Section 2)?

( ) Oxygen Valve OFF (Section 2)?

( ) Mass flow controllers returned to their original settings? (Section 6.1.4)

( ) All blanks filled in the prior sections of this manual? (Tables 6.1, 6.2)

CAUTION:

Become familiar with the location and use of all controls, indicators,

connections, and accessories, and carefully read all instructions before

attempting to operate any portion of the system.

6.3.2 Power-up and functional tests

Ensure that all physical setup procedures as outlined in Section 6.1 have been completed before

continuing with power-up and functional test sequence. Failure to do so may result in serious

damage to system components.

CAUTION:

Ensure that the system and all optional equipment and accessories are

connected to a power source of the correct voltage and wattage. Attaching

any portion of the system to an improper or inadequate power source may

cause severe damage.

Ensure that all power switches on the front panel are in the OFF position. Refer to Figure 5-1 for

locations of the switches on the basic system.

1. Turn the system Main Power Switch to the ON position. There should be an

audible sound of the circulation and cooling fans turning on. Upon power-up,

the Temperature Controller should start flashing the furnace temperature and

will alternately flash Alarm. This is due to the fact that the hydrogen solenoid

has not been energized and that the furnace is at a temperature below 920 °C.

2. Only the O2 Status LED should all be lit at this time. It should be red.

3. Turn on the Oxygen Supply Valve. The O2 LED should turn green. All others

should be red.

4. Turn on the Vacuum Pump. As the proper vacuum is obtained, the furnace vac

LED will fade from red to green if there are no leaks present and the flows are

properly adjusted.

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6.3.3 Furnace power-up

NOTE:

The furnace will not heat unless the FURN VAC and O2 LEDs are green.

Increase the furnace temperature to 950 °C by pressing the (*) key and simultaneously pressing

the up () arrow. The longer the up () arrow is pressed, the faster the number will increase. If

the value of 950 is missed, use the down () arrow and the (*) to reduce the set temperature. The

furnace is an isothermal control zone and is a standard feature with all 7090 systems. The primary

function of the furnace is to completely and quantitatively oxidize and reduce the sample. This

complete oxidation/reduction can only be successfully accomplished at very high temperatures.

The temperature range of the furnace is adjustable from ambient to 1100°C in 1°C increments.

NOTE:

As the furnace temperature increases past 925ºC, the hydrogen solenoid will

automatically be energized and the H2 LED will turn green. The Temp LED

will also turn green at this temperature.

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Figure 6-1 Nitrogen only system

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Figure 6-2 Sulfur only system

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Figure 6-3 Simultaneous nitrogen/sulfur system

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7. START-UP BASICS

1. Ensure that all status lights except for O3 are green and that all temperatures are correct

and stable.

2. Ensure that the Signal Output Cable is installed as described in Section 4.3.6.

3. Press the Auto Zero button on the front panel.

4. Record the mass flow controller settings in Table 6.1.

7.1 Baseline adjustments

1. Select SIGNAL on the LED display.

2. Turn on the integrator or other recording device to plot the baseline.

3. The baseline should be relatively close to 0.0 mV.

NOTE:

A different baseline can be established by manually zeroing the baseline with the

Manual Zero Switch located on the front panel of the 7090NS.

4. Select high gain.

5. Select a sensitivity setting of x10.

7.2 High voltage

1. Select H.V. on LED display. The H.V. display should read relatively close to 0.

2. Turn the High Voltage Switch to the ON position. The H.V. display should read 700 or

more.

3. Select Signal on the LED display.

4. Monitor the baseline to ensure that there is a shift (positive) in the baseline.

5. Press the Auto Zero button on the front panel.

7.3 Ozone generator

6. Record Signal on 7090NS front panel display in Table 7.1.

7. Turn the Ozone Generator Switch to the ON position. (The O3 LED should turn green.)

8. Monitor the baseline to measure any shifts in the baseline. Allow at least 15 minutes for

the ozone generator and analytical system to stabilize.

9. Record Signal on 7090NS front panel display in Table 7.1.

TABLE 7.1

Signal with O3 off _______________________________________

Signal with O3 on _______________________________________

10. Press the Auto Zero button on the front panel.

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Left Blank

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8. APPLICATIONS AND ANALYTICAL PROCEDURES

8.1 Important basics

This section describes the general operation of the PAC 7090NS system. Included in this section

is information on controls, connections, functional tests, troubleshooting and other basic

operating parameters. For detailed information on the function and operation of specific controls

or modules, refer to the applicable section (s) of, or addenda to, this manual. Since the PAC

7090NS system is capable of analyzing a wide variety of materials for sulfur content, the

analytical parameters may vary. The operation conditions given in this section are general and

should be used only as guidelines.

CAUTION:

Do not attempt to operate the 7090NS system until all installation and setup

procedures outlined in this manual have been successfully completed.

Figure 8-1 PAC 7090NS system

8.1.1 Gas and carrier flows

Most gas flow adjustments are performed and monitored on the front panel of the 7090NS. Mass

flow controllers are provided for Pyrolysis Oxygen, Ozone Oxygen, and Hydrogen. Some flow

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adjustments will be located on the GC to which the 7090NS system is attached. For detailed

information concerning these flow controls, please refer to the GC manual. Refer to Section 5.1

for location of the major components of the front panel of the 7090NS.

NOTE:

For more detailed information on the specific function(s) and operation of the

front panel controls, refer to Section 5.1.

NOTE:

Please refer to the 7090NS TEST Conditions Sheet for your instrument flows.

These are typical starting flows for a 7090NS system. The 7090NS system is factory calibrated

with thiophene in toluene and/or indole in toluene check standards. The actual mass flow

controller settings of your system are recorded in the attached 7090NS Test Conditions Sheet.

Please refer to this sheet as a starting point.

TABLE 8.1

Gas MFC Setting

Ozone Oxygen 25 mL/min.

Pyro Oxygen 8 mL/min.

Hydrogen 250 mL/min.

Oxygen Flow Measurement

Measure the oxygen without any power to the furnace. The flow is measured at the Oxygen Out

on the rear panel (refer to Figure 5.3).

Hydrogen Flow Measurement

The instrument must be turned on and ready for operation to be able to measure the hydrogen.

The oxygen must be at 30 psi minimum, the P1 torr value below 250, and the furnace above

750°C for the hydrogen solenoid to be energized. The flow is measured at the Hydrogen Out on

the rear panel.

Chromatographic Column Flow Measurements

Refer to the manufacturer’s Column Information Sheet for optimum conditions and optimum

column operating parameters.

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8.1.1 System flow considerations

Operating the 7090NS system with excess flows can reduce the ability of the pump to maintain

adequate pressure, and therefore, analytical results may vary. In a normally operating system, the

system flow considerations are as follows:

Furnace Temp = 950ºC (Top – Displayed)

= 1050ºC (Bottom – Not Displayed)

O2 Flow = 4 to 12 mL/min

H2 Flow = 110 to 350 mL/min

He Flow = 90 to 150 mL/min

O3 Flow = 20 to 90 mL/min

P1 Furnace Pressure = 80 to 350 torr

P2 Detector Pressure = 8 to 40 torr

Column Flow = 1 to 25 mL/min

Capillary Column = 0.100 to 0.530 mm

Figure 8-2 Normal operating system

8.1.2 System gas flow adjustments

The 7090NS system requires oxygen and hydrogen, (for sulfur mode only), to operate properly.

Oxygen is used in the oxidation step of the pyroreactor, and hydrogen is used in the reduction

step of the pyroreactor. See Section 3.2, equations (1) and (2) for reactions.

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8.2 Optimizing sulfur detection

1. Ensure that all flows are set according to factory preset. Refer to Section 8.1.1

for details.

2. Inject the check standards shipped with the instrument. (500 - 1000 ppb S as

thiophene in toluene)

3. When the instrument is optimized, the chromatogram will be comparable to the

one found in the 7090NS Test Conditions package.

The system flows may need adjusting when first received from the factory or when installing new

ceramic pyrotubes. The chromatograms in Figure 8-3 are general guidelines on what to expect

when adjusting the hydrogen and oxygen flows for sulfur analysis.

Figure 8-3 Chromatograms

Figure 8-3a Figure 8-3b Figure 8-3c Figure 8-3d

Flows set correctly H2 Flows – Too Low H2 Flows – Too High 02 Flows – Too Low

Use these chromatograms and the flowcharts on the following pages to optimize your system for

sulfur detection. See Section 8.3 to optimize your system for nitrogen.

