MultiTek Operation

MultiTek ®
Operation Manual
8824 Fallbrook Dr.• Houston, Texas 77064 • USA

Phone: (800) 444-TEST or (281) 580-0339 •FAX: (281) 580-0719
service@paclp.com • sales@paclp.com • web site: www.paclp.com
®
MULTITEK ANALYZER
© 2012 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.
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,
the MultiTek®
trademark, and Petroleum Analyzer Company, L.P.’s distinctive color trademark as used
on its instruments and in these materials, are trademarks or service marks or registered
trademarks or registered service marks of Petroleum Analyzer Company, L.P. in the U.S.
and other countries and are its sole and exclusive property.
MS Windows, MS Windows XP, and MS Windows Professional are registered

trademarks of Microsoft Corp.
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 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 from small 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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Policy Statement
The instructions given herein cover generally the description, installation, operation, and
maintenance of subject equipment. PAC reserves the right to make engineering
refinements that may not be reflected in this manual. Should any questions arise which
may not be answered specifically by these instructions, they should be directed to PAC
for further detailed information and technical assistance.
Your satisfaction and safety are important to PAC, and a complete understanding of this
manual is necessary to attain these objectives. As the ultimate user of this apparatus, it is
your responsibility to understand its proper function and operational characteristics. This
instruction manual should be read thoroughly and all operators should be given adequate
training before attempting to place this unit in service. Awareness of the stated cautions
and warnings, and compliance with recommended operating and maintenance parameters
are important for safe and satisfactory operation.
This unit should be used only for its intended operation; alterations will void the
Warranty.
This manual contains confidential and proprietary information…

This is the property of PAC L.P. This manual and all information disclosed herein shall
not be used to manufacture, construct, or fabricate the goods disclosed herein; shall not be
exploited or sold; shall not be copied or otherwise reproduced in whole or in part and shall
not be revealed or disclosed to others or in any manner made public without the express
written permission of PAC L.P.
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REVISION HISTORY
Rev A First release September 2009
Rev B Diagrams and Software Updates April 2010
Rev C Software Updates, Corrections November 2010

& Added Content
Rev D Software Updates and Corrections August 2011
Rev E Software v2.0.0.0 Updates January 2012

Trademark Update / Material Safety
Data Sheets (MSDS)
Copyright ©2012, by PAC L.P., 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.
1.27.12
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Software License
1. Under this Software License Agreement (the "Agreement"), PAC L.P. (the "Vendor") grants to the user (the "Licensee") a
non-exclusive and non-transferable license (the "License") to use MultiTek® Software (the "Software").
2. "Software" includes the executable computer programs and any related printed, electronic and online documentation and
any other files that may accompany the product.
3. Title, copyright, intellectual property rights and distribution rights of the Software remain exclusively with the Vendor.
Intellectual property rights include the look and feel of the Software. This Agreement constitutes a license for use only and
is not in any way a transfer of ownership rights to the Software.
4. The Software may be loaded onto no more than one computer. A single copy may be made for backup purposes only.
5. The rights and obligations of this Agreement are rights granted to the Licensee only. The Licensee may not transfer or
assign any of the rights or obligations granted under this Agreement to any other person or legal entity. The Licensee may
not make available the Software for use by one or more third parties.
6. The Software may not be modified, reverse-engineered, or de-compiled in any manner through current or future available
technologies.
7. Failure to comply with any of the terms under the License section will be considered a material breach of this Agreement.
License Fee
8. The original purchase price paid by the Licensee will constitute the entire license fee and is the full consideration for this
Agreement.
Limitation of Liability
9. The Software is provided by the Vendor and accepted by the Licensee "as is". Liability of the Vendor will be limited to a
maximum of the original purchase price of the Software. The Vendor will not be liable for any general, special, incidental
or consequential damages including, but not limited to, loss of production, loss of profits, loss of revenue, loss of data, or
any other business or economic disadvantage suffered by the Licensee arising out of the use or failure to use the Software.
10. The Vendor makes no warranty expressed or implied regarding the fitness of the Software for a particular purpose or that
the Software will be suitable or appropriate for the specific requirements of the Licensee.
11. The Vendor does not warrant that use of the Software will be uninterrupted or error-free. The Licensee accepts that
software in general is prone to bugs and flaws within an acceptable level as determined in the industry.
Warrants and Representations
12. The Vendor warrants and represents that it is the copyright holder of the Software. The Vendor warrants and represents that
granting the license to use this Software is not in violation of any other agreement, copyright or applicable statute.
Acceptance
13. All terms, conditions and obligations of this Agreement will be deemed to be accepted by the Licensee ("Acceptance") on
installation of the Software.
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Term
14. The term of this Agreement will begin on Acceptance and is perpetual.
Termination
15. This Agreement will be terminated and the License forfeited where the Licensee has failed to comply with any of the terms
of this Agreement or is in breach of this Agreement. On termination of this Agreement for any reason, the Licensee will
promptly destroy the Software or return the Software to the Vendor.
Force Majeure
16. The Vendor will be free of liability to the Licensee where the Vendor is prevented from executing its obligations under this
Agreement in whole or in part due to Force Majeure, such as earthquake, typhoon, flood, fire, and war or any other
unforeseen and uncontrollable event where the Vendor has taken any and all appropriate action to mitigate such an event.
Governing Law
17. The Parties to this Agreement submit to the jurisdiction of the courts of the State of Texas for the enforcement of this
Agreement or any arbitration award or decision arising from this Agreement. This Agreement will be enforced or construed
according to the laws of the State of Texas.
Miscellaneous
18. This Agreement can only be modified in writing signed by both the Vendor and the Licensee.
19. This Agreement does not create or imply any relationship in agency or partnership between the Vendor and the Licensee.
20. Headings are inserted for the convenience of the parties only and are not to be considered when interpreting this
Agreement. Words in the singular mean and include the plural and vice versa. Words in the masculine gender include the
feminine gender and vice versa. Words in the neuter gender include the masculine gender and the feminine gender and vice
versa.
21. If any term, covenant, condition or provision of this Agreement is held by a court of competent jurisdiction to be invalid,
void or unenforceable, it is the parties' intent that such provision be reduced in scope by the court only to the extent deemed
necessary by that court to render the provision reasonable and enforceable and the remainder of the provisions of this
Agreement will in no way be affected, impaired or invalidated as a result.
22. This Agreement contains the entire agreement between the parties. All understandings have been included in this
Agreement. Representations which may have been made by any party to this Agreement may in some way be inconsistent
with this final written Agreement. All such statements are declared to be of no value in this Agreement. Only the written
terms of this Agreement will bind the parties.
23. This Agreement and the terms and conditions contained in this Agreement apply to and are binding upon the Vendor's
successors and assigns.
Notices
24. All notices to the Vendor under this Agreement are to be provided at the following address:
PAC L.P., Attn: Software Development Dept.
8824 Fallbrook Drive, Houston, TX 77064
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STANDARD LIMITED WARRANTY

OF
PETROLEUM ANALYZER COMPANY, L.P.
I. Limited Warranty
1. Limited Warranty. Petroleum Analyzer Company, L.P. (“PAC”) offers a limited warranty on each of its products against
failure due to defects in material and workmanship for a period ending the earlier of (i) eighteen (18) months from the date of the
invoice relating to the sale of the product and (ii) twelve (12) months from the date of installation of the product (collectively,
the “Initial Warranty”). During the Initial Warranty, PAC offers a limited warranty against failure due to defects in material and
workmanship on each part of a product repaired or replaced by an authorized service person for a period ending the later of (a)
the remaining term of the Initial Warranty of the product and (b) ninety (90) days from the date of such repair or replacement.
After expiration of the Initial Warranty, PAC offers a limited warranty against failure due to defects in material and
workmanship on each part of a product repaired or replaced by an authorized service person for a period ending ninety (90) days
from the date of such repair or replacement. PAC further offers a limited warranty that the products and parts it sells will
conform to PAC’s written specifications therefore. The foregoing limited warranties cover parts and labor only and PAC does
not warrant and will not reimburse the buyer of its products (“Buyer”) for any costs relating to the access by service persons of
PAC to the product at issue. The foregoing limited warranties cover only the repair or replacement of defective parts and such
determination will be in the sole discretion of PAC. In its sole discretion, PAC may make repairs or replacements under these
limited warranties with either new or refurbished parts. To the extent, Buyer’s product cannot be remedied under these limited
warranties through repair or replacement of parts, Buyer may return the product for a refund of the purchase price, less a
reasonable reduction in such purchase price equal to the depreciation expense incurred by Buyer relating to such product. The
limited warranties of this Section 1.1 are further subject to those warranty exclusions set forth below in Section 1.2.
2. Limited Warranty Exclusions. EXCLUDING THE WARRANTIES PROVIDED FOR IN SECTION 1.1., PAC
PROVIDES ALL PRODUCTS TO BUYER “AS-IS,” WITHOUT ANY OTHER WARRANTY OF ANY KIND. PAC
DISCLAIMS ANY AND ALL EXPRESS OR IMPLIED WARRANTIES OF MERCHANTABILITY, FITNESS FOR A
PARTICULAR PURPOSE AND NON-INFRINGEMENT OF THE INTELLECTUAL PROPERTY OF OTHERS. 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. 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 therefore; (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 labor expenses associated with field repairs or the repair or replacement of defective parts in the engine or power
unit of any product if such product has been in the possession of the owner or operator for greater than twelve (12) months.
There is no warranty for products determined to be, in PAC’s sole discretion, damaged 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 UV lamps.
3. Non-PAC Products. PAC does not in any way 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. If a manufacturer warranty is so
assigned to PAC, PAC will only be bound to comply with the length of time associated with such warranty. All other terms of
such warranty will be governed by this Standard Limited Warranty and PAC’s General Terms and Conditions incorporated
herein by reference.
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4. Expenses on 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 products 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.2., Buyer shall be liable for all direct expenses incurred by PAC to conduct the inspection and
review of the product.
5. Exclusive Remedy. THE FOREGOING LIMITED WARRANTY 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.
6. Procedure and Costs. All limited warranty claims must be made in writing promptly following discovery of any defect.
Buyer must hold defective 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.
7. 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 PAC SHALL NOT BE LIABLE FOR ANY DIRECT, INDIRECT, INCIDENTAL,
PUNITIVE OR CONSEQUENTIAL DAMAGES, INCLUDING LOST PROFITS, LOST SAVINGS OR LOSS OF USE,
WHETHER BUYER’S CLAIM IS BASED IN CONTRACT, TORT, WARRANTY, STRICT LIABILITY OR
OTHERWISE, WHICH BUYER MAY SUFFER FOR ANY REASON, INCLUDING REASONS ATTRIBUTABLE TO
PAC. Buyer agrees these limitations on PAC’s liability are reasonable and reflected in the amounts charged by PAC for its
products.
2. Overpowering Circumstances. This Standard Limited Warranty does not cover and PAC L.P. 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 strikes or riots,
war, damages or improper operation due to intermittent power line voltage, frequency, electrical spikes or surges, unusual shock
or electrical damage; or (iii) accident, fire or water damage, neglect, corrosive atmosphere or causes other than ordinary use.
3. Limitation on Warranty Claims. Prior to any obligation of PAC L.P. 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 L.P. of the limited warranty claim within sixty (60) days from the date Buyer knew or had reason to know
of the defect.
8824 Fallbrook Dr. • Houston, Texas • 77064 - 9912 • USA

Phone 800-444-TEST or 281.580.0339 • Fax 281.580.0719
service@paclp.com • sales@paclp.com •www.paclp.com
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CE Notice
The symbol indicates PAC’s compliance with the European Union (EU) directives and standards
listed below:
 EMC Directive
 89/336/EEC
 EN 55022: 1994, Class A/B – “Information Technology Equipment - Radio Disturbance

Characteristics Limits and Methods of Measurement”
 EN 550082-1: “Electromagnetic compatibility – Generic Immunity Standard,” “Generic

Standard Class Residential, Commercial, and Light Industry”
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.
Declarations of Conformity, in accordance with the preceding directives and standards, have been made
and are on file with each device’s manufacturer.
Issued 2009
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 your importer on the end-of-life disposal in a way that
you will care for disposal by your own, would you 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 however uses the marking in all EC-Member states.
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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 products 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 products
being returned as is, at the buyer’s expense.
ON-SITE REPAIR
If a PAC L.P.’s 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. If service is rendered at times other than normal work
periods, then special service rates may apply.
Record of Serial Number and Purchase Date

Serial Number: ________________________
Purchase Date: _________________________
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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 upon the
carrier by the recipient as follows:
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.
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Contact Us
If you have any questions about your Antek MultiTek® Analyzer, contact us using the
information below or on the next page:
PAC L.P.
8824 Fallbrook Drive
Houston, Texas 77064
http://www.paclp.com
Phone Number: (800) 444-TEST or (281) 580-0339
Fax Number: (281) 580-0719
Email Support: sales@paclp.com
service@paclp.com
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PAC LP
8824 Fallbrook Drive
Houston, TX 77064
USA
Web: http://www.paclp.com
Phone: USA +1 281 940 1803
France +33 231 264 300
Germany +49 9343 6400
Singapore +65 6742 8453
Netherlands +31 10 462 4811
Russia & CIS +7 495 617 10 86
China +86 10 65072236
South Korea +82 2 785 3900
Thailand +65 6412 0890
Abu Dhabi +971 2 446 9671
Fax: USA +1 281 580 0719
France +33 231 266 293
Germany +49 9343 640 101
Singapore +65 6742 8759
Netherlands +31 10 462 6330
Russia & CIS +7 495 913 97 65
China +86 10 65072454
South Korea +82 2 785 3977
Thailand +65 6412 0899
Abu Dhabi +971 2 446 9672
Sales: USA mailto:sales@paclp.com
France mailto:sales@paclp.com
Germany mailto:sales@paclp.com
Singapore mailto:sales@paclp.com
Netherlands mailto:acbv@paclp.com
Russia & CIS Alexander.sungurov@paclp.com
China sales@paclp.sg
South Korea sales@paclp.sg
Thailand sales@paclp.sg
Abu Dhabi sales.middleeast@paclp.com
Service: USA service.usa@paclp.com
France service.france@paclp.com
Germany service.germany@paclp.com
Netherlands service.netherlands@paclp.com
Russia service.russia@paclp.com
India service.india@paclp.com
Singapore service.singapore@paclp.com
China service.china@paclp.com
South Korea service.southkorea@paclp.com
Thailand service.thailand@paclp.com
Abu Dhabi service.middleeast@paclp.com
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Table of Contents
Software License .................................................................................................................v
RETURN POLICY ........................................................................................................x
Inspection ........................................................................................................................xi
Contact Us ........................................................................................................................ xii
Table of Contents ................................................................................................................1
SECTION 1 INTRODUCTION .......................................................................................7
Introduction ...............................................................................................................7
System Components..................................................................................................9
Computer Requirements .........................................................................................11
General Specifications ............................................................................................12
Environmental Requirements..................................................................................13
Electrical Requirements ..........................................................................................14
Gas Requirements ...................................................................................................15
SECTION 2 INSTALLATION ......................................................................................23
Introduction .............................................................................................................23
Hardware Installation ..............................................................................................23
PC Installation/Configuration .................................................................................24
MultiTek® Software Installation .............................................................................27
MultiTek® IC Sampler Control Software Installation .............................................38
Vendor Specific IC Analyzer Software Installation................................................41
Pressure / Leak Tests ..............................................................................................49
Instrument Leak Check Preparations ......................................................................50
Gas Flow Controller (GFC) Testing .......................................................................55
Diagnostic Testing ..................................................................................................59
Furnace Power Up...................................................................................................60
Nitrogen Detector Cooling ......................................................................................60
System Pressure ......................................................................................................61
GFC5 and GFC6 Gas Flow Adjustment .................................................................62
Operational Standby................................................................................................63
Instrument Blank Test .............................................................................................64
Primary Testing Checklist.......................................................................................66
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SECTION 3 NITROGEN / SULFUR OPERATION ...................................................67
MultiTek® Software ................................................................................................67
Connect to Analyzer ...............................................................................................68
Configuration of the MultiTek® Analyzer .............................................................76
Comparing Instrument Parameters Versions ..........................................................81
Create Standards List ..............................................................................................82
Method Creation and Calibration............................................................................85
First and Second Order Calibration Curves ............................................................93
Comparing Method Versions ..................................................................................95
Create and Run a Sequence.....................................................................................96
View Results ...........................................................................................................98
View QC History ..................................................................................................102
Alarm Monitoring .................................................................................................102
Diagnostics............................................................................................................104
Task Scheduler ......................................................................................................105
Audit Trail.............................................................................................................106
SECTION 4 ANALYTICAL PROCEDURES & SUGGESTIONS ..........................107
System Gas Flow Considerations .........................................................................107
Furnace Temperature ............................................................................................108
Sample Handling ...................................................................................................109
Calibration.............................................................................................................111
Sample Analysis....................................................................................................119
Operational Hints ..................................................................................................120
Important Factors for Nitrogen and Sulfur in Certain Sample Types ...................122
SECTION 5 IC SAMPLER CONTROL OPERATION ............................................131
IC Sampler Control Software................................................................................131
Connect to Instrument ...........................................................................................131
Configuration of the IC Sampler Control Software ..............................................135
Diagnostics............................................................................................................136
Running a Sequence ..............................................................................................137
Starting the Sequence ............................................................................................142
Flow of Operation .................................................................................................143
View Alarms .........................................................................................................144
Setting up the Dionex ICS2100 with the MultiTek® IC Software .......................145
Chromeleon Server Configuration ........................................................................145
Loading the Chromeleon IC sequence ..................................................................151
Setting up the Metrohm 881 Compact IC Pro with the MultiTek® IC Software ..152
Method Editor Screen ...........................................................................................156
Sequence Table Configuration ..............................................................................157
Analysis of Halides on the MultiTek® IC .............................................................157
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General Guidelines for Sample Analysis ..............................................................158

Identification and Integration of Target Compounds ............................................158
Blank Analysis ......................................................................................................160
Calibration.............................................................................................................161
System and Sample Treatment..............................................................................161
Water Quality and Use ..........................................................................................161
Columns (general) .................................................................................................161
Dionex ...................................................................................................................161
Metrohm................................................................................................................161
Analyzing Samples ...............................................................................................162
Important Factors for Halides in Certain Sample Types .......................................163
SECTION 6 MAINTENANCE / TROUBLESHOOTING ........................................169

Introduction ...........................................................................................................169
Routine Maintenance ............................................................................................169
Preventive Maintenance ........................................................................................170
Changing the UV Lamp ........................................................................................170
Troubleshooting and Service Guide ......................................................................181
APPENDIX A STANDARDS FOR ANALYSIS.........................................................195
Common Conversions ...........................................................................................195
Exponential Form..................................................................................................195
Making Standards .................................................................................................195
Chemicals for Nitrogen and Sulfur Standard Preparation.....................................197
Chemicals for Halides Standard Preparation ........................................................199
APPENDIX B MATERIAL SAFETY DATA SHEETS – MSDS .............................201

INDICATING DRIERITE™ .................................................................................201
OZONE (O3) .........................................................................................................203
MOLECULITE™ .................................................................................................206
APPENDIX C STATIC AND DYNAMIC IP ADDRESSING ..................................209

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SAFETY LABELS
Failure to follow instructions and procedures contained in this manual could result in
death or serious injury and are intended for use by qualified personnel only. Maintenance
procedures included in this document must be performed by qualified and trained
personnel. Do not perform installation or maintenance operations or procedures outside
the scope of this manual.
WARNING
FIRE HAZARD
UV LIGHT HAZARD
BURN HOT SURFACE HAZARD
SHOCK HAZARD
ELECTROCUTION VOLTAGE HAZARD
BURN HAZARD HOT SURFACE
ELECTRIC GROUND HAZARD
RELEASE OF PRESSURE HAZARD

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In This Manual
 The MultiTek® Analyzer Operation manual contains the following sections:
 Section 1 – Introduction: Gives a description of the MultiTek® Analyzer, product components,

requirements, and specifications.
 Section 2 – Installation: Contains specific procedures for installing and configuring your MultiTek®
Analyzer with required and optional equipment.
 Section 3 – Nitrogen/Sulfur Operation: Describes the processes and procedures necessary for daily
operation of the MultiTek® Analyzer.
 Section 4 – Analytical Procedures & Suggestions: This section provides analytical information that
can be essential to the proper application of the MultiTek® Analyzer.
 Section 5 – ICD Sampler Control Operation: Describes the processes and procedures necessary for
operation of the IC Sampler Control Software.
 Section 6 – Troubleshooting & Maintenance: A guide to troubleshooting and regular maintenance of

the MultiTek® Analyzer.
 Appendix A – Standards for Analysis: Information on making standards and chemicals used.
 Appendix B – Material Safety Data Sheets – MSDS: Safety information about Moleculite, Ozone and
Drierite.
 Appendix C – Static and Dynamic IP Addressing: Setting a static IP address in a MultiTek® instrument
and setting the MultiTek® instrument IP addressing back to dynamic.