To optimize for sulfur detection, use the following flow charts to determine the course of action.

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Figure 8.3a Figure 8.3b Figure 8.3c Figure 8.3d

Record all mass flow controller Settings in Table 6.1

See Page 58-59

See Page 57

See

Page 59

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Figure 8.3a Figure 8.3b Figure 8.3c Figure 8.3d

Return to “Instrument Ready”

Page 60

See Page 56

See Page 58-59

See Page 59

Figure 8.3b

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Return to “Instrument Ready”

Page 60

Figure 8.3a Figure 8.3b Figure 8.3c Figure 8.3d

Return to “Start Here” Page 6059

Return to “Figure 8-3b”

Return to “Figure 8-3d”

See Page 57

See Page 56

See Page 59

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Figure 8.3a Figure 8.3b Figure 8.3c Figure 8.3d

Return to “Start Here” Page 6059

Return to “Figure 8-3b”

Return to “Figure 8-3b”

Return to “Instrument Ready”

Page 60

See Page 56

See Page 57

See Page 58

Section 4.3

Section 9.5

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8.3 Optimizing nitrogen detection

Use the chromatograms in the Figures on the next page and the flowchart following to optimize

your system for nitrogen detection.

Figure 8-4 Optimizing flows

Figure 8-4a Figrue 8-4b

Flows set correctly Oxygen flow set too low

Record all mass flow controller Settings in Table 6.1

Figure 8.4a Figure 8.4b

See

Page 62

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Return to “Instrument Ready”

Page 64

Figure 8.4b Figure 8.4a

Return to “Instrument Ready”

Page 64

See

Page 56

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9. SERVICE INFORMATION

9.1 Furnace temperature controller programming procedure

9.1.1 Initial power up

Action Controller Display

Turn instrument on

Initial message upon power up will flash alternatively between “inPt”

and “none”. The controller is requesting the type of thermocouple that will

be used.

To Set Thermocouple Type

To set the thermocouple type. Press and hold the * and then press the

button 4 times for the type K thermocouple. To accept the value, release

the *.

To advance to the next question press the button once.

To Select Celsius or Fahrenheit

The controller message will now flash alternatively between “unit” and

“none”. The controller is requesting the type of temperature display

preferred.

To set the temperature display: Press and hold the * and then press the

button once until the display shows oC. To accept the value, release the *.

To advance to the next question press the button 1 time.

Select Furnace Relay The controller message will now flash alternatively between “SP 1 .d” and

“none”. The controller is requesting the type of relay that is required.

To set the relay type. Press and hold the * and then press the - button 2 times

until the display for the relay type is SSd. To accept the value, release the *.

NOTE:

When the controller is initially turned on, it automatically enters programming

diagnostics at level 5 and requires the three questions listed above to be

answered before continuing with the other programming steps. To return to

different levels at any time, press the button repeatedly until the controller

message flashes alternatively between “level” and “5” or the existing level.

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Action Controller Display

The next questions are on level 2. To go to level 2, press the button 3 times

until the controller display flashes alternatively between “level” and “5”.

The controller will then be at the beginning of the level 5 programming.

To change levels, press and hold the * and then press the button 3 times

until the controller message flashes alternatively between “level” and “2”.

To accept the value, release the *.

Select Alarm Parameters

Note:

For Sulfur Detectors only, although it is always programmed

on both nitrogen and sulfur. This gives an “AL” display to

indicate a temperature lower than the setpoint.

To set the alarm type for the Hydrogen Solenoid, press the button 5 times

until the controller message flashes alternatively between “SP2.A” and

“none”.

To set the alarm output type, press and hold the * and then press the

button 5 times until the controller message display is “FS.Lo”. To accept the

value, release the *.

Set Furnace Power Limit %

To set the upper limit of the furnace, press the button 2 times and the

controller message display will flash alternatively between “PL. 1” and

“100”. Hold the * and press the button until the controller display

flashes alternatively between “PL. 1” and “85”.

The PL. 1 value should be set at a value low enough to heat slowly, yet reach

the desired temperature. A value too low will not reach temperature and a

value too high will heat very quickly which in some cases reduces the

overall life of the furnace. The 7090 will typically use a value of 85.

Set Furnace Upper Limit

To set the upper limit of the furnace, press the button 5 times and the

controller message display will flash alternatively between “hi.SC” and

“1200”.

To change the upper limit set point, press and hold the * and use the á button

or the button to adjust the setpoint value either up or down and adjust the

setpoint value to 950. To accept the value, release the or the and then

release the *.

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Action Controller Display

The next questions are on level 1.

To change to level 1, press and hold the * and then press the button 8 times until the

controller message flashes alternatively between “level” and “1 ”. To accept the

value, release the *.

Set the Cycle Time of the Furnace

Press the button 6 times until the controller message flashes alternatively between

“CyC.t” and “20”.

Press and hold the * and then press the button or the button to adjust for an

initial cycle time of 4.0. To accept the value, release the *.

Adjust the Hydrogen Solenoid Setpoint Temperature

Press the button 3 times until the controller message flashes alternatively between

“SEt.2” and “0”.

Press and hold the * and then press the button or the button to adjust for a

setting of 925 degrees. To accept the value, release the *.

To accept the parameters go to normal operation, simultaneously press the button

and the * button and hold them pressed until the display reads “PArk”.

9.1.2 Temperature Set Procedure

To set the furnace temperature, press and hold the * and use the button or the *

button to increase or decrease the desired temperature value. Release the * to accept the

setpoint value.

9.1.3 Auto Tune Procedure

To eliminate overshoots or undershoots at the setpoint value, it may be necessary to

autotune the controller. Ensure that the controller is at the approximate operating

temperature.

Press and hold the ⟨ button and the button for approximately 5 seconds or until the

display flashes between “tunE” and “oFF”.

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Action Controller Display

Press and hold the * and press the 'f' button 3 times until the display reads “At.SP”.

To accept the value, release the *.

Press and hold the 'f' button and the 'f' button for approximately 5 seconds or

until the display flashes between “tunE” and “At.SP” and “1000” or the

actual temperature of the furnace. This will take about 5 minutes to calculate

the “Cycle Time Value” and there will be a light in the upper left hand corner

of the display that will blink during the Autotune procedure.

At the end of the Autotune procedure the user must enter the calculated

value of the cycle time.

Press and hold the 'f' button and the â button for approximately 5 seconds or

until the display flashes between “tunE” and “oFF”.

Press the 'f' button 5 times until the display reads “CyC.t”.

Press and hold the * and press and hold the 1' button until the display does not

change any more and the display reads “A —” or the calculated value. If the

display reads “A 3.8”, then 3.8 is the optimum value. To accept the value, release

the 1' button and then release the *.

Press and hold the á button and the 1' button for approximately 5 seconds or

until the display flashes the actual furnace temperature.

The furnace should now stop at the desired temperature.

To Reset all Default Conditions

Simultaneously press the 'f' button and the 1' button and hold them pressed

until the display reads “tunE”.

Press the 1' button 1 time and the display will flash alternatively “LEVL” and

“1”.

The reset function is on level 3.

To change levels, press and hold the * and then press the 'f' button 2 times until

the controller message flashes alternatively between “level” and “3”. To

accept the value, release the *.

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Action Controller Display

Press the '1 button 12 times until the display flashes alternatively between

“reset” and “none”.

Press and hold the * and then press the '1 button 1 time until the controller

message display is “ALL” . To accept the value, release the *.

Simultaneously press the '1 button and the È button and hold them pressed until

the display flashes alternatively between “inPt” and “none”. The controller is now

ready to be reprogrammed.

9.2 Thermal Electric Cooler (TEC) Temperature Controller Programming Procedure

9.2.1 Initial Power up

Action Controller Display

Turn instrument on.

Initial message upon power up will flash alternatively between “inPt” and “none”. The

controller is requesting the type of thermocouple that will be used.

Set Thermocouple Type

To set the thermocouple type. Press and hold the * and then press the '1 button 10

times until the display is for the type RTD thermocouple. To accept the value,

release the *.

To advance to the next question press the '1 button 1 time.

To Select Celsius or Fahrenheit

The controller message will now flash alternatively between “unit” and “none”. The

controller is requesting the type of temperature display preferred.