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Terms Used in This Manual
To show menu selections in this manual, the > symbol is used. For example,
1. Click Start > Programs > PAC.
The following terms are used in this guide:
Term Meaning
Select To pick an item that begins an action (this includes menu

commands and buttons)
Click To press the left mouse button once
Right-click To press the right mouse button once
Double-click To press the left mouse button twice in rapid succession

without moving the mouse
Dialog box A temporary window that contains options or information

you can edit, select, or use
2. PAC L.P. is also referred to as PAC or Antek throughout the chapters and appendices of this manual.
3.
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The Antek MultiTek® Analyzer is also referred to as MultiTek®, or MultiTek .
Assumptions
The MultiTek® Analyzer is generally installed onsite by a trained service technician. However, on occasion, it
may be necessary to move the hardware or reinstall the software. The hardware and software installations
require the following:
Familiarity with the installation components, such as cabling, stainless steel or copper tubing for gas lines,
connectors, and fittings
 An apparatus with ability to lift and transport at least 80 pounds (36.3 kilograms)
 A working knowledge of computers and associated equipment (keyboard, mouse, and monitor)
 An understanding of scientific benchmarks for contaminates
 A knowledge of storage, handling, and use of specialty gases, such as argon, oxygen, helium, and
hydrogen

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SECTION 1
INTRODUCTION
Introduction
The Antek MultiTek® system is the most advanced, modular, analytical system available for the
detection of nitrogen, sulfur and halides in solid, liquid, or gaseous materials. Five configurations are
available: MultiTek® N for nitrogen analysis, MultiTek® S for sulfur analysis, MultiTek® N-S for
simultaneous nitrogen/sulfur analysis, MultiTek® IC for halide analysis via Ion Chromatography, and
MultiTek® N-S-IC for either simultaneous nitrogen/sulfur analysis or halide analysis in a single
instrument. Halide analysis requires the addition of an Ion Chromatography (IC) system. The MultiTek®
horizontal system may be configured for any combination of nitrogen, sulfur and halide analysis, and is
easily upgradeable.
System features include: single, dual (N-S) detector operation that can alternate with halide analysis,
Windows XP, Vista and Windows 7 compatible (32-bit & 64-bit) Antek MultiTek® Software, PC control
of instrumentation and data processing, support for 21 CFR part 11 requirements, method and data
storage capability; monitored operating parameters that assure instrument performance, instrument
control/operation from a remote location, and more.
MultiTek® software (v2.0.0.0 and later) is available in both standard and 21 CFR part 11 editions. Antek
MultiTek® Software 21 CFR part 11 Edition supports requirements for user who must be compliant with
Food and Drug Administration (FDA) regulations for electronic record keeping. Refer to the Antek
MultiTek® Software 21 CFR part 11 Addendum for details. This manual covers the standard features in
both editions used to operate the MultiTek® instrument.
The principle of operation for nitrogen and sulfur analysis begins with the complete, high temperature
oxidation of the entire sample matrix illustrated in Equation (1). The sample is combusted with oxygen at
a temperature of 1050ºC. Oxidation products include CO2, H2O, NO, SO2, and various other oxides
(designated MOX below). The combustion gases are routed through a membrane drying system to
remove all water and then to the sulfur and/or nitrogen detector module(s) for quantization.
(1) R-N + R-S + O2 → CO2 + H2O + NO + SO2 + MOX

In Equation (2), the NO is reacted with O3 (ozone), produced by an onboard ozone generator, to form
NO2* (excited nitrogen dioxide). As the metastable species decays, a photon of light is emitted at specific
wavelengths and detected by a photomultiplier tube (PMT). This chemiluminescent emission is specific
for nitrogen and is proportional to the amount of nitrogen in the original sample. Only chemically bound
nitrogen is detected — atmospheric, diatomic nitrogen (N2) is not.
(2) NO + O3 → NO2* + O2 → NO2 + hv + O2

SO2 in the combustion gases is exposed to ultraviolet radiation of a specific wavelength as shown in
Equation (3). This radiation is re-released in the form of sulfur fluorescence. This fluorescence is
detected by a photomultiplier tube (PMT) and is proportional to the amount of sulfur in the original
sample.
(3) SO2 + hv’ → SO2* → SO2 + hv”

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Nitrogen/sulfur calibration standards are analyzed to produce calibration curves. When samples of
unknown nitrogen/sulfur content are analyzed, the MultiTek® Software compares the raw sample data to
the calibration curve to generate and report nitrogen/sulfur concentrations.
MultiTek® IC is a combustion based analyzer using high temperature oxidation and steam to prepare
samples containing halides (fluorine [F], chlorine [Cl], bromine [Br]) and/or sulfur, for ion
chromatographic analysis. Under oxidative conditions at 1050ºC, in the presence of steam, compounds
containing chemically bound halides are converted into carbon dioxide, water, and the respective
hydrogen halides. If present, chemically bound sulfur is converted to sulfur trioxide and/or sulfuric acid.
The combustion products exit the furnace zone and are trapped in a condensed scrubber assembly using
an absorbing solution. The hydrogen halides become free anions and the sulfur trioxide and/or sulfuric
acid are converted to sulfate ions Equation (4). The resulting solution is then transferred to an Ion
Chromatograph (IC) where the solution components are separated and detected. The MultiTek® IC may
also be used to prepare and analyze samples that contain any of the five target ions already present as
anions.
(4) R-X + R-S + O2 + H2O → CO2 + H2O + HX + SO3 → X- + SO42-+ 3 H+
After calibration of the system using standards with known quantities of fluorine, chlorine, bromine,
and/or sulfur, the system may then be used to analyze unknown samples that may contain all to none of
the target elements.

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System Components
Basic System
• Model MultiTek® N, Model MultiTek® S, Model MultiTek® N-S, Model MultiTek® IC, Model
MultiTek® N-S-IC, Model N-IC or Model S-IC
• PC with Windows XP, Vista or Windows 7
• 4 or 8 Port Router (User Supplied)
• Antek MultiTek® Software
• IC Sampler Control Software (Only used with Model MultiTek® IC or Model MultiTek® N-S-IC,
Model N-IC, Model S-IC)
• Accessories for liquid sample analysis
Front panel indicators and control

• State LED
Ready, Sleep, Idle – Green, steady
Running – Green, blinking
Other state (Warm-up, Pre-run, Post-run, Diags) – Yellow
Instrument Power Off – Off
• Ethernet LED
Online – Blue, steady
Instrument ID – Blue, blinking
Offline – Amber
• Furnace LED
Ready (at processing temperature) – Green, steady
Warm-up / Cool-down – Yellow, blinking
Cooled down – Yellow, steady
• Alarm LED
Alarm – Red
Warning – Yellow
No Alarm/Warning – Off
• Start Button
The Start Button is active when a manual sequence is set up and ready. The operator verifies
sample is loaded and ready and then pushes the ‘Start’ button to initiate the sample run.

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Optional Equipment
• Sulfur Module, P/N 101442 (MultiTek N or IC Upgrade to MultiTek N-S, S-IC, or N-S-IC)
® ®
• Nitrogen Module 115V, P/N 101440 (MultiTek® S or IC Upgrade to MultiTek® N-S, or N-IC or N-S-
IC)
• Nitrogen Module 230V, P/N 101441 (MultiTek S or IC Upgrade to MultiTek N-S, N-IC or N-S-IC)
® ®
• IC Module, P/N 101439 (MultiTek® N, S or N-S Upgrade to MultiTek® N-IC, S-IC, or N-S-IC)
• MultiTek® Trace Nitrogen Upgrade Kit 115V, P/N 102905
• MultiTek® Trace Nitrogen Upgrade Kit 230V, P/N 102934
• MultiTek® LLS Module, P/N 101445
• Model 734 Gas/Liquid Inlet System

Series Configuration (X) Option (Y) Voltage (Z)
9908X-Y-ZZZV 7- Automated 1-Gas/Liquid 115
8- Manual 2-Gas 230
3-Liquid
• Model 735 Liquid Solid Syringe Drive

Series Configuration Voltage (X)
99230-XXXV Horizontal 115
99230V-XXXV Vertical 230
• Model 737-M Temperature Programmable Inlet

Series Configuration
101719 (With Turbo) (International Only)
• Model 740 Multi-Matrix Sampler

Series Configuration (X) Voltage (Z)
99091-X-ZZZV 0 - Standard 115
230

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• Model 748 Robotic Autosampler

Series Configuration (X) Voltage (Z)
33127-X-ZZZV 4- Vertical 115
6- Horizontal 230
• Model 758 Liquid Autosampler

Configuration / VAC 230 VAC 115 VAC 100 VAC
Vertical 102667 102668 102669
Horizontal 102670 102671 102672
NOTE
Installation and operation of the Basic System and most optional equipment will be discussed in
this manual. Further information may be supplied in other manuals or addenda to this manual.
Computer Requirements
Minimum system requirements
• 2 GHz 32-bit (x86) or 64-bit (x64) processor
• 1 GB of system memory
• 20 GB free hard drive space (80 GB recommended)
• Operating systems supported:
• Windows XP Pro SP2 or newer
• Windows XP x64Edition, SP2
• Windows XP Professional 32 bit, SP3
• Windows Vista Business 32 bit
• Windows Vista Ultimate 64 bit SP2
• Windows 7 Ultimate32 bit
• Windows 7 Professional 64 bit
• Screen resolution of 1024 x 768 pixels with 128 MB of graphics memory
• DVD-ROM drive
• Fast Ethernet at 100 Mbit/s
• USB 2.0 port

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General Specifications
Physical
Height: 51.5 cm (20.25 in)
Width: 53.3 cm (21.0 in)
Depth: 61.0 cm (24.0 in)
Weight: 36.3 kg (80 lb)
Power Requirements
Stable 115 VAC, 50/60 Hz, 1500 W or Stable 230 VAC, 50/60 Hz, 1500 W
IC Analyzer: 100-240 VAC, 50/60 Hz, 3A maximum
Gas Requirements:
Dry* oxygen: 3 bar (40 psig), 99.75%, 400 – 650 mL/min
Dry* argon: 3 bar (40 psig), 99.99%, 50 – 200 mL/min
*Dry is defined as 5 ppm water, maximum
Isothermal Temperature Zones

Pyro Zone: ambient to 1100°C in 1°C increments
Auxiliary Zones: two auxiliary zones available
Water Requirements- IC Module Only

16 Mega ohms, Type 1 H2O – minimum acceptable purity
18 Mega ohms, Type 1 H2O – recommended
Environmental Information
Pollution degree 2
Installation category II
Altitude 2000 m or below
Humidity 50 to 80%
Temperature 5°C to 40°C
Methods
Storage of methods for analytical parameters, including calibration curves and sample analysis
data are available. All methods for the Sulfur and Nitrogen analysis are preserved and controlled
by the Antek MultiTek® Software. For Halides analysis, the methods are preserved and controlled
for sample introduction by the Antek IC Sampler Controller software, but the IC specific methods
and sample analysis data are preserved and controlled by the IC vendor software.
Timed Events
Each method may contain a number of timed events for control of the external devices and internal
control functions. Included are:
a. External events of sample accessories
b. Start Run
c. Baseline duration
d. Integration Start/Stop

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Printer (user supplied)

A printer may be used for reporting analytical parameters, methods, and results.
Cautions and Warnings

This manual provides the users with various caution and warning messages. Failure to consider
these messages can lead to severe instrument damage and/or personal injury.
Environmental Requirements
Ambient Temperature
Operational stability requires a constant room temperature. Therefore the instrument must be
operated only in a facility with environmental controls to ensure optimal performance. Operation
of the MultiTek® system in variable environmental conditions does not ensure the accuracy of the
results.
Corrosive or Dusty Atmosphere
A corrosive atmosphere will in time cause problems with solder joints, electrical contacts and the
thermoelectric cooler. Dust and dirt that may be swept in by cooling fans may collect and retain
moisture thus causing corrosion and short circuits. Dust may also collect on heat transfer surfaces
causing reduced radiation and resulting in component damage.
Space Requirements
Approximately 72 x 30 inches (183 x 76 cm) of bench space is required for the MultiTek® System in
the horizontal configuration. The bench space requirement for the vertical configuration is 43 x 30
inches (109 x 76 cm) or 60 x 30 inches (152 x 76 cm) with the 734 gas box. The bench should be
capable of supporting at least 350 pounds (159 kg) which is sufficient supporting weight required for
a full system configuration. Adequate air space should be provided around the instrument.
Ventilation/Flammables
Reasonable ventilation associated with a “typical” modern laboratory environment is normally
acceptable. Do not allow heated/cooled drafts of air to vent onto the MultiTek® System.
WARNING
Furnace operates at a temperature in excess of 1000ºC and can serve as an ignition source.
Ethernet Connection
One 10/100 Ethernet connection using a standard RJ-45 jack, with access to a local intranet, should
be available for each instrument and PC.
NOTE
Adequate safeguards must be set up by network administrators to control access to this intranet to
prevent unauthorized or unwanted access to the instrument and/or PC running Antek MultiTek® Software.

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Electrical Requirements
Electrical Power
The Antek MultiTek® instrument and PC utilize stable 115 VAC, 50/60 Hz or 230 VAC, 50/60
Hz. A 15 amp circuit is required for 115 VAC and an 8 amp for 230 VAC. A good ground is
necessary for each component. The basic system requires five (5) electrical outlets plus those
required for sample introduction accessories. Check “Optional Equipment” for additional electrical
requirements.
WARNING
A poor ground may present a severe shock hazard.
115 VAC 230 VAC Outlets
Accessory Amperes Amperes Required
Model 734 2.0 1.0 1
Model 735 1.0 0.5 1
Model 737 (230 VAC only) 12.0 1
Model 748 1.0 0.5 1
Model 740 1.0 0.5 1
Model 758 1.4 0.7 1
NOTE
Some accessories, such as the Model 737-M Temperature Programmable Inlet only support a 230 VAC
operation.
The mains supply voltage fluctuations are not to exceed 10 percent of the nominal supply voltage.
WARNING
A poor ground may present a severe shock hazard. If a replacement power plug is used, confirm that
wiring is correct and that the plug is rated to carry the maximum current.

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Gas Requirements
The Antek MultiTek® system will perform best when supplied with high quality gases. Gas
suppliers have different grades and designations for gas. Care should be taken when choosing the
gases to be used.
WARNING
High-pressure gases should be handled with extreme care. Ensure that all relevant safety precautions
are carefully followed and all gas lines, regulators, gas purifiers, etc. are specified for the intended use.
CAUTION
When using a liquid leak detector, care should be taken not to wet any electrical/electronic components
or contaminate the analytical flow system. Severe component damage or errant results may occur.
Gas Quality
Chromatographic (high purity) grade argon (or helium) and chromatographic (high purity) grade
oxygen are required to operate the Antek MultiTek® System. Gas streams must be regulated at 40
psig and in-line gas dryers are suggested.
Oxygen ............................ 3.0 bar (40 psig), 99.75%, (minimum) maximum moisture 5 ppm
Argon*............................. 3.0 bar (40 psig), 99.99%, (minimum) maximum moisture 5 ppm
Instrument Air ................ 3.0 bar (40 psig), 99.75%, (minimum) maximum moisture 5 ppm
maximum CO2 400 ppm
maximum THC1 10 ppm
*Helium may be substituted for Argon as a carrier gas. (Software adjustment is required)
Gas Supply
All supply gases should be delivered through clean, dry chromatographic grade tubing. Various
solvents may be used provided they are capable of dissolving oils or greases. All solvents should
be reagent grade or better.
All national pipe thread (NPT) connections or pipe threaded 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 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.
Figures 1-1a through Figure 1-4 illustrates a general flow diagram for the supply gases to an Antek
MultiTek® system.

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Figure 1-1a: General Gas Supply Flow Diagrams (Nitrogen-Sulfur-IC)

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Figure 1-1b: General Gas Supply Flow Diagrams (Nitrogen - Sulfur)

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Figure 1-2: General Gas Supply Flow Diagrams (Sulfur)

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Figure 1-3: General Gas Supply Flow Diagrams (Nitrogen)

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Figure 1-4: General Gas Supply Flow Diagrams (LLS-Low Level Sulfur)

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Rear Panel
Refer to Figures 1-5 and 1-6 to locate interface connections on the rear of the MultiTek® system.
Figure 1-5: Fitting Locations – Horizontal MultiTek®
Carrier Loop
734 Inlet
Carrier Gas
Inlet O2 Inlet
System
Vent

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Figure 1-6: Fitting Locations – Vertical MultiTek®
734 Inlet
Carrier Loop
Carrier Gas O2 Inlet

Inlet
System
Vent

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SECTION 2
INSTALLATION
Introduction
The Antek MultiTek® software package provides computer controlled timed events to control sample
introduction devices, auto samplers, and sample valves. It also controls all flows, high voltage settings,
data collection, and detector settings. The Antek MultiTek® Software is specific to the N-S detection;
a separate Antek MultiTek® IC Sampler Control Software is used for the MultiTek® IC which will be
discussed later in the manual.
Additionally, there is the Antek MultiTek® Software 21 CFR part11 Edition that provides support for
those who must comply with 21 CFR part11 requirements for record keeping and security. Refer to
the Antek MultiTek® Software 21 CFR part11 Addendum for details.
MultiTek® software automatically determines which peripherals have been employed. This is a
dedicated software package capable of simultaneously integrating the peak areas of Nitrogen and
Sulfur detector signals.
Hardware Installation
Drain and Vent
Install the drain and vent. Waste fluids can be collected in one single container or directly plumbed to
a drain.
Gas Connections
Using pre-cleaned (for GC applications) copper gas lines compatible with the MultiTek® system, connect
the supply gases to the proper gas inlet fittings. Refer to Figures 1a thru 4 that illustrate the general flow for
the gases supplied to the MultiTek®.
After all gas fittings have been connected, they should be carefully checked for leaks. Procedures later in
this section should be followed to determine the integrity of the gas connections in the flow paths.
Compression Fittings
Teflon® or metal tubing: Insert tubing through the nut. Slide the ferrule over the tubing. Insert tubing
with the ferrule until the tubing bottoms in the fitting. Secure the nut finger-tight plus one turn with a
wrench (Figure 2-1a).
Figure 2-1a: Compression Fittings

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Glass tubing: Position ¼” nut first, then slide the Teflon® ferrule over glass arm. Insert male fitting
until glass arm bottoms out in the base of male fitting, then secure finger-tight. Back out glass arm tip
1 mm so that bevel inside male fitting does not chip glass arm tip. Tighten until male nut threads are
nearly covered (Figure 2-1b). Do not over tighten.
Figure 2-1b: Glass to Metal Fitting

Step 1 Step 3
1 mm gap
Step 2 Step 4
Optional Equipment
MultiTek® operates many of its peripherals directly. The software is designed to recognize optional
equipment connected to the MultiTek®, and based on this, customize dialog and standby requirements.
A list of optional accessories is included in Section 1. Additional information concerning optional
equipment is also available in other manuals or addenda to this manual.
Before installing accessory or optional equipment or proceeding to the primary testing section of the
installation procedure, become familiar with the locations and various features of the MultiTek®.
Pyrotube Installation/Configuration
The MultiTek® instrument utilizes several variations of pyrotubes. Only properly trained operators
should perform the installation and or configuration of any pyrotube. These pyrotubes are intended for
the analysis of solid, liquid, and gas samples. For systematic procedures for the installation and or
configuration of a pyrotube, please refer to the accessory manuals or addenda.
PC Installation/Configuration
PC configuration
To avoid interruptions to the MultiTek® software operations, the Windows OS must be configured in
the following way:
From the Control panel, go to System properties and enable the Automatic Updates by checking
“Notify me but don’t automatically download or install them” (Figure 2-2), and then click the Apply
button.

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Figure 2-2: Automatic Updates
Open Windows Firewall, tab to Exceptions (Figure 2-3).
Figure 2-3: Windows Firewall
Click Add Port… button, type the name and Port number as shown in Figure 2-4a, then click OK.
Next click Add Port… button again, type the name and Port number as shown in Figure 2-4b, then
click OK.

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Figures 2-4a: Add Port… Figure 2-4b: Add Port…
Disable the Screen saver, change power management scheme to “Always on”, and configure the
monitor and hard drives to never turn off or go to system standby (Figure 2-5).
Figure 2-5: Display Properties

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MultiTek® Software Installation

Installing the Software
Insert the Antek MultiTek® Software media into your PC. At the opening screen, select the software
to be installed (Figure 2-6). If the opening screen does not appear, run CD_Start.exe from the media
root directory. If you are installing the Antek MultiTek® Software 21 CFR part 11 Edition, refer to the
Antek MultiTek® Software 21 CFR part 11 Addendum for details – see the opening screens below.
Figure 2-6: MultiTek® Software Installation Opening Screen
Standard Edition 21 CFR part 11 Edition
Adobe® Reader
If Adobe® Reader is not installed on your PC, it can be installed from the MultiTek® Software media
(Figure 2-7). Adobe® Reader is needed to open .pdf documents including this manual.
Figure 2-7: MultiTek® Software CD Screen Adobe Reader

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Antek MultiTek® Software may be installed in a local computer or on a network system. The
MultiTek® instrument itself has a limited user interface of four LEDs and a Start push button on the
front panel. Multiple MultiTek® analyzers may be run from a single PC – four is the recommended
maximum using a minimum system configuration PC. The system block diagram is illustrated below
in Figure 2-8.
MultiTek® default network configuration utilizes a router to assign an IP address to the instrument.
For this a router with DHCP enabled is required. With Antek MultiTek® Software v2.0.0.0, and later,
a static IP address may be set in the MultiTek® after initial setup. A static IP address allows
connection to the instrument through a network switch, or directly from the PC’s Ethernet port as long
as the PC is on the same subnet as the instrument (Appendix C).
NOTE
For initial installation, a network router is required to assign an IP address to each MultiTek® instrument.
DHCP must be enabled in the router. After initial setup is complete, a static IP address and subnet can be set.
If a static IP address is used, both the MultiTek® and PC must be on the same sub network.
NOTE
The router/switch/PC must be powered on and running before the MultiTek® is powered on.
Figure 2-8: System Block Diagram
MultiTek® Instrument MultiTek® Instrument MultiTek® Instrument

(No. 1) (No. 2) (No. n)
Router*
Windows PC
(MultiTek® Software)
* A switch can be used in place of a router if a static IP address is set in the instrument(s).
The Windows user must have administrator rights in order to be able to install the software.
Additional requirements server: Network 100 MBit/s, stable and permanent monitor with a minimum
screen resolution 1024 x 768.

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NOTE
MultiTek® instrument software uses a database management system to store data. Microsoft SQL Server
2005 must be installed and configured before running the software. MS SQL Server 2005 has a variety of
editions to meet different user’s need. Different editions of SQL Server 2005 have different hardware and
software requirements for installation. Please refer to this website for the requirements:
http://msdn.microsoft.com/en-us/library/ms143506(SQL.90).aspx
NOTE
Microsoft SQL Server 2005 manages memory for each instance. Different editions may utilize different
memory management architectures, and therefore, different database memory capacity. By using AWE
(Address Windowing Extension) and the Locked Pages in Memory privilege, you can provide the maximum
amount of memory to the SQL Server Database Engine. Please refer to the website below for the maximum
memory that each SQL server edition can support:
http://msdn.microsoft.com/en-us/library/ms187499(SQL.90).aspx
NOTE
If MS SQL Server 2005 Express edition is used, SQL Server Management Studio Express 2005 must be installed
separately. Installing other editions of SQL Server will automatically install the SQL Server Management
Studio. While MS SQL server 2005 Express edition is free, it has 4GB database capacity and many other
limitations. It is customer’s choice and responsibility to select the appropriate edition of SQL Server 2005 that
meets their needs.
If you have a previous version of the MultiTek® Software, it will install without loss of data and it updates
the existing database. However, it is recommended (and good practice) to back up the database prior to
installing the new version of software. See Section 6 “Backing up the Database”.
NOTE
In previous versions of the MultiTek® software installation package, prerequisites were not installed
automatically.
MultiTek® software installation begins with installing the necessary prerequisites. The necessary items,
.NET 3.5 and SQL Server 2005 will be installed automatically. The system may request a restart.
To install Antek MultiTek® software, click MultiTek® Software button from opening screen (Figure
2-9) and follow the installation process.

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Figure 2-9: Antek MultiTek® Software
For the version of software to be installed, the following screen will appear indicating the minimum
version of MultiTek® firmware required (Figure 2-10).
Figure 2-10: Antek MultiTek® Software Installation
Click the Next button (Figure 2-11).

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Figure 2-11: Antek MultiTek® Setup Screen
After reading the Software License Agreement, check the I Agree button and click Next to proceed
(Figure 2-12).
Click the Next button (Figure 2-13).

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Click the Next button. (Figure 2-14.)
The server name selected has to be identical to the initial server selected during the Microsoft SQL
server software installation, which will be used by MultiTek® software. (The server name can also be
copied from “Microsoft SQL Server Management Studio” start screen and pasted in this field).
Select the “Windows Authentication” mode then click OK (Figure 2-15).
Figure 2-15: Database Login

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NOTE
If the database has been installed, the following dialog window will appear. If the database has not been
installed, this window will not appear. (Figure 2-16.)
Figure 2-16: Database Screen
Click OK to start installation and wait until finished. After installation is complete, click the Close
button.
The software installation can be verified from “Start -> All programs -> Antek -> MultiTek folder”
(Figure 2-17).
Figure 2-17: MultiTek® Folder Location
The installation program will place a shortcut to the software on the desktop to launch the Antek MultiTek®
software.

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SQL Server Management Studio Installation

To install SQL Server Management Studio Express, click SQL Mgmt Studio button from opening
screen and follow the installation process (Figure 2-18).
Figure 2-18: SQL Management Studio Introduction Screen
Click Next button until the installation is complete.
Configuring SQL Server
After SQL server is installed, its properties need to be configured.
Open Microsoft SQL Server Management Studio; connect to the server where the MultiTek® database
will be installed (Figure 2-19).
Figure 2-19: Connect to Server Screen
Right click the Server name, select the correct SQL server instance present, and then click Properties
from the list.
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Figure 2-20: Microsoft Server Management Studio
Click Security from Select a page list in Server Properties window; click SQL Server and Windows
Authentication mode radio button for Server authentication, then click the OK button (Figure 2-21).
Figure 2-21: Server Properties
Click Finish (Figure 2-22).

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Figure 2-22: SQL Server Setup Completion
Click Start \ All Programs \ Microsoft SQL Server 2005 \ Configuration Tools \ SQL Server
Configuration Manager to launch the manager. Click SQL Server 2005 Services in the left pan, then in
right pan right click the server MultiTek® software will be using (SQL Server SQLEXPRESS for this
case), click properties (Figure 2-23).
Figure 2-23: SQL Server Configuration Manager
Tab on Log on, select Local System from Built-in account dropdown list, then click OK button
(Figure 2-24).

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Figure 2-24: SQL Server Account Login
Click Yes when this dialog window pops up (Figure 2-25).
Figure 2-25: SQL Account Confirmation Change
After software installation is complete, reboot your computer.

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MultiTek® IC Sampler Control Software Installation

MultiTek® IC Sampler Control Software controls the function of the IC module of MultiTek®
instrument. The MultiTek® IC module prepares samples for ion chromatographic (IC) analysis on
either a Dionex ICS2000/ICS2100 IC system or a Metrohm 881 Compact Pro IC system. The IC
analyzers run under their own software: Chromeleon for the Dionex; MagIC for the Metrohm. The
MultiTek® Software and the MultiTek® IC Sampler Control software can run simultaneously on the
PC. The software packages for the IC analyzers communicate using a set of communications signals
specific to the IC system in use. Physically, both the MultiTek® and IC analyzer must be connected to
the PC by Ethernet and USB cables respectively. The MultiTek® and IC analyzers must be connected
to each other by a vender specific IC input cable for signal synchronization. No data from the IC
analyzer is stored by the MultiTek®. All sample information and analysis results are stored by the IC
analyzer software. Unless entered into the IC sample table, generally in a comments section, the IC
system does not store any MultiTek® parameters used for sample preparation.
NOTE
DHCP must be enabled in the router. After initial setup is complete, a static IP address and subnet can be set
using Antek MultiTek® Software (Appendix C).
NOTE
The router must be powered on before the MultiTek® is powered on.
Figure 2-26: Block Diagram of the System

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To install the software, click IC Control Software button from opening screen and follow the
installation process (Figure 2-27).
NOTE
To install this software Microsoft .NET framework 3.5 must be pre-installed. Click the .NET 3.5 button from
opening screen and follow the installation process to finish the installation. After software installation is
complete, reboot your computer.
Figure 2-27: IC Control Software
For the version of software to be installed, the following screen will appear indicating the minimum
version of MultiTek® firmware required (Figure 2-28).
Figure 2-28: IC Control Software Required Firmware Version

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Click Next button (Figure 2-29).
Figure 2-29: IC Control Software Setup
Figure 2-30: IC Control Software Folder Selection
Figure 2-31: IC Control Software Folder Confirmation

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Click Close button to finish ICSamplerControl software installation (Figure 2-32).
Figure 2-32: IC Control Software Completion
Figure 2-33: MultiTek® IC Sampler Control Software folder location
Vendor Specific IC Analyzer Software Installation
For information on installation of the Dionex or Metrohm IC analyzers, please refer to the specific
manufactures’ manual.

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Power-up, Registration and Configuration

Before proceeding with the primary function testing of the MultiTek®, it will be necessary for the
MultiTek® Software to be running and communicating with the instrument.
Connection and Power-up

The MultiTek® Analyzer is PC controlled; default connection is via a network router using dynamic IP
addressing. For initial setup, the instrument, router and PC must be connected as shown in the System
Block Diagram (Figure 2-8). Static IP addressing is also supported, but can only be done once the initial
setup has been completed (Appendix C). MultiTek® Software must be running on a Windows PC in
order to operate the MultiTek® analyzer. All the settings and results data are stored on the PC.
NOTE
NOTE
WARNING
The Antek MultiTek® software and hardware must be installed, and Sections 2, 3, 4 (N-S) and/or 5
(IC) of this manual reviewed and understood.
CAUTION
Ensure that the correct power cords are used and plugged into the appropriate outlets.
CAUTION
Become familiar with the location and use of all controls and software functions and carefully read all
instructions before attempting to operate any portion of the system.
NOTE
Ensure that installation check list is complete, (Primary Testing Checklist in this sub-section).
Turn on the computer and monitor power switches. Make sure all accessory jumpers are plugged into
the rear panel of the MultiTek® instrument, and cables are securely connected between the instrument
and accessories. Turn on the accessories and wait until they are running and stabilized. Then apply
power to the MultiTek® electronics and combustion furnace by activating the two power switches on the
rear of the MultiTek®. Wait approximately 15 seconds until the State LED on the instrument front panel
turns to green, and then launch Antek MultiTek® Software from computer.

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IMPORTANT
All accessory jumpers must be plugged into the rear panel of instrument prior to applying power to
the MultiTek®.
Instrument Registration and Logon

When the MultiTek® software logon screen appears, enter the user name and password (default: admin;
password). Select the instrument and click on Logon (Figure 2-35). New or previously unregistered
instruments must first be registered. Click the Register button to register the instrument (Figure 2-34).
For new instruments and installations, when the pop-up “Do you wish to use any existing instrument
database?” appears, select No (Figure 2-34).
Figure 2-34: Register Instrument
Once the MultiTek® has been registered, you may then logon to claim the instrument (Figure 2-35) or
configure the IP address if changing the IP addressing (See Appendix C).
IMPORTANT
An instrument’s name and serial number are stored in non-volatile memory on the instrument’s processor
board. If the processor board is replaced, the name and serial number will revert to default values. Also the
instrument will not reconnect to its database, including methods and instrument parameter settings, unless
restored during the Registration process.
If the processor board has been replaced, follow the instructions in Section 3, Connect to Analyzer, to
restore the instrument name and serial number, and reconnect to its database.

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Figure 2-35: Instrument Logon
Configure IP Address
MultiTek® IP Address Configuration

The MultiTek® Analyzer is PC controlled; default connection is via a network router using dynamic IP
Block Diagram (Figure 2-8). Static IP addressing is also supported, but can only be done once the initial
setup has been completed – refer to Appendix C. MultiTek® Software must be running on a Windows
PC in order to operate the MultiTek® analyzer. All the settings and results data are stored on the PC.
NOTE
MultiTek® Main Screen

After an analyzer has been claimed, the software will go to the main analyzer window (Figure 2-36).
Depending on the configuration of the instrument, data for Nitrogen, Sulfur or both (neither if the
instrument is IC-only) will be displayed.

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Figure 2-36: Main Screen
Configuration of the MultiTek® Analyzer

To configure the analyzer, click Instrument Parameters on the “Setup” menu. Instrument Parameters
are saved in multiple versions starting from version 1. However, only one version may be applied to the
instrument at a time. The “Currently applied” check box indicates the current version that has been
written to the instrument (Figure 2-37). This section is for initial setup and installation. Refer to Section
3 for more information regarding configuration of MultiTek®.
The analyzer name and serial number are displayed in the “Identification” tab of “Instrument
Parameters” screen (Figure 2-37). IT-Administrator and Service level user can modify both;
Administrator level users can only modify instrument name; User level has no authority to modify
either.

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Figure 2-37: Instrument Parameters – Identification

Currently applied version check box
Common Tab
Once a version is saved it can no longer be changed, however any created version may be sent to the
instrument by clicking on the Write to instrument button.
Configurations and Instrument Parameters are displayed in the “Common” tab (Figure 2-38). Choosing
“User defined” allows all components to be enabled or disabled as well as modification of their set-
points and tolerance ranges.
To make changes to the current version and apply it to the instrument:

1. Click Edit button on the toolbar (Figure 2-38);
2. Modify set points and other parameters;
3. Click Save button on the toolbar to save the modified parameters to a new version and
automatically write them to the instrument (Figure 2-39).
4. Click Close button to close the “Instrument Parameters” window if done.
NOTE
If you select Close instead of Save, a dialog box will ask if you want to save a new version. Clicking on “Yes” will
save the settings in a new version, but will not write the new version to the instrument.
To apply the settings of a previously saved version to the instrument:

1. Select the desired version from the “Version” list on the toolbar (Figure 2-38);
2. Click Write to instrument button to apply the selected version to the instrument;
3. Click Close button to close the “Instrument Parameters” window when done.