To set the temperature display: Press and hold the * and then press the '1 button 1 time

until the display is oC. To accept the value, release the *.

To advance to the next question press the '1 button 1 time.

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Action Controller Display

Select Thermal Electric Cooler Relay The controller message will now flash alternatively between “SP 1 .d” and “none”.

The controller is requesting the type of relay that is required.

To set the relay type. Press and hold the * and then press the '1 button 2 times

until the display for the relay type is SSd. To accept the value, release the *.

NOTE:

When the controller is initially turned on, it automatically enters the

programming diagnostics at level 5 and requires the three questions listed

above to be answered before continuing with the other programming

steps to return to different levels at any time press the 1' button

repeatedly until the controller message flashes alternatively between “level”

and “5” or the existing level.

The next questions are on level 3. To go to level 3, press the button 3 times until the

controller display flashes alternatively between “level” and “5”. The controller will

then be at the beginning of the level 5 programming. To change levels, press and hold

the * and then press the 1' button 2 times until the controller message flashes

alternatively between “level” and “3”. To accept the value, release the *.

Select Reverse Mode

To set the relay to react opposite when firing the relay for the thermal electric

cooler, press the '1button 4 times until the display flashes alternatively between

“rEV.d” and “none”.

Press the * and the '1until the display is “1D.2R” Release the * and press the 1' 4 times

until the display flashes alternatively between “level” and “3”.

The next questions are on level 2. The controller is now at the beginning of the

level 3 programming. To change levels, press and hold the * and then press the â

button 1 time until the controller message flashes alternatively between “level” and

“2”. To accept the value, release the *.

Select Alarm Parameters

To set the alarm type for the Hydrogen Solenoid, press the '1 button 5 times until the

controller message flashes alternatively between “SP2.A” and “none”. To set the

alarm output type, press and hold the * and then press the '1 button 5 times until the

controller message display is “FS.Lo”. To accept the value, release the *.

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Action Controller Display

Set Thermal Electric Cooler Upper Limit

To set the upper limit of the thermal electric cooler, press the '1 button 3

times and the controller message display will flash alternatively between “hi.SC”

and “1200”.

To change the upper limit set point, press and hold the * and use the '1 button or the

1' button to adjust the setpoint value either up or down and adjust the setpoint value to

35. To accept the value, release the '1 or the 1' and then release the *.

Set Thermal Electric Cooler Lower Limit

To set the lower limit of the thermal electric cooler, press the '1 button 1 time

and the controller message will flash alternatively between “lo.SC” and “32”.

To change the lower limit set point, press and hold the * and then press and hold

the '1 button or the 1' button to scroll the setpoint value either up or down until the

setpoint value is -20. To accept the value, release the 1' button and then release the

*.

The next questions are on level 1.

To go to level 1, press the '1 button repeatedly until the controller display flashes

alternatively between “level” and “2”. The controller will then be at the beginning

of the level 2 programming. To change to level 1, press and hold the * and then press

the 1' button 1 time until the controller message flashes alternatively between “level”

and “1”. To accept the value, release the *.

Set the Cycle Time of the Thermal Electric Cooler

Press the '1 button 6 times until the controller message flashes alternatively between

“CyC.t” and “20”.

Press and hold the * and then press the '1 button or the 1' button to adjust for a initial

cycle time of 4.0.

To accept the parameters go to normal operation, simultaneously press the '1 button

and the 1' button and hold them pressed until the display reads “PArk”.

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9.2.2 Temperature Set Procedure (see following text)

To set the thermal electric cooler temperature, press and hold the * and use the '1 button or the 1' button to increase or decrease the desired temperature value. Release the * to accept the setpoint value.

Start with a setting of 4.

Action Controller Display

9.2.3 Auto Tune Procedure

To eliminate overshoots or undershoots at the setpoint value, the user may

need to autotune the controller. Ensure that the controller is at the

approximate operating temperature.

Press and hold the 'f' button and the 1' button for approximately 5 seconds or

until the display flashes between “tunE” and “oFF”.

Press and hold the * and press the 'f' button 3 times until the display reads “At.SP”.

Press and hold the 'f'button and the 1' button for approximately 5 seconds or until

the display flashes between “tunE” and “At.SP” and “5” or the actual

temperature of the thermal electric cooler. This will take about 5 minutes to

calculate the “Cycle Time Value” and there will be a light in the upper left hand

corner of the display that will blink during the Autotune procedure.

At the end of the Autotune procedure the user needs to enter the calculated

value of the cycle time.

Press and hold the 'f' button and the 1' button for approximately 5 seconds or

until the display flashes between “tunE” and “oFF”.

Press the 'f' button 5 times until the display reads “CyC.t”.

Press and hold the * and press and hold the âbutton until the display does not

change any more and the display reads “A —” or the calculated value. If the

display reads “A 3.8”, then 3.8 is the optimum value. To accept the value,

release the 1' button and then release the *.

Press and hold the 'f' button and the 1'button for approximately 5 seconds or until

the display flashes the actual thermal electric cooler temperature.

The thermal electric cooler should now rest at the desired temperature.

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Action Controller Display

To reset all default conditions

Simultaneously press the á button and the 1' button until the display reads

“tunE”.

Press the 1' button 1 time and the display will flash alternatively “LEVL” and

“1”.

The reset function is on level 3.

To change levels, press and hold the * and then press the Ç button 2 times until the

controller message flashes alternatively between “level” and “3”. To accept the

value, release the *.

Press the Ç button 12 times until the display flashes alternatively between

“reset” and “none”.

Press and hold the * and then press the Ç button 1 time until the controller

message display is “ALL” . To accept the value, release the *.

Simultaneously press the Ç button and the 1' button until the display flashes

alternatively between “inPt” and “none”. The controller is now ready to be

reprogrammed.

9.3 Board Alignment Procedures

See following page.

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9.3.1 Printed Circuit Boards Overview

The following is a list of printed circuit boards (PCB) in the Model 7090 with a brief

explanation of their functions.

1. 103603 —Ozone Generator: This board provides the firing for the ozone

generator transformer firing. (Refer to Section 9.3.2 for adjustment

procedures.)

2. 58137—Signal Pre-amp: This board is located within the photomultiplier

housing assembly. The photomultiplier tube (PMT) connects to this board and

the voltage to the photomultiplier tube (PMT) is distributed here. (No

adjustment required.)

3. 58141—Signal Processor: This board receives the signal from the Signal Pre-

amp board. The gain, sensitivity settings, and autozero are selected on this

board. The signal level is also driven from this board. (Refer to Section 9.3.3

for adjustment procedures.)

4. 58160—High Voltage Power Supply: This board provides the voltage to the

Signal Pre-amp PCB and ultimately to the PMT. The 0–5 vdc voltage that

controls the actual setpoint is received from the 7090 Display Select PCB

(58183). (Refer to Section 9.3.4 for adjustment procedures.)

5. 58167—Detector Interconnect: This board is the main distribution of the power

within the detector tray(s). The 58141 Signal Processor PCB (58141) and the

High Voltage Power Supply PCB (58160) both plug directly to this board. The

gain, autozero, and the sensitivity selection switches are located on this board

and are distributed accordingly. (No adjustment required.)

6. 58183—7090 Display Select: This board controls the selection of all available

displays other than those controlled at the detector tray(s) and provides status

lights for instrument parameters such as flows and vacuum levels. Control

parameters for all Mass Flow Controllers and high voltage to the High Voltage

Power Supply board (58160). (Refer to Section 9.3.5 for adjustment

procedures.)

7. 58185—7090 Signal Output: The output board is located on the rear panel of

the instrument and is the location for connecting the signal level outputs to

chart recorders or integrators. (No adjustment required.)

8. 58186—7090 Power Distribution: The power distribution controls the

distribution of all power to the analyzer. The power to the detector trays and all

power supplies and transformers are located on this board. The instrument

fuses are located on this PCB and can be easily accessed from the rear of the

instrument. (No adjustment required.)

9. 58193—Mass Flow Controller: The mass flow controllers are all connected

with this common board. It provides the + 15 VDC power requirement as well

as the control voltage and mass flow read to the 7090 Display Select PCB (58

183). (No adjustment required.)

10. 58210 —H2 Control LED Status: This board contains the LEDs that indicate

the switch position of the 7090 Display Select PCB (58183). (No adjustment

required.)