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Figure 2-38: Instrument Parameters

Selected Version Edit Save
Write to instrument button Setpoint boxes – enter new values

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Figure 2-39: Saving Instrument Parameters and Writing to Instrument
Editing Gas Flow Settings
Before setting the gas flow controllers (GFC’s) on the MultiTek®, it is important to note that there are
general guidelines for flows. These guidelines can vary from application to application. If you are
uncertain about proper flows for your system, please refer to Section 4 of this manual or contact your
local PAC representative.
NOTE
The following procedures regarding gas flows and pressures are used to check initial instrument
performance and ensure the sample flow path and internal gas supply lines are leak free to a
pressure of 2 – 4 psi (~14 – 28 kPa).
MultiTek® Software and Firmware automatically detect the GFC’s present in your system. GFC’s not
detected are dimmed in the Hardware setting screen; up to six gas flow controllers can be present.
Confirm that all gas flow controllers present in your system are indicated.
To set the flows for the various portions of the flow path of the MultiTek®, click the Edit button at the
top of the Instrument Parameters, Common panel, enter the new value in the Setpoint field to the
right of the GFC to be changed (Figure 2-38). When complete, click the Save Button, then click Yes to
save the new version and automatically write it to the instrument (Figure 2-39), then click OK. See
GFC5 & GFC6 Gas Flow Adjustment later in this section for information regarding adjustment of
carrier gas flow to the 734 Gas Box, or gas flows for other applications using GFCs 5 & 6.

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Pressure / Leak Tests
The following section describes the procedures needed to complete successful gas supply and flow path
leak check.
CAUTION
Carefully follow all instruction and guidelines in the following leak check procedures. Failure to do so may
cause severe system component damage.
WARNING
Do not exceed recommended pressure. If higher pressure is used, severe and irreparable damage may
be done to fragile system components.
CAUTION
While performing the following leak check procedure, do not over tighten fittings. Over-tightening can
cause restrictions, which will affect instrument performance. If ferrules need replacement the fittings
should be tightened according to the guidelines described in the beginning of Section 2 of this manual.
Gas Supply to Instrument Leak Check
1. Activate the Instrument Parameters, Common screen as discussed in Power-up portion of the
Functional Test sub-section.
WARNING
Do not apply greater than 60 psi for this leak check procedure.
2. Click the Edit button. Enter “0” in the Setpoint box for GFC1 (Argon). This sets the Argon flow to
a value of 0 mL/min. Also, set GFC’s for Pyro O2, Ozone O2 (if present) and Carrier O2, (GFC’s 2-
4), and any other GFC’s present to 0 mL/min. Click the Save button, then click Yes to save new
version and automatically write it to the instrument (Figure 2-41), then click OK.
3. Apply pressure (40 – 60 psi) to the instrument by turning on the gases at the cylinder regulators.
Note the pressure applied and turn off the cylinder valve and ensure that the pressure does not drop.
4. If the pressure does not drop, then there is no leak between the regulators and the GFC inlet
manifold in the MultiTek®. This will not apply if there are other instruments being used on the same
supply or the regulator is not properly secured to the cylinder. Repeat this process for all supply
gases. If the pressure drops, check all the fittings between the gas supply outlet and the GFCs, as
shown in Figure 2-40, including the connections between the GFC Input Manifold and GFCs.
Repeat this procedure if required.

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Figure 2-40: Gas Supply to GFC Leak Check Points
Instrument Leak Check Preparations

A successful flow path leak check can only be accomplished if the instrument gas plumbing routes are
identified and understood. Use the flow path diagrams shown in Section 1 to identify the tubing location
and flow characteristics of the instrument being tested. Prepare the instrument for the low pressure leak
check as follows.
Click the Edit button (Figure 2-38). Enter “0” in the Setpoint box for GFC1 (Argon/Helium). This sets
the Argon/Helium flow to a value of 0 mL/min. Set the Carrier O2 to 300 mL/min (GFC4); set all other
GFC’s present to 0 mL/min. Click the Save button, then click Yes to save new version and
automatically write it to the instrument (Figure 2-39), then click OK.
After the new settings are sent to the MultiTek® for each GFC, flow controlling begins. The screen
updates once per second, so there may appear to be a delay in the changing of the flows.
Adjust the oxygen supply pressure to ~ 5 psi (34.5 kPa) either at the cylinder regulator or with an in-line
pressure regulator. This is a low enough pressure that it should not damage the instrument. If this
pressure is exceeded, the Tygon® tubing on the pressure sensor may dislodge. This often occurs if the
regulators are defective.
Instrument Leak Check (Complete Flow Path)

Upon completion of the installation of the pyrotube and optional equipment, it is necessary to confirm
the MultiTek® is leak free. Prepare the MultiTek® for the Low Pressure Leak Check as described in the
Instrument Leak Check Preparations sub-section.
CAUTION
Do not exceed recommended pressure of 5 psi (34.5 kPa). If higher pressure is used, severe damage can
be done to system components.

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NOTE
All gas flows will be shut down by the MultiTek® firmware whenever system pressure exceeds 40 kPa (5.8
psi). Go to the Common panel in Instrument Parameters. Select the desired version then click on “Write
to Instrument” to restart the gas flows.
1. Locate the final exit point (vent) of the flow path gases. Certain configurations may have more than
one exit point. Flow diagrams in Section 1 (Figures 1-1a – 1-4) and later in this section can give
guidance. Most final vent points are located on the MultiTek® rear panel. See Figure 2-41.
Figure 2-41: MultiTek® Horizontal Rear Panel
2. Open the Instrument Status panel (Figure 2-42). Monitor the Carrier O2 (GFC4) read-out. The
actual values will drop below ten if no leaks are present in the system; the system pressure will also
rise above 20 kPa. This may take a few minutes. When the pressure inside the instrument equals the
supply pressure, there should be no flow in the instrument. There will be flow when a leak is present
because gas is still flowing into the instrument to equalize the pressure left by the leak.

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Figure 2-42: Monitoring GFC Flow Rates

System Pressure Carrier O2 Flow Rate
3. If there is a leak present in the system, a leak check must first be performed on the membrane dryer
to ensure that it is not leaking. Locate and remove the exit fitting on the membrane dryer. Hold
your finger over the exit to seal. Monitor GFC4, Carrier O2, flow rate. The actual values will drop
below ten if no leaks are present in the system; the system pressure will also rise above 20 kPa. If
the values do not drop below ten, there is a leak in the membrane dryer. Replace the membrane
dryer. Repeat the procedure for the new dryer.
4. If a leak is present, proceed to the flow path segment leak test procedures that follow.
Furnace Section Leak Check

Most leaks occur in the furnace section, particularly the pyrotube. This is primarily a result of the heat
and sample introduction process that occurs during sample analysis. Leaks can also result from
improper pyrotube installation, compression of heat sensitive (plastic) ferrules used to attach tubing to
the pyrotube, and other factors related to routine analytical practices. When a leak is detected using the
complete system leak check procedure previously discussed in this sub-section, it is helpful to divide the
overall flow path into two segments and investigate accordingly. Unless there has been some
maintenance or other activity associated with the detector section of the flow path, it is recommended
that the investigation begin in the furnace area. Leak-check the furnace section flow path as follows.

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WARNING
Do not exceed the recommended pressure of 5 psi (34.5 kPa). If higher pressure is used, severe and
irreparable damage may be done to fragile system components.
NOTE
psi). Go to the Common panel in Instrument Parameters. Select the desired version then click “Write to
Instrument” to restart the gas flows.
CAUTION
Furnace temperatures are extreme, cooling of the furnace before proceeding with this leak check
procedure is recommended.
1. Locate the exit point of the flow path gases from the pyrotube. Certain configurations may have
more than one exit point. The entrance or exit connections to the membrane dryer can be convenient.
Flow diagrams in Section 1 (Figures 1-1a – 1-4) and later in this section can give guidance. See
Figure 2-43.
Figure 2-43: Furnace Flow Path
2. Plug the flow path exit vent (or vents) from the pyrotube at the membrane dryer.

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4. If a leak is present, investigate for loose fittings, cracked pyrotube and other leak sources in the
furnace section flow path shown in Figure 2-43. Repeat furnace section leak test until leak free.
5. Reassemble the flow path and repeat the Instrument Leak Check (Complete Flow Path) procedure to
confirm the overall system is leak free. If there is still a leak present, proceed to the next part:
Detector Section Leak Check Procedure.
Detector Section Leak Check Procedure

Leaks can occur in the detector section, particularly the fittings to the reaction chamber. This often is a
result of recent maintenance. Leaks can also result from improper tubing installation, compression of
reaction chamber ferrules and other factors related routine analytical practices. When a leak is detected
using the complete system leak check procedure previously discussed in this sub-section, it is helpful to
divide the overall flow path into two segments and investigate accordingly. If no gas leak is found in the
furnace section of the flow path (above), the leak investigation can then continue in the detector area.
Leak-check the detector section flow path as follows:
CAUTION
Do not exceed recommended pressure of 5 psi. If higher pressure is used, severe and irreparable damage
may be done to fragile system components.
NOTE
psi). Go to the Common panel in Instrument Parameters select the desired version then click on “Write to
Instrument” to restart the gas flows after the pressure drops back to normal.
WARNING
Beware of electrical shock hazards present in the detector section.
1. Locate the exit point of the flow path gases from the detector section. Certain configurations may
have more than one exit point. Flow diagrams in Section 1 can give guidance. See Figures 1-1a
through 1-4.
2. Plug the flow path exit vent (or vents) at the detector exit, scrubber or vent.
4. If the flow rate does not drop, a leak is present. Investigate for loose fittings, cracked tubing and
other leak sources in the detector section flow path shown in Figures 2-43 and repeat detector section
leak test until leak free. Reassemble the flow path and repeat the complete flow path leak test
procedure, previously discussed in this sub-section, to confirm the overall system is leak free.

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Gas Flow Controller (GFC) Testing

This section provides the procedures needed to confirm proper installation and basic GFC function and
gas control features of the Antek MultiTek®.
WARNING
High pressure gases should be handled with extreme care. Ensure that all relevant safety precautions
are carefully followed and all gas lines, regulators, gas purifiers, etc. are specified for the intended use.
WARNING
When analyzing any potentially hazardous materials (i.e. irritants, corrosives, carcinogens, etc.), ensure
that all relevant safety precautions have been carefully followed and possibly ventilate the area of the
analyzer with fresh air, an exhaust fan, or locate the entire analyzer inside a fume hood.
CAUTION
After the system pressure setpoint and tolerance are entered, the gas flow settings must support the
system pressure within the setpoint range. If the system pressure varies outside the setpoint range, a
system warning will occur until the problem is corrected.
Argon
1. Activate the Instrument Parameters, Common screen as discussed in Power-up portion of the
Functional Test sub-section.
WARNING
Do not apply greater than 60 psi for this leak check procedure.
Argon is normally used as the major portion of the carrier gas used to sweep the volatilized sample from
the inlet area into the high temperature (oxidative) portion of the pyrotube. Normally, 120 to 140
mL/min argon flow is required to provide an even sweep of the sample inlet.
Helium can be substituted for Argon if that is the gas that is available (see Changing Carrier Gas to
Argon or Helium). From the Antek MultiTek® Main Screen, activate the Instrument Parameters,
Common panel (Figure 2-38) and click the Edit button.
NOTE
For certain applications, Argon may not be necessary or desirable. In these cases, proceed to the next
sub-section - Carrier Oxygen.
2. Enter “0” in the Setpoint box for GFC1 (Argon). This sets the Argon flow to a value of 0 mL/min.
Also, set GFC’s for Pyro O2, Ozone O2, Carrier O2 (if present), (GFC’s 2-4), and any other GFC’s
present to 0 mL/min. Click the Save button, then click Yes to save new version and automatically
write it to the instrument (Figure 2-39), then click OK.

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®
The normal argon pressure level to the MultiTek is 3.0 bar (40 psig). When using certain accessories,
the argon line pressure may need to be increased to 4.0 bar (60 psig).
CAUTION
Unless specifically stated, the supply pressure of gases used with the ANTEK MultiTek® system should not
exceed 4.0 bar (60 psig).
3. Connect a bubble flow meter or some other gas flow measurement device to the final system vent
fitting indicated in Figure 2-41. Some flow paths may have multiple vents.
4. Adjust the argon flow to the desired rate by entering the value into the Setpoint box as described in
Step 1; monitor the Actual box to ensure the flow rate is correct. The default flow rate is 130
mL/min. Optimum argon flow rates for specific application(s) will be determined by experience.
5. Confirm that the indicated flow is delivered by measuring with a gas flow measurement device.
Carrier Oxygen
WARNING
Oxygen is a strong oxidizer and greatly accelerates combustion.
Oxygen is normally mixed with the argon carrier to improve the volatilization and combustion
characteristics of the sample. In certain, rare solid applications and with certain types of samples,
oxygen may be completely substituted for the Argon carrier (i.e., aqueous samples, soil samples, etc.).
Normally, 10 to 40 mL/min Carrier Oxygen flow is required when mixed with argon. From the Antek
MultiTek® Main Screen, activate the Instrument Parameters, Common panel (Figure 2-38) and click
the Edit button.
WARNING
Extreme care should be taken when using Carrier Oxygen in the analysis of volatile, flammable samples.
1. Set the Carrier Oxygen to 0.0 mL/min. Click the Edit button. Enter “0” in the Setpoint box for
GFC1 (Argon). Also, set GFCs for Pyro O2, Ozone O2 (if present), GFC’s 2&3, and any other GFCs
2. Set the supply pressure of the oxygen to the recommended level as outlined in Section 2. The
normal oxygen pressure level is 3.0 bar (40 psig).
CAUTION
3. Connect a bubble flow meter or some other gas flow measurement device to the system vent fitting
indicated in Figures 2-41 and Figures 1-1a – 1-4.

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4. Adjust the Carrier O2 flow to the desired rate by entering the value into the Setpoint box as
described in Step 1; monitor the Actual box to ensure the flow rate is correct. Default flow rate is
25 mL/min. Optimum oxygen flow rates for specific application(s) will be determined by
experience.
5. Confirm that the indicated flow is delivered by measurement with a gas flow measurement device.
Pyro Oxygen
WARNING
This is the main oxygen supply to the high temperature, oxidative portion of the pyrotube. Typically,
400 to 450 mL/min Pyro oxygen flow is required to maintain a safe excess of oxygen and ensure
complete oxidation of the sample. From the Antek MultiTek® Main Screen, activate the Instrument
Parameters, Common panel (Figure 2-38) and click the Edit button.
CAUTION
Do not attempt to analyze samples without an adequate supply of oxygen to the oxidative zone. This may
result in incomplete combustion and the formation of fine carbon particles (coking). The coking may
cause irreversible damage to the membrane dryer and may also cause reduction or complete loss of
sensitivity by the detector(s).
1. Set the Pyro Oxygen to 0.0 mL/min. Click the Edit button. Enter “0” in the Setpoint box for GFC2
(Pyro O2). Also set GFCs for Ozone O2 (if present), Carrier O2, GFCs 3&4, and any other GFCs
2. Set the supply pressure of the oxygen to the recommended level as outlined in Section 2. The normal
oxygen pressure level is 4.0 bar (60 psig).
CAUTION
indicated in Figure 2-41 and 1-1a – 1-4. Some flow paths may have multiple vents.
4. Adjust the Pyro O2 flow to the desired rate by entering the value into the Setpoint box as described
in Step 1; monitor the Actual box to ensure the flow rate is correct. Default flow rate is 450
mL/min. Optimum oxygen flow rates for specific application(s) will be determined by experience.
5. Confirm that the indicated flow is delivered by measurement with the gas flow measurement device.

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Ozone Oxygen
WARNING
WARNING
Do not turn on ozone generator without oxygen flow through ozone cell.
This is the oxygen supply to the ozone generator. This control is operational for systems containing a
nitrogen detector (e.g., MultiTek® N and MultiTek® NS). Optimum flow for the ozone oxygen is 20 - 40
mL/min. From the Antek MultiTek® Main Screen, activate the Instrument Parameters, Common
panel (Figure 2-38) and click the Edit button.
WARNING
Do not apply oxygen to the ozone generator until all gas connections have been completed and leak
checked. If gas connections are not complete and leak free, ozone may leak out and present a health
hazard.
CAUTION
It may be desirable to maintain a very small flow of oxygen (approximately 5 mL/min) across the ozone
generator when the system is not in use. This will prevent the condensation of moisture in the generator
cell and possible cell damage. Ozone generator must have gas flow before power-up.
1. Set the Ozone Oxygen to 0 mL/min. Click the Edit button. Enter “0” in the Setpoint box for GFC2
(Pyro O2). Also set GFC’s for Pryo O2, Carrier O2, GFC’s 2&4, and any other GFC’s present to 0
mL/min. Click the Save button, then click Yes to save new version and automatically write it to the
instrument (Figure 2-39), then click OK.
2. Set the supply pressure of the oxygen to the recommended level as outlined in Section 2. The
normal oxygen pressure level to the MultiTek® is 3.0 bar (40 psig).
CAUTION
indicated in Figure 2-41 and 1-1a – 1-4. Some flow paths may have multiple vents.
4. Adjust the Ozone O2 flow to the desired rate by entering the value into the Setpoint box as described
in Step 1; monitor the Actual box to ensure the flow rate is correct. Default flow rate is 35 mL/min.
Optimum oxygen flow rates for specific application(s) will be determined by experience.
5. Confirm that the indicated flow is delivered by measurement with the gas flow measurement device.

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Changing Carrier Gas to Argon or Helium

The next hardware setting that can be modified is the gas used as an inert carrier. This can be changed
in the Instrument Parameters, Common panel. From the Antek MultiTek® Main Screen, activate the
Instrument Parameters, Common panel (Figure 2-38) and click the Edit button.
First determine the gas to be used as an inert carrier in the MultiTek®. Select the correct gas (Ar or He)
for GFC1, and/or GFC6. Click the Save button, then click Yes to save new version and automatically
Diagnostic Testing
Antek MultiTek® diagnostics can be performed from the “Diagnostic Display” screen by selecting the
Launch Diagnostics Editor button in the upper right corner of the main screen. The accessories’
functions can be tested from the Diagnostics screen (Figure 2-44). Only those accessories connected to
the instrument will have a check in its box. Also the furnace temperature controller can be locked by the
IT-administrator to prevent any changes using the controller’s front panel.
If there are multiple MultiTek® instruments on the same network, the Ethernet LED can be made to flash
by checking the Identify instrument box to identify the MultiTek® currently accessed.
NOTE
For the 737 inlet furnace, Actual Temperature is reported only during run-time, not while the MultiTek® is
in Idle mode.
Figure 2-44: Diagnostics Screen

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Furnace Power Up
WARNING
The Furnace operates at a temperature in excess of 1000o C; it can serve as an ignition source and cause
severe burns.
Furnace Control
To heat the combustion furnace perform the following steps. Turn on both the Furnace and electronics
power switched on the rear of the MultiTek®. A furnace controller is located inside the front panel of
the Antek MultiTek®. However, there is no manual operation of the furnace controller required by the
user. MultiTek® software and firmware control the furnace temperature setting.
NOTE
The temperature controller contains no user serviceable parts. Warranty is void if this controller shows
evidence of tampering.
Furnace Operations Overview

1. Loss of power to the MultiTek® will result in stoppage of all operations and the switching of all
controls defaults to the OFF position. When power is restored the furnace will heat up to its last
temperature setting.
2. Furnace temperature is monitored as a condition for instrument operation; default value is 1050o C.
Setpoint values must be entered using the Instrument Parameters, Common panel (Figure 2-38)
and click the Edit button.
3. Click the Save button, then click Yes to save new version and automatically write it to the
Nitrogen Detector Cooling

Detector cooling control is performed by the Nitrogen Module board in the Nitrogen Module – no
manual controls are available. To cool the nitrogen detector perform the following steps.
CAUTION
Detector cooling helps stabilize the nitrogen detector and reduce electronic noise; condensation can
occur. Detector cooling temperatures of 5o – 10o C are typical.