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CAUTION:

High voltages are present during operation of the ozone generator. Ensure that

safe work conditions are established and used.

NOTE:

The Ozone Generator board cannot be properly adjusted unless installed with a

working ozone cell.

NOTE:

The ozone circuit will not work if the pressure is not 30 psi. Also, the pressure sensor

will not disengage until pressure drops below 28.5 psi.

9.3.2 Ozone Generator Board – p/n 103603

1. Setup Ozone Generator / Ozone PCB test rig, as shown in picture below:

RotometerPN 23098

Pressure regulatorPN 21067

30 psi 25 cc/min

Ozone Generator

Ozone MeterTELEDYNE 454H

Ozone scrubberPN 71137-2

P-3Oxygen

Exhaust

2. Install jumpers to JP4, JP5, and JP6 on Ozone PCB.

3. Connect 5 VDC to the Ozone Generator PCB at location H2 with the Positive 2,

Negative Pin 1.

4. Leave H1 connector on Ozone PCB unconnected.

5. Set up a DMM to measure frequency.

6. Connect the DMM Black lead to TP3 on ozone PCB.

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7. Connect the DMM Red lead to TP6 on ozone PCB.

8. Start flow of Oxygen into Ozone Generator.

9. Apply power to the Ozone Generator.

10. Adjust potentiometer R1 so that DMM shows 120 ± 1Hz.

11. Allow the Ozone generator board to stabilize for 10 minutes.

12. The ozone meter should read between 1.5 and 3 % of ozone.

13. Turn off power and shut down oxygen flow to Ozone Generator.

14. Wait for 1 min for Ozone Generator to power down.

15. Configure the jumpers JP4 and JP6 on the Ozone PCB for the target instrument.

Leave H2 unconnected.

9.3.3 Signal Processing (58141R3 Alignment Procedure)

Figure 9-2 Signal Processing Board

58141 Connector Identification

J1 Remote Zero J10 Signal Out

J2 Auto Zero J11 Span

J3 Manual Zero J12 Scaled Output

J4 Sub-panel Board J13 Zero

J5 Display J14 High/Low

J6 Rear Output Board

(Signal & Auto Zero Combined) J15 PMT Power

J7 PMT Signal In J16 PM 390

J8 4-20 ma Output J17 External 4-20 ma

J9 Sensitivity

1. Place shorting jumper on JP2. (Display Select)

2. Place a shorting jumper on the left two pins of JP6. (Unscaled display)

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3. Place a shorting jumper on the right two pins of J11. (Scale option ON)

4. Place a shorting jumper on the left two pins of J7. (For field adjustment, this

jump must be made or a working PMT pre-amp must be installed )

5. Use a jumper to momentarily short the left side of R74 to the bottom pin of

JP3, JP4, or JP5 (+5 vdc). (Clears Zero register)

6. With a Digital Volt Meter, insert the black meter lead into TP1 (Ground). Insert

the red lead into TP2. Adjust R54 for 0.0 mvdc.

7. Use a jumper to short the left side of R7 to the left side of R21 (analog ground).

8. Remove the 16 pin ribbon cable from J4.

9. Switch S1#1 to the on position (S1#1 up = x50).

10. Move the Red lead to the right side of R3 1, adjust R1 for 0.0 mvdc.

11. Move the Red lead to the left side of R73, adjust R50 for 0.0 mvdc (± 5mvdc).

(Auto Zero Setpoint)

12. Move the jumper on JP6 from the left two pins to the right two pins. (Scaled

Display)

13. Place the Red lead to the bottom of R39, adjust R34 for -0.9 mvdc . (This is the

offset adjustment that allows a full scale output on the model 9000. The

adjustment should allow the raw data after the A/D module to be around 0.100

VDC. If more/less adjustment is required/desired the -0.9 mvdc is subject to

change to get a 0.100 VDC reading.)

14. Move the jumper on JP6 from right two pins to the left two pins. (Unscaled

display)

15. Completely remove the jumper installed in step 3 (left side of R7 to the left

side of R21–analog ground).

16. Move the red lead to the right side of R3 1.

17. Momentarily short the two pins of J1 to autozero the board.

18. If the board is properly adjusted and working, the voltage should stabilize

within 3.0 mvdc of 0.00.

19. Vary the millivolt output by applying a millivolt input or varying the voltage to

the PMT and auto zeroing several times. (This can also be accomplished by

shorting the bottom of JP5 to the left side of R74.)

20. To adjust the front panel display, measure R3 1 and adjust R30 so that the

display value is 100 times the result. e.g: 1.70 volts measured, display should

be 170.

21. To test the sensitivity settings measure R31 input with S1 #1 up and apply the

value to X (100%). e.g: 1.70 volts measured, display should be 170—Panel

display 170.

22. Move the jumper from JP2 to JP1

23. Return all switches to the down position and replace the 16 pin ribbon cable.

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Switch Position R31 Value Display Reading

#1 up only 1.70 VDC 170

#2 up only 0.85 VDC 085

#3 up only 0.34 VDC 034

#4 up only 0.17 VDC 017

9.3.4 High Voltage Power supply voltage (58160) Adjustment

Figure 9-3 High Voltage power supply board

9.3.4.1 Jumper Positions

1. Set JP1 to the Right (for VAC or VDC greater than 15V).

2. Set JP2 to the Right (for 15V or greater AC or DC).

3. Set JP3 to the Right (for 0-5VDC control voltage).

4. Set JP4 to the Left (for external control).

5. Short D3.

9.3.4.2 Board adjustment

1. Apply power to the board and adjust for an output of –600VDC. As the board is

set for external control, supply the control voltage of 3.0VDC that represents

600VDC and adjust P3 for 600VDC at TB1 positions 1 and 2.

2. Adjust P1 for the proper monitor voltage at TP1 and TP2 (ground). For 0-1VDC

monitor output adjust P1 for 0.6VDC.

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NOTE:

For a 0—5 VDC output, TP1 should be 1000=5v, 800=4v, 600=3v…etc. For a 0-1

VDC output, TP1 should be 1000=1v, 800=0.8v, 600=0.6v…etc.

9.3.5 Display Select Adjustment Procedure (58183)

9.3.5.1 Required Test Equipment

1. Digital Volt Ohm Meter

2. Vacuum Pump

3. Calibrated Vacuum Meter

4. 2 Pin Jumpers

5. 58183/58185 Test Fixture or completed instrument

9.3.5.2 Preliminary notes

The front panel lights will not be on unless there is 5 volts present from the pressure sensor.

9.3.5.3 Power Supply Test Points

1. TP3 Common

2. TP2 +15 VDC

3. TP4-15 VDC

4. TP9 +5 VDC

9.3.5.4 Meter adjustment

1. Turn selector knob to the 3rd position (Ozone).

2. Insert black lead into TP3.

3. Measure 5 vdc on pin 2 of JP1.

4. Install a jumper on JP1.

5. Insert the red lead into TP13.

6. Adjust P7 until the front panel display reads 500 (Ignore all decimals if

present).

7 Remove jumper.

9.3.5.5 Oxygen Pressure Sensor

1. Ensure that the Oxygen Pressure sensor light comes on when:

a. O2 is greater than 30 psi.

b. Test fixture O2 Sensor Simulation switch is energized.

c. When JP2 Oxygen Bypass is jumped.

9.3.5.6 Furnace Vacuum Adjustment

1. Turn the selector switch to the Furnace vacuum read. (Position 1).

2. Adjust P2 until display reads 760.

3. Using an approved vacuum sensor, determine the torr reading of a vacuum

pump. For testing purposes, assume 30 torr is the low end vacuum.

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4. Apply known vacuum to the P1 port on the vacuum sensor.

5. Adjust P1 for the torr value determined in step 4.

6. Remove the vacuum and adjust P2 until the display reads 760.

7. Repeat steps 5–7 until no further adjustments are required.

9.3.5.7 Detector Vacuum Adjustment

1. Turn the selector switch to the Furnace vacuum read. (Position 1).

2. Adjust P5 until display reads 760.

3. Using an approved vacuum sensor, determine the torr reading of a vacuum

pump. For testing purposes, assume 30 torr is the low end vacuum.

4. Apply known vacuum to the P1 port on the vacuum sensor.

5. Adjust P4 for the torr value determined in step 4.

6. Remove the vacuum and adjust P5 until the display reads 760. 14. Repeat steps

5-7 until no further adjustments are required. 7.3.5.8

9.3.5.8 Temperature Span Adjustment

1. Apply mv source to thermocouple input on 58186 printed circuit board or heat

the furnace to 950°C.

2. Ensure ribbon cable is properly connected.

3. Insert the black lead into the common (TP3).

4. Insert the red lead into the High setpoint Test Point (TP6).

5. Adjust P15 until the DVM displays 42.0 mvdc.

6. Insert the red lead into the Low Setpoint test point (TP5).

7. Adjust P14 until the DVM displays 36.5 mvdc.

8. Monitor both the Temperature LED and the Cal 3200 display as the mv source

is increased and decreased. Ensure that the LED is green only between the

reported temperature of 900° and 1050°.

9. Monitor the Hydrogen LED and ensure that the LED turns green at the reported

temperature of 925°.

9.3.5.9 Mass Flow Controller Adjustment

1. Measure the voltage at TP17 with the red lead to ensure a stable 10 volt

reference.

2. If there are no mass flow controllers present, use jumpers to temporarily

simulate MFCs by placing jumpers on RC2 pins (9,10 Ozone), (11,12 O2),

(13,14 Hydrogen).

3. On the front panel, turn the display selection switch to the “Ozone” (Position

3).

4. Measure the voltage at TP12 with the red lead.

5. Adjust P9 until the DVM is 2.5 vdc.

6. Ensure that the front panel display meter reads 25.0 (cc/min). Flow must be

present to read correctly.

7. Measure the actual flow to ensure the proper flow from the Mass Flow

Controller.

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8. On the front panel, turn the display selection switch to the “Oxygen” (Position

4).

9. Measure the voltage at TP11 with the red lead.

10. Adjust P10 until the DVM is 1.0 vdc.

12. Ensure that the front panel display meter reads 10.0 (cc/min). Flow must be

present to read correctly.

13. Measure the actual flow to ensure the proper flow from the Mass Flow

Controller.

14. On the front panel, turn the display selection switch to the “Hydrogen”

(Position 5).

15. Measure the voltage at TP18 with the red lead.

16. Adjust P8 until the DVM is 2.5 vdc. (This is the maximum voltage that can be

applied to the Hydrogen controller.)

17. Measure the voltage at TP10 with the red lead.

18. Adjust P11 until the DVM is 1.0 vdc.

19. Ensure that the front panel display meter reads 100 (cc/min). Flow must be

present to read correctly.

20. Measure the actual flow to ensure the proper flow from the Mass Flow

Controller

9.3.5.10 Furnace Vacuum Setpoint Adjustment

1. Turn the selector switch to the Furnace Vacuum Setpoint read. (Position 6).

2. Adjust P3 fully until display reads 250. 7.3.5.1

9.3.5.11 High Voltage Adjustment Channel A

1. Measure the voltage at TP16.

2. Adjust P12 until the voltage reads 5.0 VDC.

3. Measure across J2.

9.3.5.12 High Voltage Adjustment Channel B

1. Measure the voltage at TP 15.

2. Adjust P13 until the voltage reads 5.0 VDC.

3. Measure across J1.

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9.4 Fuse Requirements

Fuse Description 115 VAC 230 VAC

b & c Main Fuse (8 amp) (5 amp)

d Fuse 70 VAC (transformer secondary)

Furnace voltage

(10 amp) (10 amp)

e Fuse Furnace Transformer (8 amp) (5 amp)

f Fuse 24 VAC (2 amp) (2 amp)

g Fuse 24 V Transformer (2 amp) (1 amp)

h Fuse temperature controller (1 amp) (1 amp)

i Fuse 5 VDC Power Supply Ozone Generator (1 amp) (1 amp)

j Fuse 15 V Power Supply Mass Flow controllers (1 amp) (1 amp)

k (1 amp) (1 amp)

l Detector trays (1 amp)

(Slo-blo)

(1 amp)

(Slo-blo)

NOTE:

The main fuses are located in the fuse drawer located in the housing of the power

receptacle. Use a small screwdriver to release the latch and the drawer will easily

slide out.

9.5 Leak Check Procedures

9.5.1 Mass Flow Controller Scaling Procedure and Vacuum Test

1. Connect the “Sample IN” line to the exit of the furnace.

2. Connect the “Hydrogen Out” to the Furnace Base “Hydrogen Inlet”.

3. Connect the “Oxygen Out” to the side arm of the Furnace Inlet Adapter

Assembly.

4. Install a column plug on the bottom arm of the Furnace Inlet Adapter

Assembly.

5. Turn the O3 (ozone), O2 (oxygen to the furnace base), H2 (Hydrogen to the

Furnace base) trimpots 100 % counterclockwise. (OFF)

6. Attach a 50 psi gas oxygen line with a pressure gauge and a toggle valve to the

bulkhead labeled “Oxygen In” on the rear panel.

7. Open the oxygen valve to apply pressure to the analyzer.

8. Turn off the O2 valve, and monitor the pressure to ensure that the O2 pressure

does not drop which would indicate a leak in the supply line or a leaking Mass

Flow Controller (MFC).

9. If there are no leaks, turn the “Display Select” knob to the O3 (Ozone) position.

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10. Attach a digital flow meter to the exit of the scrubber tube vent.

11. The initial reading of the digital flow meter should be 0.

12. Turn the O3 (ozone) adjustment trimpot until the front panel display reads 25.0

the display.

13. The digital flow meter should read 25.0 ±3 %.

14. If the flow is good, turn the “Display Select” knob to the O2 (oxygen to the

furnace base) position.

15. Turn the O2 (oxygen to the furnace base) adjustment trimpot until the front

panel display reads 10.0.

16. The digital flow meter should read 35.0 ±3 %.

17. Turn the O3 (ozone), O2 (oxygen to the furnace base) trimpots 100 %

counterclockwise. (OFF)

18. Disconnect the digital flowmeter from the scrubber vent.

19. Disconnect the furnace heater cable from the rear panel of the Model 7090 to

prevent heating.

20. Attach a known good vacuum to the scrubber vent.

21. Turn the “Display Select” knob to the P1 position.

22. Turn the vacuum pump on and ensure that the display on the front panel

indicates a vacuum less than 035 torr.

23. Attach a 50 psi gas hydrogen line to the bulkhead labeled “Hydrogen In” on the

rear panel.

24. Open the cylinder valve to pressurize the line.

25. Immediately close the cylinder valve and monitor the pressure gauges on the

cylinder. If the pressure drops, this is an indication of a leak in the supply line.

26. If the pressure does not drop, open the cylinder valve and let it remain open.

27. Disconnect the hydrogen out line from the rear of the analyzer and plug the line

with a brass plug.

28. Attach a digital flowmeter to the “Hydrogen Out” bulkhead.

29. On the 58183 printed circuit board, turn the P8 trimpot 100 % clockwise.

(OFF)

30. Trick the Hydrogen Solenoid to “Open” by:

a. Changing the Cal3200 SP1 alarm setting to 0°C or,

b. Using a millivolt source as a thermocouple to indicate 950°C

31. Turn the H2 (hydrogen to the furnace base) trimpots 100 % clockwise. (ON).

32. Increase P8 until the digital flow meter is at 625 cc/min (maximum H2 flow).

33. Turn the H2 (hydrogen to the furnace base) trimpots 100% counterclockwise.

(OFF).

34. Return the Hydrogen Solenoid to normal operation.

35. Disconnect the digital flow meter from the “Hydrogen Out” bulkhead.

36. Reattach the “Hydrogen Out” line to the “Hydrogen Out” bulkhead on the rear

of the analyzer.

37. Turn off the vacuum pump and allow the vacuum to bleed.

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38. Disconnect the column plug from the bottom arm of the Furnace Inlet Adapter

Assembly.

39. Connect the capillary column to the base of the Furnace Inlet Adapter

Assembly.

40. Turn the vacuum pump on.

41. Turn the ozone flow to 25 cc/min.

42. Increase the O2 flow to 10.0 cc/min.

43. The P1 value should be approximately 110 torr.

If a leak is suspected and cannot be found, a pressure test might help localize the leak.

9.5.2 Pressure Test (With Furnace)

Do not pressurize above 10 psi.