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Detector Cooling
controls to the OFF position. When power is restored the detector coolers will cool to its last
temperature setting.
2. Detector cooling can improve detector stability; however, excessive cooling to temperatures below
5º C is not recommended.
3. Detector cooling is monitored as a condition for instrument operation. Setpoint values must be
entered using the Instrument Parameters, Common panel (Figure 2-38) and click the Edit button.
System Pressure
WARNING
Do not exceed 5.0 psi (34.5 kPA) system pressure, higher pressure indicates excessive gas flows or a flow
path restriction. If high pressure is used, severe and irreparable damage may be done to fragile system
components.
NOTE
psi). Go to the Common panel in Instrument Parameters. Select the desired version then click “Write to
Instrument” to restart the gas flows after the pressure has dropped back to normal.
Pressure Control
1. For systems that do not utilize vacuum systems, flow path system pressure is primarily controlled by
GFC settings (Argon, Carrier O2, Pyro O2) that supply gases to the instrument pyrotube.
2. From the Antek MultiTek® Main Screen, activate the Instrument Parameters, Common panel
(Figure 2-38). Note the System pressure. Typical readings will be between 0.2 psi and 1.75 psi
(1.38 kPa and 12.41 kPa) depending on the configuration and instrument condition.
3. Backpressure fluctuations during leak testing can cause Hardware Error messages.
System Pressure Overview

controls to OFF. When power is restored, the GFC’s will restore gas flows to the sample flow path.
System pressure reading should return to preset values.
2. System pressure can be monitored as a condition for instrument standby. Setpoint values must be
entered using the Instrument Parameters, Common panel (Figure 2-38) and click the Edit button.
3. Click the Save button, select the new version from the drop down menu and click “Write to
Instrument” at the bottom of the panel.

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GFC5 and GFC6 Gas Flow Adjustment

GFC5 can be used to control carrier gas (Ar/He) flow to the 734 Gas Box. GFC6 can be used to control
Ar/He gas flow when an additional source or higher flow rate is needed.
GFC5 Gas Flow Control to 734 Gas Box
1. Where needed, carrier gas flow to the 734 Gas Box can be controlled by GFC5. Argon/Helium is
brought from the GFC Input Manifold to GFC5. The outlet for GFC5 is connected to the AUX
outlet of the GFC Output Manifold where it is available for the 734 (Figure 2-41).
2. Flow to the detector reaction chamber is controlled by adjustments to GFC5 through the MultiTek®
Software. The goal is to establish stable carrier gas flow to the 734.
3. Ensure flow path components are installed per instructions and guidelines provided in the 734
manual.
4. Activate the Instrument Parameters, Common panel (Figure 2-38) and click the Edit button.
Adjust the Setpoint for GFC5 so that detector flow is 20 - 25 mL/min (25 mL/min maximum).
WARNING
Do not set the flow rate above 25 mL/min to the 734 Gas Box. Coking will most likely result if the flow
rate is exceeds 25 mL/min.
6. Confirm and adjust (if required) the GFC setting to match desired flow to the 734. Measurement of
flow to the 734 can confirm carrier gas flow controlled by GFC5.
GFC6 Gas Flow Control
1. Ensure the flow path components are installed as required by the application.
2. Activate the Instrument Parameters, Common panel (Figure 2-38) and click the Edit button.
Select the correct gas (Ar or He) depending on the gas used. Adjust the Setpoint for GFC6 so that
detector flow is the desired rate in mL/min.
4. Confirm and adjust (if required) the GFC setpoint to match desired flow rate.

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Operational Standby
CAUTION
Do not introduce sample materials into the Antek MultiTek® until Operational Standby is achieved.
WARNING
Software safeguards prevent the start of analysis (data collection) until Operational Standby is
achieved.
Operational Standby/ Correcting Instrument Alarm Messages

Software control parameters allow the MultiTek® user to be assured the instrument parameters are
nominal before beginning analysis. Deviations from these expected conditions result in an “Alarm
Message” that must be resolved before an instrument sequence can be initiated. Instrument Alarm
messages and the actions required to correct them are listed below.
Message: TEC cooler is out of tolerance.

Action: 1. Check temperature reported on Instrument Status to determine if
cooler is working.
2. Set cooler to expected temperature. Allow time for cooling to occur.
3. Check the Nitrogen Module fan is running with airflow front to back.
Message: Furnace temperature is out of tolerance.

Action: 1. Check furnace temperature as reported on Instrument Status and
compare to furnace controller to determine if furnace is working.
2. Set furnace to expected temperature on Instrument Parameters, Common
Panel.
3. Restart Antek MultiTek® software to reinitialize and correct any
communication errors.
Message: Gas Flow Controller (GFCx;) flow rate is out of tolerance.

Action: 1. Check flow rates in Instrument Parameters screen.
2. Set GFC to proper flow (Hardware Settings screen). Allow time (15
seconds) for flow readings to register. Confirm flow volumes (see
Functional/TEST, this Section.
3. Check gas supply.
Message: UV lamp is present but UV Intensity is 0.

Action: 1. Enable Sulfur Module and UV lamp on (Instrument Parameters,
Common panel); allow 5 - 30 minutes for warm up of lamp.
2. Check UV Lamp Fuse inside the front panel for 24V.
3. Ensure Ozone is not flowing back into the Sulfur chamber.

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Message: Ozone Generator is present but not turned on.

Action: 1. Turn ozone generator on (Instrument Parameters, Common panel);
allow 10 minutes for generator to stabilize.
2. Check oxygen flow to ozone generator (Instrument Status) is more
than 15 mL/min.
Software Alarm Messages
Message: Nitrogen Module communication lost

Action: 1. Check that cable connectors are plugged in and firmly seated.
2. Check Nitrogen Module is fully inserted.
Message: Sulfur Module communication lost
Action: 1. Check that cable connectors are plugged in and firmly seated.
2. Check Sulfur Module is fully inserted.
Instrument Blank Test

Periodically and at instrument start-up, it is important to perform an analysis in which no sample is
introduced while allowing the MultiTek® Analyzer to go through its analytical program. This exercise is
commonly referred to as an “instrument blank.” This procedure can provide valuable information
regarding system contamination, component performance, and overall instrument stability. It is also a
convenient and safe starting point for the new user without the risk of improper sample combustion,
which can soot (coke) the system.
1. In the method screen, confirm your active method and ensure that the MultiTek® is in a fully
functional standby condition with no Alarms.
2. If the system shows an alarm, check on the error by viewing the Instrument Status or Alarm screen
(see Figure 2-45). Consult the MultiTek® Operation Manual Operational/Standby and other
sections as appropriate to assist in troubleshooting and clearing the alarms. Once the alarm
conditions have been resolved, select Acknowledge all. After the alarms are cleared, select Close to
return to the main screen.
NOTE
If during the instrument blank procedure a nitrogen/sulfur response is seen, run the sample blank
procedure again to “clean” the system. A few runs may be necessary at start-up. Repeat as necessary to
obtain a “flat” baseline. See Section 4 – Analytical Procedures & Suggestions in the MultiTek® Operation
Manual for guidance regarding baseline noise, integration and control.

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Figure 2-45: Alarm Screen
3. If this is the initial set up of MultiTek®, create a Method and Sequence to run the instrument blank
test. Follow the instructions in Section 3 to create a Method (See Figures 3-26 – 3-32). Note:
calibration of the Method is required. Create an Instrument Blank method and sequence following
instructions in Section 3, and guidelines in Section 4.
4. Run the instrument blank by running the Instrument Blank sequence. Do not introduce any sample.
5. Monitor the Run Control screen. The baseline should track from the left of the screen (Figure 2-46).
Figure 2-46: Instrument Blank Test

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Primary Testing Checklist

The following is a checklist that can be used to assure that the MultiTek® is ready to enter routine operation.
__________ System located properly?
__________ Accessories (if any) installed?
__________ Gas lines with specified pressures and flows installed?
__________ Vents installed (if required)?
__________ Pyrotube properly installed?
__________ Leak check for pyrotube and detector flow path performed?
__________ Electrical/Electronic control interconnections correct?
__________ Furnace at operating temperature?
__________ Thermoelectric cooler at operating temperature?
__________ Computer operational with Antek MultiTek® Software?
__________ Hardware Error messages resolved.
Once the above checklist is complete, the MultiTek® can be setup for an instrument blank test. When
the user prepares to analyze samples, instrument parameters compatible with the samples and calibration
standards need to be determined and set in the methods. Sections 3 & 4 describe the general procedures
needed to analyze the Antek Installation Check samples.

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SECTION 3
NITROGEN / SULFUR OPERATION
MultiTek® Software
System Block Diagram
The MultiTek® Analyzer is PC controlled. MultiTek® Software must be running on a Windows PC in

order to operate the MultiTek® analyzer. All the settings and results data are stored on the PC. The
analyzer itself has limited user interface with four status LEDs and a “Start” push button.
Figure 3-1: The system block diagram
MultiTek® Instrument MultiTek® Instrument MultiTek® Instrument

(No. 1) (No. 2) (No. n)
Router
Windows PC
(MultiTek® Software)
To control multiple instruments simultaneously, a software instance for each instrument connected may
be run on the same PC. Ensure the PC has the resources necessary to support the maximum number of
instruments that can be connected.
Quick Start Steps

The following steps may help you to quickly start and operate the instrument.
1. Connect to analyzer
2. Creating user accounts
3. Configuration of MultiTek® Analyzer
4. Create standards list
5. Calibrate the MultiTek®
6. Run a sequence
7. View results
8. View QC history
9. Alarm Monitoring
10. Diagnostics
11. Task scheduling
12. Audit trail

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Connect to Analyzer
Before running the MultiTek® software, ensure the MultiTek® analyzer has been powered on. In
addition, ensure the PC is connected to the MultiTek® analyzer via a LAN through a router.
NOTE
Launch the MultiTek® software by double clicking the Antek MultiTek® software shortcut on the
desktop. The MultiTek® software starts with a logon screen. The logon screen includes an analyzer list,
displaying all the analyzers that have been registered into the PC’s MultiTek® software database and any
other analyzer found on the network. If an analyzer has not yet been registered, the user may add the
analyzer by selecting the analyzer and clicking on the Register button. If any analyzer on the network
has been turned on, it’s claiming computer name, state, and alarm information will be updated to the list
in real time. Analyzers registered in the database but not found on the network will show a “?” entry.
Figure 3-2: Antek Logon
Follow the steps below to connect to (claim) an analyzer:

1. Enter User ID and Password; (Defaults – admin, password)
2. Select an instrument from the instrument list;
3. Register the instrument if it’s new to the database (see IMPORTANT Note below);
4. To work offline, check the “Work offline” box;
5. Click Logon button.

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If the “Work offline” check box is clear, the software will directly control the MultiTek® and run in the
online mode. Otherwise, it will run in the offline mode. The “Work offline” box will be checked if the
instrument is powered off, claimed by another instrument, or is no longer connected to the LAN. In the
offline mode the software is not connected to an instrument, and thus cannot run methods or collect data.
However, the software can still access data stored in the database. The offline mode may be used to edit
methods or samples, create sequences, view results and view QC history after collecting data.
If an analyzer is already claimed by a user, subsequent users can only work in offline mode with this
instrument.
Register Instruments
IMPORTANT
An instrument’s name and serial number are stored in non-volatile memory on the instrument’s processor
board. If the processor board is replaced, the name and serial number will revert to default values. Also
the instrument will not reconnect to its database, including methods and instrument parameter settings.
Follow the instructions for previously registered instruments to restore the name and serial number,
and reconnect the instrument to its database only if the processor board has been replaced.
New instruments and installations: When the pop-up “Do you wish to use any existing instrument
database?” appears, select No (Figure 3-3).
Once the MultiTek® has been registered, click Logon to claim the instrument (Figure 3-5).
Figure 3-3: Register Instrument

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Previously registered instruments with replaced processor board: An instrument previously

registered in the MultiTek® Software and has had its processor board replaced, will show up as a new
instrument to be registered. In this case the instrument can be re-registered with its original name and
serial number. The physical address (MAC) will be that of the new processor board.
When the pop-up “Do you wish to use any existing instrument database?” appears (Figure 3-3), select
Yes, select the correct instrument name and click OK (Figure 3-4), then click Logon (Figure 3-5).
Figure 3-4: Reconnect to Instrument Database
Figure 3-5: Instrument Logon

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MultiTek® Main Screen

After an analyzer has been claimed, the software will go to the Main analyzer screen.
Figure 3-6: Main Screen
MultiTek® Main Window Layout – Views and Options
The main window has the following areas:

• Title Bar
o Displays “Instrument Name <(offline)> – Software Name”
• Menu Bar: File, Setup, Control, Help
• Toolbar
o Displays current state and alarm of the connected instrument
o Displays current method name and sequence name
o Displays frequently used command buttons

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• Workspace with tabs for main features
o Main features: Run Control, Instrument Status, Result, QC History
o Popup dialog boxes are used for supporting features, such as
 Sample Editor
 Method Editor
 Sequence Editor
 Instrument Parameters
• Status Bar
o General message area
o Database status
o User name
o Access level
• Sample, Method and Detector (left-hand side)
o Injection, Tray and Vial Numbers
o Method Run and Cycle times
o N/S Detector output and Maximum values
• Signal Display Graph
o N and/or S Signals
o Track/Pause
o Axis Scroll/Zoom
o Select
o Zoom Box
o Zoom to Fit
o Time Meter: 1 min, 10 min, 1 hour, 8 hours
If the instrument is configured as Nitrogen-only or Sulfur-only, the Main Screen will only display and
plot data for the active detector (Figure 3-7).
Figure 3-7: Main Screen – N or S only Configurations

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Popup Dialog Boxes
A Typical Popup Dialog Box (Sequence Editor for example) is below in Figure 3-8.
Figure 3-8: Sequence Editor
A dialog box normally has controls on both top and bottom:

• Top: Database table access toolbar. It may contain the following buttons.
o Navigation buttons: Go to Previous/Next record
o Add: Add a new record
o Edit: Edit the current record
o Save: Save the current record
o Save as: Save the current record to a new name
o Export: Export current record to a text file (csv)
o Print: Print current record to a printer as pdf or secure pdf file
o Compare: Compare versions to determine differences between them
• Bottom left: Instrument access buttons such as “Send to instrument”
• Bottom right: Commit buttons that close the dialog box such as Run, Close
Lock Software Feature

New in MultiTek® Software v2.0.0.0 is a feature that allows the user to lock the individual instance
running to prevent changes, or interruptions, while running sequences or other critical operations. No
other instance of the software will be affected by locking this instance. To lock the instance of
MultiTek® Software running, click the padlock icon at the top of the Main Screen (Figure 3-9). The
popup will appear to verify whether the user wants to lock the software or not. Click Yes to lock the
software, or No to return to the Main screen (Figure 3-10, left).

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Figure 3-9: Main Screen – Lock Software Feature

Lock software
Once locked, the Unlock application popup will appear (Figure 3-10, right). Only the user logged in
when the software was locked, or users at higher levels (see Creating and Managing User Accounts), can
successfully unlock the software. To unlock that instance, enter the user ID and password, for the user
who was logged in (or higher level user) when the software was locked, and click OK. Access to that
instance will resume.
Figure 3-10: Lock and Unlock Software
Creating and Managing User Accounts
Click on the “User Management” icon on the tool bar to launch the “User Management” window (Figure
3-11). IT Administrator, Service or Administrator level users have full authority to access the software,
while those at User level cannot change instrument parameters, create or calibrate a method. If logged
on at the IT Administrator, service or administrator level new users can be created; existing users may
be activated or deactivated, or set to a different access level.