1. Adjust the oxygen supply pressure to 10 psi.

2. Plug the bulkhead on the rear panel labeled “Hydrogen Out” and “Hydrogen

In”.

3. Plug the exit of the ozone scrubber tube.

4. Connect the 1/8" “Sample Inlet” to the furnace vent.

5. Connect the furnace base O2 Inlet to the bulkhead on the rear panel labeled

“Oxygen Out”.

6. Turn on the Model 7090.

7. Turn the hydrogen, oxygen and ozone flow adjustments located on the front

panel 100 % fully clockwise (On).

8. Open the toggle valve for the oxygen and pressurize the system.

9. Turn off the toggle valve and ensure that the pressure holds for 3 minutes.

10. If leak cannot be found, bypass the furnace by connect the 1/8" “Sample Inlet”

to the bulkhead on the rear panel labeled “Oxygen Out”.

a. If pressure holds, there is a leak in the furnace.

b. If pressure drops, the leak is in the instrument plumbing and

interconnections.

11. Once there are no leaks, remove plugs.

12. Turn the hydrogen, oxygen and ozone flow adjustments located on the front

panel 100% fully counterclockwise (OFF).

13. Return the oxygen cylinder pressure to 50 psi.

9.6 Start-up & Shutdown Procedures

For optimum performance, the instrument should remain on at all times to maintain stability.

Shutdown the instrument only during maintenance or long periods of inactivity. Recalibration of

instrument is typically required after any shutdown or when normal gas flows are not maintained.

9.6.1 Start-up Procedure

1. Oxygen and helium should be off at the cylinders.

2. Turn on main power switch. O2 status light should be red.

3. Open oxygen cylinder. O2 status light should turn green, all other status lights

should be red. If O2 light is not green, check cylinder pressure.

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4. Turn on vacuum pump. Furnace vacuum should be < 120 torr, and status light

should turn green. Detector vacuum should be < 20 torr. Furnace pressure may

increase with temperature.

5. While furnace heats, check oxygen and ozone flows. They should be at preset

conditions.

6. Hydrogen solenoid should turn on when temperature reaches ~925°C (sulfur

instruments only).

7. Temperature should be set at 950°C. When this is reached temperature status

light should be green. All status lights except for O3 should now be green.

8. Set the detector display for high voltage and turn on the high voltage power

supply. Value should be set at ~750 volts.

9. Set the detector display to sensitivity and press the autozero switch. The

display should approach and remain near 000.

10. Turn on the ozone generator. The display (signal) should increase. At this point

all lights should be green.

11. Allow oxidation period of preferably overnight.

12. Open toggle valve for helium make up flow. P1 pressure will increase 100 to

150 torr. (sulfur instruments only).

13. Slowly bring the hydrogen flow (if sulfur instrument) up until the display reads

the recommended setting. Turn clockwise until display value is reached.

Furnace vacuum should be approximately the predetermined value. Detector

vacuum should be < 30 torr.

9.6.2 Shutdown Procedure

A long-term shutdown is defined as a period of no analytical operation for more than four days. If

the system is to be shut down for a long period of time, the following steps should be taken:

1. Turn off hydrogen at mass flow controller (sulfur instruments only).

2. Turn off helium make up flow using toggle valve.

3. Turn off ozone generator.

4. Turn off high voltage power supply.

5. Allow oxidation period.

6. Program furnace temperature to zero.

7. Allow furnace to cool to ambient temperature.

8. When furnace is cool, turn off vacuum pump.

9. Turn off main power, then turn off oxygen and hydrogen at their cylinders.

9.7 Routine Maintenance

The PAC 7090 System is a relatively low maintenance analyzer. Regular care of a few items should keep

the system operating at peak level. The following is a recommended routine maintenance

schedule:

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9.7.1 Daily

1. Check cylinder supply pressure for all supply gases.

2. Check all gas flows via mass flow controller display.

3. Check all analytical parameters including temperatures, detector settings, etc.

4. Check the validity of any calibration curve being used by analyzing at least one

standard of known concentration and comparing the results to the existing

curve.

9.7.2 As Needed

1. Lenses may need to be cleaned from time to time. Residue may accumulate on

the lenses of the reaction chamber. Generally this is only performed on a

yearly basis, but if response decreases steadily or the system exhibits poor

repeatability, it may be an indication that the lenses need cleaning.

2. Replace any items in the analytical flow path which have degraded with use

(i.e. Pyrotubes, interconnect tubing, O-rings, etc.).

3. Empty and recharge the scrubber with fresh material. Refill kits (P/N 72001)

are available from PAC. (Normally done once a year)

9.7.3 Reaction Chamber Cleaning Procedures

In the event the lens in the detector reaction chamber needs cleaning or replacement, the

following steps should be taken:

1. Turn the main power switch of the 7090 system to the OFF position and

unplug the power cord from the power source.

WARNING:

Ensure that the power cord has been unplugged from the power source before

continuing. If power is applied while servicing internal components, a severe

electric shock hazard may exist.

2. Remove the side panel of the 7090 system.

3. Locate the sulfur detector module on the left of the 7090 system.

4. Carefully remove all interconnecting tubing associated with the detector

reaction chamber assembly, noting their location and orientation.

5. Remove the reaction chamber assembly from the PMT housing by rotating

the reaction chamber clockwise while holding the PMT housing stationary.

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CAUTION:

The PMT is extremely light sensitive. All operations involving the exposure of the

PMT should be conducted in darkness or a very low light situation.

6. Carefully extract the reaction chamber assembly from the housing noting its

orientation.

7. Carefully cover the open end of the PMT housing with a soft lint-free cloth.

NOTE:

At this point, the reaction chamber assembly may be repaired or replaced with a new

assembly.

8. Unscrew the lens ring and carefully remove the lens ring and cutoff lens,

noting their location.

9. Carefully clean the lenses and the reaction chamber with a soft, lint-free cloth

and a solvent such as acetone or methanol.

10. Dry the lenses and the reaction chamber with a soft, lint-free cloth and

ensure that no particles or lint are on the lenses.

11. Install a new silicone O-ring and install the cutoff lens and the lens ring. Secure

the lens ring.

12. Install the reaction chamber assembly into the PMT housing.

13. Replace all interconnecting tubing.

CAUTION:

Ensure that all interconnections are properly installed. Improper connections may

cause damage to system components.

14. Replace side panels.

15. Perform the start-up sequence outlined in Chapter 5 and confirm proper

operation of the repaired reaction chamber assembly.

16. Resume normal operation.

9.8 Practical Troubleshooting Checklist

9.8.1 Gases

1. Gases on

2. Oxygen pressure at 40 psi

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3. Hydrogen (if present) is at 40–65 psi

4. Leak check performed

9.8.2 Instrument Conditions

1. Main Power Switch is on

2. All lights are on

3. Fuses are good

4. Proper gain selection (Hi/Low)

5. Proper sensitivity selection (x50, x25, x10, x5, x1)

6. Auto zero light off

7. Displayed signal level ~ zero

8. Autozero light comes on when selected

9. High Voltage switch on and display shows voltage

10. O3 switch on

11. Display shows voltage change

12. Furnace should heat or be at temperature

13. All lights green

9.8.3 Vacuum Pump

1. Vacuum pump is on

2. Fuses are good

3. Display vacuum changes from 760 when the vacuum pump is turned on

9.8.4 Furnace

1. Furnace is at temperature

2. Fuses are good

3. Temperature controller is programmed

4. Cables are connected

5. O2 pressure must be 40 psi to heat

6. Vacuum must be below setpoint

9.8.5 Gas Chromatograph Conditions

1. Injector temperature

2. Injection valve

3. Septum

4. Column type and selection

5. Column temperature

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6. Detector temperature

7. Column flows

9.8.6 Proper Integrator Channel selected

1. Ensure appropriate integrator channel is selected.

9.8.7 Detection Problems

1. PMT voltage on

2. High Voltage on

3. Temperature correct

4. No gas leaks

5. Flows correct

6. Reaction chamber lens is clean

7. Pyrotubes are oxidized and in good condition

8. Instrument cooling fans turning and unobstructed

a. Main fan (rear panel)

b. Thermal Electric Cooler (Nitrogen only)

9.8.8 Noise Problems

1. PMT voltage not too high

2. Flows not too high

3. No light leaks

4. No gas leaks

5. Gains and settings not too high

6. Check main power in.

9.8.9 Practical Troubleshooting Hints

Answers to the following questions will help the Service Department better troubleshoot and

determine the problem with your instrument.