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Click on the plus sign to add a user, or the edit icon to edit a user’s level, active status, password
or electronic signature. To load an electronic signature, click Load signature to browse for and select
the .bmp the file. The signature may be removed by clicking the Remove button.
Figure 3-11: User Management
All user levels are able to change their password after logging on.
Figure 3-12: Password Change

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Configuration of the MultiTek® Analyzer

To configure the analyzer, click Instrument Parameters on the “Setup” menu. Instrument Parameters
are saved in multiple versions starting from version 1. However, only one version may be applied to the
instrument at a time. The “Currently applied” check box indicates the current version that has been
written to the instrument (Figure 3-13).
The analyzer name and serial number are displayed in the “Identification” tab of “Instrument
Parameters” screen. IT Administrator and Service level user can modify both; Administrator level users
can only modify instrument name; User level has no authority to modify either.
Figure 3-13: Instrument Parameters – Identification

Currently applied version check box
Once a version is saved it can no longer be changed, however any created version may be sent to the
instrument by clicking on the Write to instrument button.
Configurations and Instrument Parameters are displayed in the “Common” tab (Figure 3-14).
To make changes to the current version and apply it to the instrument:

1. Click Edit button on the toolbar (Figure 3-14);
2. Modify set points and other parameters;
3. Click Save button on the toolbar,click Yes to save the modified parameters to a new version and
automatically write them to the instrument (Figure 3-15), then click OK.
NOTE
If you select Close instead of Save, a dialog box will ask if you want to save a new version. Clicking on “Yes” will
save the settings in a new version, but will not write the new version to the instrument.
To apply the settings of a previously saved version to the instrument:

1. Select the desired version from the “Version” list on the toolbar (Figure 3-14);
2. Click Write to instrument button to apply the selected version to the instrument;

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Figure 3-14: Edit and Save Settings
Selected Version Edit Save Print Compare Expand/Collapse
Write to instrument Setpoint boxes – enter new values
Figure 3-15: Saving Instrument Parameters and Writing to Instrument

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The configuration selected will determine the detector signals and related parameters displayed on the
Main and Instrument Status screens, as well as those displayed and available for modification in the
Method Editor screens and Calibration Sequences.
The Common tab has three sections: Configurations, Components and detector enable/disable. This
tab may be collapsed to only show the Standard configuration options (Figure 3-16), or expanded to
display all the component settings (Figure 3-14). The Standard button is used to select a default
configuration and associated component settings. The User defined button allows the configuration and
settings to be customized for a specific application. In the upper right part of the panel (detector) you
can enable or disable the Nitrogen and Sulfur detector modules, UV Lamp (for Sulfur) and the Ozone
Generator (for Nitrogen).
IMPORTANT
If a module is enabled but not present, an alarm will occur; no sequences will be allowed to be run.
Standard Configurations
There are three major standard configuration selections: Solid, Liquid or Gas, supporting NS, N-only, S-
only or IC-only standard configurations. Selecting one of the sub-options automatically sets the default
configuration of detector modules and component settings.
Liquid and Gas configurations (Figures 3-16 & 3-17) support configurations utilizing the 734
Gas/Liquid (LPG) Sampler, 740 Multimatrix, 735 Syringe Drive and Liquid Autosamplers.
Liquid samples require a Liquid Autosampler with a 740/735 combination for horizontal instruments, or
735 Syringe Drive by itself for single, manual injections. Liquid Autosamplers and 735 Syringe Drives
are used alone on vertical instruments.
Figure 3-16: Standard Liquid Configuration
Expand/Collapse

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Gas/LPG samples require the 734 Gas/Liquid Sampler. For small amounts of solids, the 740
Multimatrix is used with the 735 Syringe Drive.
Figure 3-17: Standard Gas Configuration
NS configuration has both Nitrogen and Sulfur modules. N-only, S-only and IC-only are the
configurations with only a single detector: Nitrogen, Sulfur, or IC module, respectively. Additionally,
the S-only option supports standard Sulfur and Low-Level Sulfur (LLS). A standard single-pass
pyrotube is used for standard Sulfur detection; a double-pass pyrotube is used in the LLS configurations.
Nitrogen detection is not supported in LLS configurations. The 734 Gas/Liquid Sampler can be used
with all configurations.
Solid configuration selection (Figure 3-18) is for MultiTek® configurations using the 737-M Solids
Sampler. Refer to the MultiTek® 737-M Solids Sampler Addendum manual for configuration and
parameter settings.
Figure 3-18: Standard Solid Configuration

737-M Connected (X if not present)

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User Defined Configurations

Click on the Expand/Collapse button to view the default component settings of the standard
configurations. To enable or disable the detectors individually or change settings, select User defined
(Figure 3-19).
Choosing User defined allows all components to be enabled or disabled as well as modification of their
set-points and tolerance ranges. For example, an NS configuration could be used to record Sulfur-only
data by creating a version with the Nitrogen Module and Ozone Generator disabled. Also, the operator
could determine if a module is responding or not by disabling and enabling the UV Lamp for the Sulfur
Module, or Ozone Generator for Nitrogen module.
Figure 3-19: User Defined Configurations

Expand/Collapse

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Comparing Instrument Parameters Versions

To view parameter changes between versions, click on the Compare button at the top of the Instrument
Parameters screen (Figure 3-14). Choose the two versions to be compared and click Compare (Figure 3-20);
click Close to select other versions to compare, or click Close again if finished.
Figure 3-20: Compare Instrument Parameter Versions

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Create Standards List

Blanks and standards can be added in the Sample Table using the Sample Editor. The Sample Editor
window may be opened by clicking Sample Editor icon at the top of the Main screen (Figure 3-6), or
the “Sample” menu item on the Setup menu. Click Edit, then Add icon on the toolbar to add new
samples. After creating the samples, click the Save icon to save the sample table. A Filter function is
available to reduce the number of samples and sample types displayed. Other icons at the top of the
Sample Editor screen are Export (csv file), Print, View history and Compare. View history and
Compare apply only to individual samples and are only active if the number in the Sample version
column is greater than 1.
Figure 3-21: Sample Editor

Filter Add Edit Save
NOTE Once a sample has been created, it cannot be deleted from the database.
The following table describes the columns in the Sample Editor.

Column Description Example
Sample state The state of a sample. It may be Gas, Liquid or Solid. Liquid
Timestamp Logged into the database and used to track data 8/11/2009
9:35 PM
Sample ID It is used to identify samples in all other windows. L5001
Version The version of a sample. Once a sample is saved, it will not 1
be overwritten. Changes are saved as new versions.
Sample name A name to describe the sample, optional Test 001
Sample type Blank: Sample with blank concentration value (0 ppm). Blank
Standard: Sample with known concentration value. It may Standard
be used for calibration and QC check standards.
S- Conc (ppm) Known value for a standard sample. For values in the ppb 25
range are entered as 0.nnn, e.g., 0.125 stands for 125 ppb.
N-Conc (ppm) Known value for a standard sample. For values in the ppb 25
range are entered as 0.nnn, e.g., 0.125 stands for 125 ppb.
Availability Indicates if the sample shall be available for testing.

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AutoFit
AutoFit is an optional feature for adjusting the PMT voltage to the maximum value for the highest
concentration sample in the calibration sequence. If used, it should be done only once before running the
calibration sequence. AutoFit can be run for the detectors individually as well as together.
The following precautions must be taken when using AutoFit:

1. If the highest concentration standard in the calibration sequence table is less than 10ppm, a PMT
voltage of 600V should be adequate. Using AutoFit in this case is not advised as AutoFit may
increase the PMT voltage to the point where the baseline noise is excessive.
2. Before AutoFit, all parameters, hardware settings and timed events should be saved.
3. The calibration sequence must have been created and saved before AutoFit is run.
4. AutoFit may require up to 8 injections to complete. AutoFit is finished when the State changes
to Idle.
5. Because AutoFit may run up to 8 injections, multiple vials of the standard should be prepared to
insure an adequate amount is available. The operator should keep watch over the analyzer and
software during this process. The sample in the vials may need to be replaced during this
process.
6. After running Calibration, the user should not be required to perform AutoFit again because the
PMT voltage has already been optimized.
To start, click AutoFit in “Method Editor”. Another pop-up will appear to let the user select which
module(s) to AutoFit (Figure 3-22). S, N, or both may be checked. After a module is checked, the
maximum concentration from the calibration sequence will be shown in editor box. This is the
concentration of the sample which is going to be used to AutoFit. Click AutoFit in the active
window and the process will start.
Figure 3-22: Method Editor: Calibration-AutoFit

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Below is an example AutoFit executed for both Nitrogen and Sulfur detector modules.
Figure 3-23: AutoFit in Progress
When AutoFit is finished, the software will automatically change the Method PMT voltage to the
best value and inform the user of the change (Figure 3-24).
Figure 3-24: AutoFit Complete
After the user accepts the change, the new PMT voltage will be sent to the instrument. The PMT
voltage change can be verified from Instrument Status screen (Figure 3-25).
Figure 3-25: Instrument Status Screen

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Method Creation and Calibration

The Method Editor window is used to setup methods for the instrument. A method includes parameters
for peripherals, hardware settings, timed events, and calibration sequences and coefficients.
Methods can only be created in the online mode and linked to the claimed instrument. Methods created
for one instrument are not directly available to other instruments, but can be exported or printed. The
method editor is accessible to IT-administrator, Service and Administrator level users only.
Steps to create and calibrate a method:

1. Click on the Method editor at the top of the Main screen. Create a new method or save one existing
method as a new method.
2. Set hardware parameters to the recommended values in the “Hardware settings” tab.
3. If the liquid autosampler (748 or 758) is used, set parameters to recommended values in the “Liquid
autosampler” tab.
4. If the inlet furnace (737-M) is used, set the profile to recommended values in the Inlet furnace
profile tab.
5. In “Timed events” tab:
a. Set cycle time (this time must be greater than the liquid autosampler cycle time, if used).
b. Set autosampler start time to 0:01 or greater.
c. Set baseline duration and detector signal integration times for each detector, these are estimated
values and can be adjusted after the calibration finishes.
d. In the check box, check all necessary accessories for running the sample, then set the time to the
proper values. Important: Accessories (and status plugs) must be connected to the MultiTek®
to be used by the software.
6. In Calibration tab:
a. Click the Sequence button then setup a calibration sequence table. Important: Calibration
standards should have already been entered in the Sample table
b. “Autofit” can be used to seek the maximum PMT voltage for the highest concentration standard
in the calibration sequence table. However, 600 – 700 V works for most sample types.
c. Click the Calibrate button and select which range in the calibration sequence table needs to run,
then click OK to start running the calibration sequence.
7. After the calibration sequence run is finished, go to “Results” tab to check whether the baseline
duration and signal integration time has been set properly. If not, go back to the “Timed events” tab
of the Method editor and adjust the times as necessary to optimize the response.
8. Click the Recalculate button.
9. View the calibration curve and the correlation coefficient. Then determine whether or not to use
the results, or rerun specific standards. Click Close to save adjustments.
10. After a method is calibrated, it can be used to run unknown samples, or QC check standards.
The Method Editor has 5 tabs: Liquid autosampler, Inlet furnace profile, Hardware settings, Timed
events, and Calibration (Figure 3-26). Above the tabs is a box for “Blank correction” plus drop-down
boxes for “Baseline” and “Correction”. “Blank correction” is used, once the value of the blank response
has been determined, to subtract that value from the response of calibration standards, QC samples and
unknown samples using the method. “Baseline” is used to select either horizontal or tangential baseline
calculation. Baseline is the value subtracted from the response during the integration time to determine
the signal response due to the sample. Horizontal baseline calculation is a constant value; tangential
calculates an increasing or decreasing value tracking a rising or falling baseline. “Correction” provides
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the means to visually compare results by eliminating baseline variations from the graph – only in
Horizontal Baseline mode; select “Zero corrected” and recalculate the method to affect results of
previous sequence runs.
The Liquid autosampler tab lists the parameters used for an injection cycle; syringe size reported by
the autosampler is shown at the top (Figure 3-26). The parameters are discussed below.
IMPORTANT
For each parameter note the multiplier in parentheses. It is used to determine the volume, timing or
rate of the parameter.
Figure 3-26: Method Editor: Liquid Autosampler
Clean cycles (3) – used to eliminate/minimize carry-over contamination from one sample to the next.
There are two different clean cycles prior to sample injection and one after; two cycles use solvent and
one the sample itself. One pre-injection solvent, two sample and three post-injection cycles are
recommended initially. Depending on the composition of the sample, more or fewer may be needed;
additional clean cycles will extend the time required for each injection.
Clean Cycle fill volume should be greater than the Sample fill volume or the same if the maximum
syringe volume is used.
- The number specifies how many microliters (µL) are to be used.
Pull-up delay, speed and count parameters are used to minimize the formation of bubbles in the injection
sample. Bubbles can introduce errors into calculations of sample concentration results as well as affect
repeatability (%RSD). Adjust these parameters to minimize or, ideally, eliminate bubbles.
- Pull-up delay is in tenths of one second – entering 10 results in a delay of one second.
- Pull-up speed is in tenths of microliters per second – entering 10 results in a 1 µL/s rate.

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Sample fill volume is determined by the amount of sample needed to accurately measure the
concentration of Nitrogen and Sulfur. Lower concentrations typically require more sample to achieve
the response needed. However, injecting too much sample may result in coking the instrument, or just
wasting sample.
- The number specifies how many microliters (µL) are to be used.
Air fill volume pulls a small amount of air into the needle and syringe to prevent sample in the needle
from volatizing and ensuring the whole sample volume is injected at the desired time.
- The number specifies how many microliters are to be used.
Needle punch to injection delay and Injection to needle pullout delay are used to keep any response due
to needle insertion or pullout from affecting the instruments response to the sample.
- The delay is in tenths of one second – entering 10 will result in a one-second delay.
Sample injection speed controls how fast the sample is injected into the pyrotube. Faster injection rates
reduce integration time needed for accurate analysis, but too fast may result in coking the instrument.
Hydrocarbon-based samples typically require slower injection speed.
- Pull-up speed is in tenths of microliters per second – entering 10 results in a 1 µL/s rate.
In the Hardware settings tab, the hardware set points can be modified for each Method. However, some
components will not be accessible if they have not been selected by the user in the “Instrument
Parameters, Common” tab. The Method will record the UV lamp intensity (if the Sulfur module was
selected) at the point when the Method is first created and saved. This value, once recorded, is not
changeable for that Method.
Figure 3-27: Method Editor: Hardware Settings

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In the Timed events tab, the User can set the sample run cycle time, event time, baseline evaluation and
signal integration times. Cycle time is the duration to complete one run cycle, and is defined by the time
from the transition of Ready to Run, to the transition of Run to Post Run. The S- or N-Detector time is
to set the times for baseline data and detector integration acquisition to occur. It is referenced to the
absolute time from run cycle start. For this reason, no accessory’s event time can be set to a 00:00 time
value. Also, the cycle time must be long enough for the autosampler to complete an injection cycle. It is
not necessary to set the optimum baseline evaluation and signal integration time windows when the
Method is created. These parameters can be adjusted after the calibration run has been completed and
results updated using Recalculate option.
Baseline evaluation and integration times can be set independently for Sulfur (Figure 3-28) and Nitrogen
(Figure 3-29). This allows for optimization of each signal’s response.
NOTE
There are two approaches to set the baseline determination time: Use Duration or Use Start/Stop. If Use
Duration is selected, the base line will be evaluated in windows of duration time before the signal integration
start and after the signal integration stop. Alternately, if the Use Start/Stop is selected, the user has to set the
baseline evaluation start and stop time. The user has the option to utilize the left peak side or both left and
right peak sides. If only the left peak side change is desired, set the start and stop times to 0:00 for the right
window.
The Liquid autosampler may not be accessible if it is not connected properly or if the proper sample type
is not selected. When using the Liquid Autosampler, caution must be exercised when setting the timing
parameters in the Timed events tab. The time required for the autosampler to complete an injection cycle
(includes pre-wash, pull-up, sample injection and post-wash) must not exceed “Cycle time”.
Figure 3-28: Method Editor: Timed Events – Sulfur Module

Sulfur Baseline and Integration

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Figure 3-29: Method Editor: Timed Events – Nitrogen Module

Nitrogen Baseline and Integration
After saving a modified method, the new settings can be applied to the instrument by clicking the Send to
instrument button. However, the Method listed in the sequence table will always be sent to the instrument
before the first sample of a sequence is run, or whenever a different method is required during a sequence run.
The Calibration tab is used to set up and run the calibration sequence for the method. Before
calibrating the method, all parameter settings in other tabs must be set. The user interface of the
“Calibration” tab in the “Method Editor” is shown below.
Figure 3-30: Method Editor: Calibration
Buttons on the Calibration tab:

• Sequence: Create a calibration sequence table
• AutoFit: Run the calibration sample with the highest concentration to optimize PMT voltage
automatically
• Calibrate: Run the calibration sequence and calculate coefficients for the method

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• Recalculate: Recalculate coefficients of the method and all results using this method.
Calibration curve may be refreshed after recalculation. User can check/uncheck blank
correction and Use for S/N check boxes and then perform recalculate function.
To calibrate a new method, a calibration run sequence table must be created. Click the Sequence
button, “add standard/blank samples” using the check box, save this table and then click OK to save the
calibration sequence (Figure 3-31). Only one blank sample is allowed for each calibration run sequence.
Figure 3-31: Calibration Sequence
Click the Calibrate button, and then select the sample range from the calibration sequence list for the
calibration. Click Run, and the calibration will start.
NOTE
If the check box for the “Push Button” column is checked, the sample run will wait for the user to press the
“Start” button on the front of the MultiTek® for each sample checked.
Figure 3-32: Calibration Sequence List
Once started, Calibration can be stopped by clicking Stop Sequence ( ) on the Main screen (Figure 3-
6). The software will finish all injections for the current sample, save the results, and then stop the
“Calibration” sequence. Calibration can be paused by clicking Pause Sequence ( ). The software will
finish the current injection; save the result and hold the sequence run. The calibration can be resumed
by clicking Run Sequence ( ). Calibration can also be aborted by clicking Abort Sequence ( ). By
doing this, the software will stop Calibration immediately and discard results of the current injection for
the current sample.

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If a sample needs to be added to the middle of the calibration sequence, click Sequence tab on the Main
screen while calibration is underway and highlight line where the sample is to be inserted (Figure 3-33).
Click Insert, select the Sample ID and name from the Sample Editor that will pop up. Enter the number
of injections (# Injection), and Tray and Vial information to match the location of the sample vials.
Tray/Vial numbers for subsequent samples will also need to be updated. Samples may be added to the
end of the sequence by clicking Add and completing the sample and tray/vial information in the
Sequence table.
Figure 3-33: Insert/Add Sample: During Calibration Run
After the calibration is complete and the results have been viewed, the user can change the baseline
evaluation and the signal integration time from the “Timed Events” tab. Recalculate must be clicked in
order to re-compute the calibration curve(s) and correlation results (Figure 3-35). After the method is
saved the Select Results for Recalculation screen will appear (Figure 3-34). Selects either specific
results individually, or all results (Select all) to be recalculated, then click OK. The recalculated results
can be reviewed using the Results screen from the Main screen.

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Figure 3-34: Method Editor: Results Recalculation
The user can also exclude particular samples or particular injections of the sample from the method
calculation. To exclude particular samples, uncheck the sample from the sample list in edit mode.
Figure 3-35: Method Edit: Exclude Sample

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To exclude particular injections, the user should right-click the sample in the calibration sequence on the
Calibration tab. Click “Show Injection Details” to display the Injection Details table. Uncheck the
injection or injections to be excluded and click OK. Click Recalculate to review the effect on the
calibration results. When satisfied with the results, save the method and select the results to be
recalculated.
Figure 3-36: Method Edit: Exclude Injections
First and Second Order Calibration Curves

Depending on the composition of the sample and/or the range of concentrations, the response may be
linear or non-linear. In most cases the response is linear and the regression curve calculation is a first-
order equation – default (Figure 3-37a). The option to use a second order calibration curve is available
if needed. To use the second order calculation, click Edit then use the drop down box, Regrn Ord:,
select 2 and click on Recalculate. The 2nd Order Coeff box will then have a value (Figure 3-37b). If
the correlation value is acceptable, recalculate and save the method version, then recalculate previously
taken results as necessary.

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Figure 3-37a: Method Edit: First Order Regression Calibration Curve
Figure 3-37b: Method Edit: Second Order Regression Calibration Curve

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Comparing Method Versions

To view changes between Method versions, click Compare at the top of the Method Editor screen (Figure
3-38). Choose the two versions to be compared and click Compare (Figure 3-39); click Close to select other
versions to compare, or click Close again if finished.
Figure 3-38 Compare Method Versions

Compare
Figure 3-39 Compare Method Versions

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Create and Run a Sequence

After method is calibrated, sequences can be run to analyze unknown samples and run QC (standard)
samples. A sequence may contain one or more samples. The Sequence Editor is used to create a
sequence as well as to add samples or edit the sample list.
To create a sequence click Sequence on the Main screen (Figure 3-6), then click Add new . Select
the Sample state and enter the Sequence name (Figure 3-40). Enter sample information the in the
Unknown Sample Details pop-up table for each sample. Select the Method from those available, then
enter the number of injections, and change Multiplier, Divider, Tray and Vial entries as necessary.
Figure 3-40: Sequence Editor: Create Sequence
If the “Push Button required” option is selected for a sample, the software will pause at the “Ready”
state and wait until the Start button on the instrument is pressed. This allows time for the operator to
prepare and load the sample. The Start button is not used any other time.
Click Run on the Sequence Editor screen to start the sequence (Figure 3-41). Select the range of
samples to run and click Run on the Start Sequence pop-up.
Figure 3-41: Sequence Editor: Run Sequence (liquid/gas)

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NOTE
The top toolbar controls and the bottom Run and Close buttons are for managing the sequence while the Add,
Insert and Delete buttons are for managing samples in the sequence.
For solid samples, the actual weight for each sample inserted must be entered.
Edit Sequence during an active run

When a sequence is running, the Run Control screen displays the sequence with the current sample
being analyzed highlighted in green. To view the real time run of the current sample in the Run Control
screen, the sequence editor window can be closed in order to achieve full viewing. During an active run
sequence, lines not analyzed may be edited or additional samples added to the sequence. Use the same
procedure for adding/removing samples as for the calibration sequence (Figure 3-33).
Run Control
The features displayed (Figures 3-6 and 3-42) are as follows:
• Sample information shows the current sample and injection
• Method Run and Cycle times in minutes and seconds
• Detector signals
• Controls for manipulating the graph such as vertical or horizontal scale and axis modification
• Alarm (Warning/Error): parameter out of tolerance and may abort the sequence
Figure 3-42: Instrument Status
Instrument Status
• Displays the current state of instrument in real time
• Displays of peripheral parameters, temperatures, system pressure, gas flows and detector module
parameters (Figure 3-43).
Figure 3-43: Instrument Status

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View Results
Click the Results tab to view the results of samples run on the instrument.
The left panel on the “Results” tab displays the list of results. Each line has the format of
• <Color Code> <Test Time> <Sequence Name> <Sample ID>
Each result in the details list has a color coded icon associated with it. The color coding can be
interpreted as follows:
A 512 Alarm occurs when the autosampler does not detect a rinse/waste vial or sample vial.
The filter area under the Results list may be used to narrow the list by setting a combination of criteria.
The Results list may also be sorted in time ascending or descending order by right clicking the list and
clicking the ascending or descending button. For evaluation purposes, the results may be exported or
imported in .mtr file format (MultiTek® Results). Exported results are no longer listed unless imported
back to the Results list. The color-code icons will be changed to reflect the results have been imported.
Result(s) may be added to the Result details list on the right side to view the details and graph. Highlight
one or more results, click (Add to result details), or right-click and select “Add to result details”. The
graph on the top displays the overlay of all the signals in the “Result details” list. Selection of multiple
results is done by holding the Shift key or Control key while selecting. The selected results can also be
dragged into the “Results Details” table.

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Figure 3-44: View Results
Selected results in the “Result” list will show Injections, Sample, Method and Instrument Parameters
information by clicking the tabs to the right of the “Result details” tab.
The selected results can be exported or printed by the user. To review specific details of selected
injections, select the appropriate sample details such as, Injections, Sample, Method or Instrument
Parameters, in the “Results Details” (Figure 3-45).
Specific sequence sample run injections can be de-selected for the results calculation by unchecking the
box on the injection’s results line in the Use column, then click on the “Reprocess” button (Figure 3-46).

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Figure 3-45: Results Details
Figure: 3-46: Unused Sample Injections
Additionally, users can modify the weight for solid samples or multiplier/divider for liquid samples by
clicking Reprocess from the sample tab. The Recalculate button must be clicked on the Recalculate
Settings screen to for the change to take effect (Figure 3-47).

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Figure: 3-47: Reprocess Results
The result can be removed from the “Result details” list by highlighting the result row, right clicking the
mouse and left clicking on the popped up “Remove” menu item. In addition, the results can be removed
by highlighting and pressing the “Delete” key from the keyboard (Figure 3-48).
Figure 3-48: Results List – Remove Sample

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View QC History
In addition to viewing the “Results list”, all blank or QC samples that have been run from a sequence
will be stored in a QC history for quality control monitoring (Figure 3-49). The measured concentration
and expected concentration will be displayed together. Also, the variance between these two numbers
will be calculated and highlighted using a different color in the graph view. The ranges for the colors
can be changed by editing the number in the right-hand boxes, starting with the value for Yellow, then
Green. Click on another box to set the lower value for Yellow. The upper range for Green must be less
than the upper value for Yellow. The upper range for Red will be automatically reset by clicking
another box.
Figure 3-49: View QC History
Alarm Monitoring
The alarm function in the software checks the actual value against the set point value for all instrument
hardware components. The alarm trigger point is set in the Tolerance field on the “Common” tab of
“Instrument Parameters” window. If no alarm is triggered, the “Alarm” status will be Green and
display None. If an alarm is triggered, the status changes to Yellow and reads Warning (Figure 3-50a),
or Red and displays Error (Figure 3-50b). Clicking the Alarm button on the main toolbar allows the
user to view and acknowledge all the active alarms. Each alarm has a code assigned to it – refer to the
table below for a complete list of alarm codes.
Under Warning conditions, monitor the Instrument Status screen and the Alarm list (Figure 3-50a). If
the condition(s) do not clear in 5-8 seconds the alarm status will change to Red and display Error.
Sequences will continue to run and may be started under Warning. However, under Error conditions,
neither Sample nor Calibration sequences are permitted to run – any sequences running will be aborted.
The Tolerance value can be increased to avoid alarms for some hardware settings. In general, this is not
recommended.

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MultiTek® Software Alarms
Alarm code Alarm level Alarm message

101 Error System initiation fail
102 Error System stack overflowed
200 Error No GFC been detected
201 Error GFC1 not working
207 Error System pressure module not working
211 Warning GFC1 out of tolerance
217 Warning System pressure out of tolerance
220 Error Ozone generator is off
301 Error Furnace temperature controller not working
311 Warning Furnace temperature out of tolerance
401 Error Sulfur module communication lost
411 Warning Sulfur high voltage out of tolerance
402 Error Nitrogen module communication lost
412 Warning Nitrogen high voltage out of tolerance
413 Warning TEC temperature out of tolerance
414 Error UV lamp intensity is too low
501 Error Autosampler communication lost
512 Warning No sample on auto sampler
514 Error Autosampler is not ready
601 Error Inlet furnace communication lost
612 Warning Inlet furnace temperature out of tolerace

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Figure 3-50a: Alarm Monitoring - Warning
Figure 3-50b: Alarm Monitoring – Error
Diagnostics
The Diagnostics window (Figure 3-51) is used to test the functionality of the available peripherals,
which includes the 735 Liquid/Solid syringe drive, the 734 Gas/Liquid Sampler, the 748 or 758 Liquid
Autosampler, and the 737-M Solids inlet furnace. Accessibility is dependent on whether the accessory
and status plug (if required) are connected to the analyzer or not. If connected, the corresponding status
check box will be checked and functions can be manually tested for that particular peripheral. If not, the
functions for the peripheral will be non-functional (greyed out).
The ETHERNET LED on the analyzer will change from solid blue to blinking blue when the Identify
instrument check box is checked. This is used to identify which instrument has been claimed by the
current software instance where more than one instrument is available.

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Figure 3-51: Diagnostics
Task Scheduler
The MultiTek® software has the flexibility to allow users to select and run a Startup and/or Shutdown
method at a desired time (Figure 3-52). If the Enable weekend operation (7 days a week) box is checked,
the Startup and/or Shutdown methods will be active all 7 days each week. Otherwise, the Startup and
Shutdown methods are only active during the normal 5 working weekdays. If a shutdown is initiated on
Friday, a startup will not occur until the following Monday.
NOTE
If using the Shutdown method, it is recommended a Startup method be set to start 1 hour prior to when the
MultiTek® will be used, to allow enough time for the instrument to stabilize.
By checking Enable method the selected method will be automatically applied to the instrument at the
time set in the Task Scheduler.
A Shutdown Method can be used to lower gas flows to preserve gas supplies during off-shift hours.
It is recommended Carrier Oxygen and Ozone Generator (if present) Oxygen flows be set to a minimum
level 10 mL/min each. Sleep mode should also be enabled when reducing gas flows to prevent “system
pressure out of tolerance” alarm. An alarm will prevent the start-up method from being applied.
By checking Enable method for End of Sequence, the selected method will be automatically applied to
the instrument after each sequence run is completed.
By checking Enable sleep mode, the analyzer will go into Sleep Mode (turn off the UV Lamp) after the
end of a sequence plus a timeout period. This will occur only if no other activity occurs during the time
set by the user (minimum is 5 minutes).
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Figure 3-52: Task Scheduler
Audit Trail
The software has Audit Trail capability to log all actions performed with the instrument by any user. The
timestamp, user, action and details are recorded and stored in the database. The history can also be
sorted by timestamp, user or action for audit view. Details for Alarms will be listed including the
parameter value at the time the alarm occurred.
Figure 3-53: Audit Trail

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SECTION 4
ANALYTICAL PROCEDURES & SUGGESTIONS
This section provides analytical information that can be essential to the proper application of the Antek
MultiTek®. Information provided includes:
• Gas flow and furnace temperature considerations
• Calibration techniques
• Preparation of standards
• Sample handling considerations
• Sample analysis and interpretation of results
• Operational hints
• Important operating factors for different types of samples
System Gas Flow Considerations
The following is a discussion of the system flow of the Antek MultiTek®. Figures 1-1a through 1-4
illustrate all interconnecting tubing and the general location of each flow related component.
NOTE
The Antek MultiTek® utilizes several flowpath configurations depending upon the application (Section 1).
Carrier gas (Ar/He) and Oxygen (O2) are supplied to the system at the rear panel and are routed to the
gas flow controller (GFC) assembly through the inlet manifold. These flow controllers and their
associated sensors provide for control and monitoring of all system gas flows. The carrier gas supplies
GFC1 (Argon or Helium). Oxygen supplies the Carrier Oxygen, Pyro Oxygen, and Ozone Oxygen
GFC2 – GFC4).
The carrier gases, Argon or Helium (GFC1) and Carrier Oxygen (GFC4) are mixed in the gas outlet
manifold and routed to the carrier loop on the rear panel. From the carrier loop, carrier gas is transferred
to the pyrolysis tube to sweep the sample into the heated combustion zone. Oxygen, from the Pyro
Oxygen flow controller (GFC2), is also routed to the pyrolysis tube. This large supply of oxygen
provides for the complete combustion of the sample.
All combustion products, including water, exit the pyrolysis tube via a glass elbow or a cyclone trap.
The cyclone trap is only used in applications (e.g., 737-M) where relatively large quantities of water are
produced during sample combustion. Water is removed from the sample stream by the membrane dryer.
The dried gas stream is routed to the N-S Modules for detection. For IC analysis, the gas stream
bypasses the dryer going directly to the IC Module.
Some systems require ozone for the reaction and detection of nitric oxide (NO). Oxygen, from the
Ozone Oxygen gas flow controller (GFC3), is supplied to the Ozone Generator. Systems containing only
a sulfur detector (MultiTek® S or LLS) do not require ozone, thus this part of the flow system is omitted.

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For systems containing only a sulfur detector (MultiTek® S or LLS) the dried combustion gases are
routed directly to the fluorescence sulfur detector and exposed to ultraviolet radiation. For systems
containing only a nitrogen detector (MultiTek® N), the dried combustion gases are routed directly to the
Chemiluminescence nitrogen detector and mixed with ozone. In systems containing both nitrogen and
sulfur detectors (MultiTek® NS), the dried combustion gases are first routed to the sulfur detector and
then to the nitrogen detector.
The reacted gases exit the detector module(s) and are routed through a MoleculiteTM/DrieriteTM
scrubber where all excess ozone is converted to O2. The total exhaust gases are then routed to portion of
the membrane dryer to sweep away excess water and then to vent.
Furnace Temperature
Pyro-Furnace
The function of the pyro-furnace is to provide the thermal energy to completely oxidize any material to
be analyzed by the Antek MultiTek®. The pyro-furnace is intended to operate at extremely high
isothermal temperatures. The temperature set points are entered via MultiTek® Software as described in
Section 3 of this manual.
All temperatures are in degrees centigrade (°C). Most analyses may be successfully accomplished at
pyro-furnace temperatures of 1050°C to 1100°C. These are quite common for aqueous or inert materials.
Some special applications may be conducted at lower furnace temperatures. As a general rule, the
pyro-furnace temperature need not be changed on a regular basis.
Programmable Inlet Furnace (Model 737-M)

The function of the programmable inlet furnace is to provide the thermal energy for the volatilization of
solid, semisolid, and viscous liquid materials to be analyzed by the Antek MultiTek®. The
programmable inlet furnace is intended to operate over a wide range of temperatures. The temperature
levels, time delays, and ramp rates are entered in the timed events in the Method screen.
All temperatures are in degrees centigrade (°C), delay times are in seconds, and ramp rates are in
degrees centigrade per minute (°C/min).
Most analyses may be successfully accomplished with programmable inlet furnace temperatures
between 100°C and 900°C. The exact temperature program required for the analysis of any specific
material must be individually determined. For example, a general temperature program for the analysis
of polyolefins would be:
— 100°C for 30 seconds;
— ramp at 50°C/min to 250°C, hold 250°C for 60 seconds;
— ramp at 100°C/min to 750°C, hold 750°C for 60 seconds; and
— cool to the original 100°C set point.
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This set of parameters will successfully analyze most polyolefinic materials. However, minor
adjustments may be necessary to obtain the optimum repeatability, accuracy, and analysis time for a
particular sample material.
As a general rule, once the temperature program parameters for a specific material have been
determined, they need not be changed.
Sample Handling
The concentration of nitrogen/sulfur in the sample and the chemical and physical composition of the
sample matrix itself will greatly determine the amount of care necessary in handling samples prior to
analysis with the Antek MultiTek®. Improper sample handling may yield results which are non-
repeatable and inaccurate. For example, touching injection needles or sample boats may introduce
nitrogen/sulfur compounds into the system and produce erroneous results.
Liquid Sample Materials

Liquid sample materials are among the easiest to contaminate or alter for a variety of reasons. Most
potential contaminates are soluble in some liquids, and the liquid sample may be placed in almost any
container. Some liquid matrices are volatile, and some are extremely hygroscopic. Many variables must
be considered when analyzing liquid sample materials. The following are some suggestions which will
help in reducing analytical error.
1. Trace Nitrogen/Sulfur/Halides - Extreme care must be taken not to contaminate the sample.
Trace amounts of nitrogen/sulfur/halides in a sample material may be changed by the slightest
mistakes in sample handling. The sample may need to be refrigerated and all glassware, syringes,
and any other apparatus used should be clean and free of nitrogen/sulfur/halides compounds to
avoid possible contamination. If trace nitrogen/sulfur/halides analysis is to be accurate, the
highest level of analytical technique should be used.
2. Volatile Nitrogen/Sulfur/Halides - If a liquid sample material contains volatile
nitrogen/sulfur/halides compounds, the sample should be refrigerated and tightly capped while
waiting for analysis. This will prevent loss of nitrogen/sulfur/halides and erroneous results.
3. Volatile Matrix - Most liquid sample materials are volatile to some extent. However, samples of
volatile organic matrices should be kept in a sealed container and refrigerated prior to analysis.
Evaporation of solvent is a major cause of analytical error in elemental analysis.
4. Reactive Nitrogen/Sulfur/Halides or Matrix - Some nitrogen, sulfur and halides compounds
and some matrices may be reactive. Extreme care should be taken when choosing a container for
these materials. Use only inert sample containers to prevent analytical errors.
As a general rule, liquid sample materials require very little pre-analysis preparation. Some materials
may need dilution or filtration, but generally no sample preparation is necessary.

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Solid Sample Materials

Solid sample materials are easier to handle and less likely to be contaminated or altered. However, solid
materials are subject to contamination by various means, and care should be taken to prevent analytical
error. Some solid materials may be contaminated by their container or by exposure to liquids or vapors.
Many solid matrices are extremely hygroscopic. Therefore, these variables must be considered when
analyzing solid sample materials. The following are some suggestions which will help in reducing
analytical error.
mistakes in sample handling. The sample may need to be refrigerated and all glassware, spatulas,
and any other apparatus used should be clean and free of nitrogen/sulfur/halides compounds to
avoid possible contamination. If trace nitrogen/sulfur/halides analysis is to be accurate, the
highest level of analytical technique should be used.
2. Volatile Nitrogen/Sulfur/Halides - If a solid sample material contains volatile
nitrogen/sulfur/halides compounds, the sample should be refrigerated and tightly capped while
waiting for analysis. This will prevent loss of nitrogen/sulfur/halides and erroneous results.
3. Hygroscopic Matrix - Most solid sample materials are hygroscopic to some extent. These
sample materials should be kept in a sealed container or possibly a desiccator prior to analysis.
Adsorption of water is a major cause of analytical error in elemental analysis.
4. Reactive Nitrogen/Sulfur/Halides or Matrix - Some nitrogen, sulfur and halide compounds
and some matrices may be reactive. Extreme care should be taken when choosing a container for
these materials. Use only inert sample containers to prevent analytical errors.
In order to obtain the most accurate and repeatable results, solid sample materials must be very
homogeneous. Therefore, solid materials of a heterogeneous nature must be mixed or homogenized.
This can be accomplished by grinding or mixing the solid material. Extreme care should be taken not to
contaminate or chemically alter the solid material in any way. After grinding, the solid material should
be remixed to eliminate any stratification of the smaller particles.
Gas and Liquefied Gas (LPG) Sample Materials

Gas sample materials are extremely easy to contaminate or alter for a variety of reasons. Most potential
contaminates are soluble in gaseous matrices, and the gas sample may be placed in a variety of
containers. Some gaseous matrices are reactive, and some are extremely hygroscopic. Tubing carrying
sample must be Sulfinert® (or equivalent) treated to prevent loss of Sulfur and Nitrogen in the sample.
Many variables must be considered when analyzing gas sample materials. The following are some
suggestions which will help in reducing analytical error.
mistakes in sample handling. All glassware, syringes, high pressure sample containers, and any
other apparatus used should be clean and free of nitrogen/sulfur/halides compounds to avoid

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possible contamination. If trace nitrogen/sulfur/halides analysis is to be accurate, the highest

level of analytical technique should be used.
2. Volatile Nitrogen/Sulfur/Halides and Matrix - Since all gas samples and all gaseous
nitrogen/sulfur/halides compounds are difficult to contain, the sample should be kept in a leak
free sample container before analysis. This will prevent loss of nitrogen/sulfur/halides and
erroneous results.
3. Reactive Nitrogen/Sulfur/Halides or Matrix - Some nitrogen, sulfur and halide compounds
and some gaseous matrices may be reactive. Extreme care should be taken when choosing a
container for these materials. Use only inert sample containers to prevent analytical errors.
All gas and LPG sample containers should be sufficiently pressurized to provide adequate sample
volume and pressure. Particularly, LPG sample containers should have at least 200 PSI (13 bar)
pressure.
Calibration
Calibration Standard Preparation
In order to analyze an unknown sample, it is first necessary to create a calibration curve using standard
liquid solutions, gas mixtures, or solid materials of known concentration for nitrogen/sulfur/halides.
Synthetic calibration standards of known concentration may be constructed or purchased for comparison
with samples of unknown concentration. Extreme care should be taken in preparing these calibration
materials. Pure substances, nitrogen/sulfur/halides free solvents, clean glassware and syringes, and an
analytical balance (0.1 mg accuracy) are necessary. The construction of synthetic calibration materials is
discussed later in this section.
Final analytical accuracy will improve as the calibration material approaches the sample material with
respect to nitrogen/sulfur/halides concentration and composition of the matrix (solvent). Accuracy will
also improve as the nitrogen/sulfur/halides compounds in the calibration standard approach the
nitrogen/sulfur/halides compounds in the sample material with respect to molecular structure.
Some suitable solvents include: water; toluene; iso-octane; butane; naphtha; methanol; ethanol;
iso-propanol; acetone; methyl ethyl ketone; etc. Some suitable nitrogen compounds include: nitrogen
dioxide; ammonia; nitric oxide; sodium nitrate; ammonium nitrate; pyridine; indole; carbazole;
erucamide; glycine; etc. Some suitable sulfur compounds include: sulfur dioxide; butyl sulfide; carbonyl
sulfide; hydrogen sulfide; dimethylsulfoxide; dibenzothiophene; etc. Some suitable nitrogen/sulfur com-
pounds include: thiourea; P-toluene sulfonamide; phenothiazine, etc.
A series of calibration standards should be constructed to cover the concentration range desired for
sample analysis. Alternatively, various amounts of a single calibration material may be analyzed in some
troubleshooting applications.