1. Does the problem stop when the ozone generator is turned off?

2. Does the problem stop when the high voltage is turned off?

3. Does the baseline move when shadows are on the instrument or when light is

shined on the instrument?

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4. Does the detector respond when a light leak is created?

5. Is furnace vacuum below 760, but not below setpoint? Could mean a broken

inner pyrotube.

6. Is furnace vacuum below setpoint when hydrogen is flowing? Is detector

vacuum below 35 torr?

7. Is furnace vac increasing? Could mean an obstruction in oxygen or supply

lines.

9.9 Analytical Troubleshooting

This section is a guide for isolating and correcting problems which may arise while operating the

PAC 7090 system.

NOTE:

The following guide is primarily concerned with troubleshooting the 7090

system. This guide should be used in conjunction with normal gas

chromatograph and column troubleshooting guides. To use this guide, simply

locate the symptom in the left column and follow suggestions for probable cause

and solution.

Before attempting to perform any troubleshooting and before taking any action to remedy an

apparent problem, ensure that all components of the analytical system and any accessories are

properly assembled.

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Symptom Probable Cause Solution

Baseline Problems: Baseline off scale - positive(+) Zero control not adjusted

PMT voltage too high

Contaminated gas supply

Contaminated pyrotube

Contaminated transfer

tubing

Contaminated reaction

chamber

Light leak

Press autozero.

Adjust PMT voltage.

Change gas supply.

Re-oxidize or replace

pyrotube.

Clean or replace tubing.

Clean reaction chamber.

Repair light leak.

Baseline off scale - negative(-) Zero control not adjusted Press autozero.

Baseline drift - positive(+) Contaminated gas supply

Contaminated septum

Contaminated pyrotube

Contaminated transfer

tubing

Contaminated reaction

chamber

Gas leak

Vacuum leak

Column bleed

Change gas supply.

Replace septum.

Re-oxidize pyrotube or replace

pyrotube. Clean tubing or

replace.

Clean reaction chamber.

Repair gas leak.

Repair vacuum leak.

Recondition column, reduce

temperature, replace column.

Baseline drift - negative(-) Contaminated septum

Contaminated pyrotube

Moisture in gas supply or

gas supply lines quenching

ozone

Replace septum.

Re-oxidize pyrotube or replace

and oxidize new pyrotube.

Change to new gas supply,

replace inline gas purifiers.

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Baseline shifts during analysis Change in system gas flow

during sample introduction

Sample size too large

Septum leak

Column bleed

Incomplete combustion of

the sample

Sample reacting with the

sample

Faulty fan motor can cause

internal temperature

instability

Check for obstruction or leak

in analytical system.

Reduce sample size.

Replace septum.

Condition column, reduce

temperature, or replace

column.

Ensure that the furnace

temperatures, split flow, and

gas flows are correct.

Convert to a non-reactive

injection system.

Check instrument fan to be on

and free from obstruction.

Baseline shift – anytime Change in gas system flows

Gas leak

Septum leak

Column bleed

Light leak

Vacuum leak

Liquid trapped in transfer

line

Moisture present in reaction

chamber housing

Faulty fan motor can cause

internal temperature

instability

Check for obstruction or leak

in analytical system or quality

of gas supply and lines.

Repair gas leak.

Replace Septum.

Condition column, reduce

temperature or replace column.

Repair light leak.

Repair vacuum leak.

Ensure that all lines are clean

and dry.

Ensure reaction chamber is

clean and dry.

Check instrument fan to be on

and free from obstruction.

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Baseline noise Unstable power source

Unstable power supply

Faulty signal cable

Faulty PMT

Faulty pre-amp printed

circuit board

Faulty amplifier printed

circuit board

Noisy ozone generator

Faulty gas regulator

Light leak

Unstable temperatures

Contaminated furnace

interface

Photomultiplier (PMT) not

cooled (Nitrogen only)

Moisture present in reaction

chamber housing

Faulty fan motor can cause

internal temperature

instability

Stabilize power.

Replace power supply.

Replace signal cable.

Replace PMT.

Replace pre-amp, printed

circuit board.

Replace amplifier printed

circuit board.

Replace ozone generator cell

or assembly.

Replace regulator.

Repair light leak.

Ensure that the ambient

temperature and the instrument

temperature zones are stable.

Clean furnace interface tubing.

Check setting or replace

cooler.

Ensure reaction chamber is

clean and dry.

Check instrument fan to be on

and free of obstructions.

Baseline Problems:

See following page.

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No Peaks Gas leak

No ozone

No sample introduction

Contaminated or spent

pyrotube

No PMT voltage

Loose cable

Faulty PMT

Faulty pre-amp printed

circuit board

Faulty amplifier printed

circuit board

Capillary column plugged

Broken inner pyrotube

(sulfur only)

Sample reacting with the

sample injection system

Septum leak

Repair gas leak.

Check ozone generator.

Check sample injector or inject

a known standard.

Re-oxidize pyrotube or replace

and oxidize new pyrotube.

Check PMT voltage.

Secure all cables.

Replace PMT.

Replace pre-amp printed

circuit board.

Replace amplifier printed

circuit board.

Break cm (in) off the inlet of

the capillary column.

Replace inner pyrotube and

oxidize pyrotubes.

Convert to a non-reactive

injection system.

Replace septum.

Negative Peaks Signal cable attached

backwards

Improper gas flows

Reverse + and – leads

Adjust gas flows.

Ghost peaks Contaminated gas supply

Contaminated septum

Contaminated pyrotube

Contaminated transfer

tubing

Contaminated column

Contaminated or reactive

injector

Change gas supply.

Replace septum.

Re-oxidize or replace

pyrotube.

Clean or replace transfer

tubing.

Condition or replace column.

Clean or replace injector

assembly.

Tailing Peaks Gas leak

Septum leak

Change in system gas flow

during sample introduction

Incorrect flows

Poor sample introduction

Replace gas leak.

Replace septum.

Check for obstruction in

analytical system.

Ensure that flows are correct

Check injection.

Split Peaks Poor capillary column

Wrong column material for

sample components

Incorrect temperatures

Replace capillary column.

Use different type of column.

Check all temperature zones.

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Low Response Gas leak

Septum leak

Change in system gas flow

during sample introduction

Incorrect flows

Poor sample introduction

Incorrect Gain, sensitivity

or PMT Voltage

Sample size too small

Dirty reaction chamber or

lens

Insufficient ozone

production

Replace gas leak.

Replace septum.

Check for obstruction in

analytical system.

Ensure that flows are correct

Check injection.

Check instrument settings.

Increase sample size or

decrease split ratio.

Clean reaction chamber and

lens.

Ensure ozone generator is on

and is producing sufficient

ozone

Changes in response Gas leak

Septum leak

Change in system gas flow

during sample introduction

Contaminated septum

Contaminated gas supply

Contaminated gas pyrotube

Unstable power source

Faulty gas regulator

Poor sample introduction

No sample introduction

Incorrect flows

Change in ozone

production

Change in PMT voltage

Abnormal ambient

temperature change Light

leak

Faulty PMT

Faulty pre-amp printed

circuit board

Faulty amplifier printed

circuit board

Dirty reaction chamber or

lens

Faulty fan motor can cause

internal temperature

instability

Replace gas leak.

Replace septum.

Replace septum.

Replace septum.

Change gas supply.

Oxidize or replace pyrotube.

Stabilize power.

Replace regulator.

Check injection.

Check sample injector.

Ensure that flows are correct.

Check ozone generator

performance. Check PMT

voltage.

Stabilize ambient temperature.

Repair light leak.

Replace PMT.

Replace pre-amp printed

circuit board.

Replace amplifier printed

circuit board

Clean reaction chamber and

lens.

Check instrument fan to be on

and free from obstruction.

Flat top peaks Saturation of electronics Reduce sample size,

concentration, or gain,

sensitivity or PMT voltage; or

increase split introduction.

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Nonlinear curve Saturation of electronics

Contaminated gas supply

Contaminated pyrotube

Poor sample introduction

No sample introduction

Incorrect flows

Change in ozone

production

Reduce sample size,

concentration, or gain,

sensitivity or PMT voltage; or

increase split introduction.

Change gas supply.

Oxidize or replace pyrotube

Check injection.

Check sample injector.

Ensure flows are correct.

Check Ozone Generator

performance.

Small linear range Saturation of electronics

Contaminated gas supply

Contaminated pyrotube

Poor sample introduction

No sample introduction

Incorrect flows

Change in ozone

production

Reduce sample size,

concentration, or gain,

sensitivity or PMT voltage; or

increase split introduction.

Change gas supply.

Oxidize or replace pyrotube.

Check injection.

Check sample injector.

Ensure flows are correct.

Check Ozone Generator

performance.

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Non-repeatable results Saturation of electronics

Contaminated septum

Contaminated gas supply

Contaminated pyrotube

Poor sample introduction

Incorrect flows

Flow path restrictions

Sample frequency too fast

Change in ozone

production

Change in PMT voltage

Ambient temperature

change

Light leak

Faulty PMT

Faulty pre-amp printed

circuit board

Faulty amplifier printed

circuit board

Gas leak

Improper sample size

Incomplete combustion of

sample

Unstable temperatures

Noise baseline

Faulty fan motor can cause

internal temperature

instability

Reduce sample size,

concentration, or gain,

sensitivity or PMT voltage; or

increase split introduction.

Replace septum.

Change gas supply.

Oxidize or replace pyrotube.

Check injection.

Ensure flows are correct.

Check fittings, ferrules,

pyrotube, and vents for

restrictions.

Reduce sample frequency

Check ozone generator

performance.

Check PMT voltage

Stabilize ambient temperature.

Repair light leak.

Replace PMT.

Replace pre-amp printed

circuit board.

Replace amplifier printed

circuit board.

Repair gas leak.

Adjust sample size.

Ensure that furnace

temperature and oxygen flow

are correct.

Ensure that the ambient

temperature and the instrument

temperature zones are stable.

Stabilize baseline.

Check instrument fan to be on

and free from obstruction.

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Inaccurate results Inaccurate calibration curve

Inaccurate calibration

standards

Saturation of electronics

Contaminated septum

Contaminated gas supply

Contaminated pyrotube

Poor sample introduction

Incorrect flows

Change in ozone

production

Change in PMT voltage

Ambient temperature

change

Light leak

Faulty PMT

Faulty pre-amp printed

circuit board

Faulty amplifier printed

circuit board

Gas leak

Incomplete combustion of

sample

Unstable temperatures

Faulty fan motor can cause

internal temperature

instability

Re-calibrate the system.

Construct new calibration

standards.

Reduce sample size,

concentration, or gain,

sensitivity or PMT voltage; or

increase split introduction.

Replace septum.

Change gas supply.

Oxidize or replace pyrotube

Check sample injector.

Ensure flows are correct.

Check ozone generator

performance.

Check PMT voltage.

Stabilize ambient temperature.

Repair light leak.

Replace PMT.

Replace pre-amp printed

circuit board.

Replace amplifier printed

circuit board.

Repair gas leak.

Ensure that furnace

temperature and oxygen flow

are correct.

Ensure that the ambient

temperature and the instrument

temperature zones are stable.

Check instrument fan to be on

and free from obstruction.

Coking (sooting) Incomplete combustion of

sample

Incorrect flows

Gas leak

Too much sample

Ensure that furnace

temperature and oxygen flow

are correct.

Ensure that flows are correct.

Repair gas leak.

Reduce sample size or increase

split introduction.

Furnace problems Oxygen pressure below 40

psi

Increase pressure.

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Furnace not heating Vacuum not below setpoint

Temperature controller is

not programmed

Furnace cable is

disconnected

Furnace fuse is blown

Transformer fuse is blown

Temperature Controller

fuse is blown

Furnace element is burnt

out

Faulty solid state relay

(SSR)

Correct vacuums.

Program Controller.

Connect furnace cable.

Replace Fuse.

Replace Fuse.

Replace Fuse.

Replace furnace.

Replace solid state relay

(SSR).

No temp readout-existing

temperature

Loose thermocouple

connector

Defective thermocouple

Faulty solid state relay

(SSR)

Secure thermocouple zone

connector.

Replace thermocouple.

Replace solid state relay

(SSR).

Overheating of a temperature

zone

Improper setpoint

Shorted thermocouple

Faulty solid state relay

(SSR)

Program controller.

Replace thermocouple.

Replace solid state relay

(SSR).

Gas system / Flow problems

Mass flow controllers indicate no

flow

No supply pressure

Closed control valve

Leaks

Restricted gas line

No power to Mass Flow

controllers (MFC)

Supply pressure greater

than 60 psi

Supply pressure less than

40 psi

Defective Mass Flow

controller (MFC)

Mass Flow Controllers

(MFC) board not secure

Loose 16-pin ribbon cable

to Mass Flow Controller

Board

Flow adjustments not made

Check supply gas.

Adjust control valve.

Correct leaks.

Correct restrictions.

Check +15VDC power supply

and fuses.

Correct gas supply pressure.

Correct gas supply pressure.

Replace defective Mass Flow

controller (MFC).

Secure board.

Secure ribbon cable.

Adjust flow settings.

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No ozone Ozone switch off

Oxygen pressure below 40

psi

Leaks in ozone system

Faulty ozone generator cell

Faulty ozone generator

printed circuit board

Faulty ozone generator

transformer

Faulty +5VDC power

supply or fuse

Turn ozone on

Increase oxygen pressure.

Correct leaks.

Replace ozone generator cell.

Replace ozone generator

printed circuit board.

Replace ozone generator

transformer.

Replace +5VDC power supply

or fuse.

No hydrogen flow Hydrogen solenoid not

energized

Flow not set

Defective Mass Flow

controller

Check hydrogen solenoid

parameters (See hydrogen

solenoid not energized below).

Correct setting.

Replace Mass Flow Controller.

Hydrogen solenoid not energized

24 VAC not present

Temperature controller not

properly set for alarm

Temperature below alarm

setpoint

Vacuum not below setpoint

Oxygen pressure below 40

psi

Check 24 VAC input/output

fuses.

Program controller.

Increase temperature.

Correct vacuums.

Increase pressure.

Furnace vacuum (P1) not reading

760 when system is open to

atmosphere

Board not calibrated Replace or recalibrate.

Furnace vacuum (P1) not below

setpoint with vacuum applied

Too much flow

Broken pyrotube

Plugged oxygen supply line

to furnace

Leaks

Bad vacuum pump

Board not calibrated

Column broken

Check gas flow settings.

Replace pyrotube.

Ensure oxygen supply line is

clean and unobstructed.

Repair leaks.

Repair or replace.

Replace or recalibrate.

Replace column.

Control Problems

No PMT voltage displayed PMT switched OFF

24VAC transformer input

fuse blown (rear panel)

24 VAC transformer ouput

fuse blown (rear panel)

24 VAC fuse blown (in

tray)

Faulty high voltage power

supply PC board

Shorted high voltage cable

Switch PMT to ON.

Replace fuse.

Replace fuse.

Replace fuse.

Replace high voltage power

supply board.

Replace cable.

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No baseline deflection when High

Voltage is turned on

High voltage not present at

photomultiplier tube

Active signal no present or

detected

Loose or defective high

voltage cable or connector

Check voltage at PMT.

Monitor signal level at

instrument display when High

Voltage is turned on or off

Secure high voltage cable

connector.

No baseline deflection when

ozone generator is turned on

Ozone not being generated

Active signal not present or

detected

+5VDC not present at

ozone generator board

Check for presence of ozone

Monitor signal level at

instrument display when ozone

monitor is turned on or off

Correct -5VDC problem.

No Auto-Zero control Loose ribbon cable

Improperly adjusted

amplifier board

PMT voltage too high

Open signal from PMT

Faulty pre-amplifier PC

board

Faulty amplifier PC board

Secure ribbon cable.

Adjust board.

Lower PMT voltage.

Check signal cable from PMT.

Replace pre-amplifier PC

board.

Replace amplifier PC board.

System Status LEDs not

energized

Oxygen pressure is below

40 psi

Increase oxygen pressure to 40

psi.

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10. DATA SHEETS

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NOTE: There is no MSDS-10 page.

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Petroleum Analyzer Company, LP.

Web site: www.paclp.com

For a complete list of contact information, refer to the Contacts section of this publication.