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NOTE
Calibration standards have a finite shelf life and should be discarded and reconstructed regularly (1 to 3
months). Calibration standards containing volatile substances should be kept in sealed containers and
refrigerated.
The following examples outline the construction of synthetic calibration materials for liquid, gas, and
solid sample analysis. These examples are intended as guidelines and are not necessarily the best
calibration materials for all analyses.
Liquid Calibration Material

Liquid calibration materials are generally the easiest to construct and analyze. In order to construct a
liquid calibration standard, the subsequent guidelines should be followed:
1. Select a suitable liquid solvent which is relatively free of nitrogen/sulfur/halides contamination
and closely resembles the samples to be analyzed. The solvent should be injected into the
analyzer to ensure that little to no nitrogen/sulfur/halides contamination exists.
2. Select a suitable nitrogen/sulfur/halides bearing material, of known nitrogen/sulfur/halides
concentration, which is soluble in the previously selected solvent. Again, the
nitrogen/sulfur/halides bearing material should resemble the sample material unknown as closely
as possible.
3. Select a concentration range in which to calibrate the system and construct the liquid calibration
standard(s) to cover this range. It is recommended to calibrate the analyzer over a range which
will include all possible sample analyses. If samples are analyzed beyond the calibrated range,
either above or below, the results may not be accurate.
Example:
Assume that the sample to be analyzed is water, and the analytical range of both nitrogen and sulfur is
10 mg/L to 100 mg/L. A suitable calibration material may be constructed with distilled, deionized
water and thiourea (CH 4 N 2 S). A suitable calibration range will be 5 mg/L to 150 mg/L in
order to completely encompass the desired analytical range.
Construct a stock solution of thiourea in water as follows:
1. Carefully weigh, with an analytical balance, 2.718 grams of thiourea.
2. Place the thiourea into a one liter volumetric flask and dilute to volume with distilled, deionized
water.
The resulting solution will contain 1000 mg/L nitrogen and 1145 mg/L sulfur. Portions of this stock
solution may be diluted with distilled, deionized water to produce the various liquid calibration materials
needed. For instance: 1) by diluting 10 milliliters of the stock solution with 90 milliliters of water, the
resulting solution will contain 100 mg/L nitrogen and 114.5 mg/L sulfur and 2) by diluting l milliliter of
the stock solution with 99 milliliters of water, the resulting solution will contain 10 mg/L nitrogen and
11.45 mg/L sulfur.
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Almost any organic or inorganic material may be used to construct calibration standards. Good
laboratory practice should be exercised at all times to ensure precise and accurate analytical data. Highly
oxidized nitrogen and sulfur bearing materials must be handled carefully when considered for use in
standard preparation. For example sulfate compounds require a long residence time in the oxidation
furnace to convert to SO2.
Gas Calibration Material

Gas calibration materials may generally be obtained by three methods: 1) purchased from a local gas
supplier, 2) produced by a commercially available gas blending system, or 3) manually constructed in
small, gas-tight containers. Of these three methods, purchased standards and standards produced by gas
blending systems are usually the most accurate and reliable. The manual construction of gas standards
can be difficult, cumbersome, and inaccurate.
When purchasing or blending gas calibration standards, these guidelines should be followed:
1. Select a suitable gas matrix which is relatively free of nitrogen/sulfur/halides contamination. The
gas should be injected into the analyzer to ensure that no nitrogen/sulfur/halides contamination
exists.
2. Select a suitable nitrogen/sulfur/halides bearing gaseous material, of known
nitrogen/sulfur/halides concentration, which is compatible with the previously selected gas
matrix.
3. Select a concentration range in which to calibrate the system and purchase or blend the gas
calibration standard(s) to cover this range. It is recommended to calibrate the analyzer over a
range which will include all possible sample analyses. If samples are analyzed beyond the
calibrated range, either above or below, the results may not be accurate.
Almost any gaseous organic or inorganic material may be used to construct calibration standards. Good
laboratory practice should be exercised at all times to ensure precise and accurate analytical data.
Solid Calibration Material

Solid calibration materials are generally very difficult to construct since this requires uniformly
distributing a nitrogen/sulfur/halides compound in a solid matrix. This process may be successfully
carried out with some solid materials if great care is taken to ensure homogeneity. However, in most
cases, it is recommended to: 1) purchase the solid calibration materials or 2) use an evaporative liquid
matrix calibration material in place of a solid matrix.
When purchasing or constructing a solid calibration material, these guidelines should be followed:
1. Select a suitable solid matrix which is relatively free of nitrogen/sulfur/halides contamination
and closely resembles the samples to be analyzed. The material should be introduced into the
analyzer to ensure that no nitrogen/sulfur/halides contamination exists.
2. Select a suitable nitrogen/sulfur/halides bearing material, of known nitrogen/sulfur/halides
concentration, which is compatible with the previously selected matrix. Again, the
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nitrogen/sulfur/halides bearing material should resemble the sample material as closely as

possible.
3. Select a concentration range in which to calibrate the system and purchase or construct the solid
calibration standard(s) to cover this range. It is recommended to calibrate the analyzer over a
range which will include all possible sample analyses. If samples are analyzed beyond the
calibrated range, either above or below, the results may not be accurate.
In many cases, it is difficult or impossible to purchase or construct accurate solid calibration materials.
In these circumstances, the use of liquid calibration materials is recommended. In order for a liquid
calibration material to be suitable for solid sample analysis, the following guidelines should be
observed:
1. Select a suitable liquid solvent which is volatile at room temperature and is free of
nitrogen/sulfur/halides contamination. The solvent should be evaporated and the residue
introduced into the analyzer to ensure that no nitrogen/sulfur/halides contamination exists.
2. Select a suitable, non-volatile nitrogen/sulfur/halide bearing material, of known
nitrogen/sulfur/halides concentration, which is soluble in the previously selected solvent. Again,
the nitrogen/sulfur/halides bearing material should resemble the sample material as closely as
possible.
3. Select a concentration range in which to calibrate the system and construct the liquid calibration
standard(s) to cover this range. It is recommended to calibrate the analyzer over a range which
will include all possible sample analyses. If samples are analyzed beyond the calibrated range,
either above or below, the results may not be accurate.
Example:
Assume that the sample to be analyzed is polyethylene for erucamide (C22H440N), a lubricant, and the
analytical range is 100 mg/kg to 1000 mg/kg. The system may be calibrated to yield results with respect
to nitrogen or erucamide. For the purpose of this example and to simplify calculations, the calibration
will be done with respect to erucamide. A suitable calibration material may be constructed with reagent
grade acetone (C3H6O) and erucamide. A suitable calibration range will be 50 mg/kg to 1500 mg/kg in
order to completely encompass the desired analytical range.
Before constructing the liquid calibration material, it is necessary to estimate the required concentration
of erucamide in the acetone matrix. This is accomplished as follows:
1. The sample weight of the polyethylene to be analyzed will be approximately 100 mg.
2. The concentration of erucamide in the polyethylene will be between 100 mg/kg and 1000 mg/kg.
3. This implies that the amount of erucamide present in each 100 mg polyethylene sample will be
between 10 µg and 100 µg.

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Therefore, a calibration solution containing 1 µg erucamide/µL should be constructed. Various micro

liter quantities of this solution may be analyzed to simulate different concentrations of erucamide in the
polyethylene matrix.
Construct the 1 µg/µL erucamide/acetone solution as follows:
1. Carefully weigh, with an analytical balance, 0.100 grams of erucamide.
2. Place the erucamide into a 100 milliliter volumetric flask and dilute to volume with reagent
grade acetone.
The resulting solution will contain 1 µg/µL erucamide. By analyzing different quantities of this solution,
an accurate calibration curve may be constructed. For instance: 1) Place 5 µL of the solution in the
quartz sample boat and allow the solvent to completely evaporate. Analyze the residue as if it were a
polyethylene sample and assume a sample weight of 100 mg. This will simulate a calibration point of 50
mg/kg.; 2) Repeat this procedure with 10, 50, 100, and 150 µL quantities of the solution to simulate
calibration points of 100, 500, 1000, and 1500 mg/kg, assuming a sample weight of 100 mg each time.
Accurately weigh sample unknowns to weight near 100 mg, enter the exact weights of the sample
unknown under the column of the sample table.
Almost any organic or inorganic material may be used to construct calibration standards. Good
laboratory practice should be exercised at all times to ensure precise and accurate analytical data. Solid
materials standards can also be constructed from controlled pilot plant and/or research facility
production.
Standard Calibration Curve(s) for Liquid Materials

In order to generate a standard calibration curve (or curves for dual detector systems) for liquid
materials, select or construct liquid calibration materials as described in the previous section. Ensure that
the MultiTek® has been assembled and tested according to all guidelines set forth in Sections 1 through
3 and that the system is ready for operation.
Follow the example given in Section 3. Perform the individual calibration material injections desired,
and the system will construct the calibration curve(s).
Normally, the precise concentration of each calibration material is input into the system. The
concentration units must be the same for each calibration standard (i.e., ppm, %, mg/L, mg/kg, etc.).
Injecting the same amount of material for calibration standards of differing concentrations is important.
The calibration curve(s) will plot integrated area or peak height on the Y-axis and concentration on the
X-axis.
If various volumes of the same material are used to calibrate the system, enter the mass of
nitrogen/sulfur in place of concentration. For example, a calibration material contains 10 ng/µL
nitrogen, and injections of 5, 10, and 15 µL of this material are introduced into the system. Enter the
absolute mass of nitrogen injected; 50 ng, 100 ng, and 150 ng. The calibration curve(s) will plot
integrated area or peak height on the Y-axis and absolute mass (ng) on the X-axis.
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The integration produced by the system will be ratioed to the user entered values for construction of the
calibration curve. However, keep in mind that all values entered for the same calibration curve must
have the same concentration units.
The proper procedure for manual injection of a calibration standard is as follows:
1. Perform the data entry as outlined in Section 3.
2. Carefully fill a clean 10 or 25 µL syringe to the 5 µL mark with the calibration solution and
remove the syringe needle from the solution. Samples of 5 to 20 µL are large enough for most
analyses.
NOTE
For the first replicate of each solution, it will be necessary to rinse the syringe with the solution several
times to prevent contamination and inaccurate analyses.
3. Draw the entire sample back into the syringe barrel until the lower liquid meniscus comes to the
2 µL mark.
4. Insert the syringe needle through the inlet septum up to the syringe barrel and allow the furnace
to burn all sample residue from the syringe needle.
5. Select the START button and inject the sample into the furnace at a controlled rate of 1 µL/sec.
NOTE
A mechanical means of sample introduction (such as the Antek Model 735 Syringe Drive, or Liquid
Autosampler) is strongly recommended in order to enhance reproducibility and accuracy, and to avoid
damage to the instrument by coking (sooting) the pyrotube, dryer and detector modules.
6. When the entire sample has been combusted and the nitrogen/sulfur/halides quantitated, a record
of the raw data with the standard concentrations will be stored in the calibration table. Withdraw
the syringe needle from the furnace.
7. Repeat the determination of each calibration sample at least three times.
The MultiTek® Software will automatically construct the calibration curve for each detector as described
above. This calibration curve and data may be observed in the Calibration panel of the Method Screen.
Standard Calibration Curve(s) for Gaseous Materials

In order to generate a standard calibration curve (or curves for dual detector systems) for gaseous
materials, select gas calibration materials as described above. Ensure that the MultiTek® has been
assembled and tested according to all guidelines set forth in Sections 1 through 3 and that the system is
ready for operation.
Calibration is done manually by following the example given in Section 3. Perform the individual
calibration material injections desired, and the system will construct the calibration curve(s).

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concentration units must be the same for each calibration standard (i.e., ppm, %, µg/m3, etc.). It is
extremely important that the same amount of material is injected each time. For example, calibration
materials with a nitrogen concentration of 5 ppm, 10 ppm, and 50 ppm are injected. By injecting exactly
l0 mL of each material, the calibration curve(s) will plot area or peak height on the Y-axis and
concentration (ppm) on the X-axis.
If various volumes of the same material are used to calibrate the system, enter the mass of
nitrogen/sulfur in place of concentration during the dialog. For example, a calibration gas contains 10
ppm nitrogen (6.25 ng N/mL), and injections of l, 5, and 10 milliliters of this material are introduced
into the system. Enter the absolute mass of nitrogen injected; 6.25 ng, 31.25 ng, and 62.5 ng. The
calibration curve(s) will plot area or peak height on the Y-axis and absolute mass (ng) on the X-axis.
The integration will be ratioed to the user entered values for construction of the calibration curve.
However, keep in mind that all values entered for the same calibration curve must have the same
concentration units.
The proper procedure for manual injection of a calibration standard is as follows:
2. Carefully fill a clean gas tight syringe or the gas sampling valve with the desired volume of the
calibration gas. Samples of one to five mL are large enough for most analysis with a gas tight
syringe.
NOTE
For the first replicate of each gas, it will be necessary to purge the sampling device with the gas
to prevent contamination and inaccurate analyses.
3. If a gas sample valve is used, proceed directly to step 4. If a gas tight syringe is used, insert the
syringe needle through the inlet septum up to the syringe barrel and allow the furnace to burn all
sample residue from the syringe needle.
4. Select the START button, wait five seconds, and inject the sample into the furnace at a
controlled rate, 0.5 to 1 mL/second when using a gas tight syringe or 20 – 25 mL/minute if using
the Model 734.
NOTE
A mechanical means of sample introduction (such as the Antek Model 734 Gas/Liquid Sampling
System) is strongly recommended in order to enhance reproducibility and accuracy.
5. When the entire sample has been combusted and the nitrogen/sulfur/halides quantitated, a record
of the raw data with the standard concentrations will be stored in the calibration table. Withdraw
the syringe needle from the furnace or return the gas sample valve to the load position.
6. Repeat the determination for each calibration level at least three times.

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above. This calibration curve and data may be observed in the Calibration screen.
Standard Calibration Curve(s) for Solid Materials

In order to generate a standard calibration curve (or curves for dual detector systems) for solid materials,
purchase or construct solid calibration materials as described above. Ensure that the MultiTek® has been
assembled and tested according to all guidelines set forth in Sections 3 and that the system is ready for
operation.
Perform the individual calibration material analyses desired, and the software will construct the
calibration curve(s).
concentration units must be the same for each calibration standard (i.e., ppm, %, mg/l, mg/kg, etc.).
Ensure that the correct sample weight is input for each calibration material. For example, calibration
materials with a nitrogen concentration of 50 ppm, 100 ppm, and 500 ppm are analyzed. By entering the
correct sample weight (in milligrams) of each material, the calibration curve(s) will plot integrator
counts/mg of sample on the Y-axis and concentration (ppm) on the X-axis.
If various weights of the same material are used to calibrate the system, enter the mass of nitrogen/sulfur
in place of concentration and enter a sample weight of 1 for each analysis. For example, a calibration
material contains 1000 mg/kg nitrogen, and analyses of 50, 100, and 150 milligrams of this material are
introduced into the system. For concentration data, enter the absolute mass of nitrogen introduced: 50,
100, and 150. The calibration curve(s) will plot integrator counts on the Y-axis and absolute mass (mg)
on the X-axis.
The proper procedure for manual introduction of a solid calibration standard is as follows:
1. Carefully weigh the solid calibration material or introduce the proper amount of the liquid
calibration material into a clean quartz sample boat.
NOTE
If liquid calibration materials are used, extreme care should be taken to ensure that all solvent
is completely evaporated before introducing the quartz sample boat into the furnace.
3. Place the quartz sample boat into the inlet portion of the MultiTek® and allow 20 seconds for the
gas flows and pressure to stabilize.
4. Select the START button to begin the temperature program or start the sample boat drive.
NOTE
A mechanical means of controlled sample introduction (such as the Antek Model 735 Sample
Drive) is strongly recommended for systems utilizing the Sample Boat Inlet Methods (i.e. Model
740 Multi-Matrix systems) in order to enhance reproducibility and accuracy.

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5. When the entire sample has been combusted and the nitrogen/sulfur/halides have been
quantitated, a record of the raw data, integrator area per milligram of sample (internally
calculated), and the standard concentrations will be stored in the calibration table. Withdraw the
quartz sample boat from the furnace if using the Multi-Matrix or allow the Model 737-M to
complete the cool down cycle, and then remove the boat.
6. Repeat the determination for each calibration material at least three times.
above. This calibration curve and data may be observed at any time in the Calibration Screen.
NOTE
For more information about making standards see Appendix – Making Standards & Common
Conversions.
Sample Analysis
Sample Analysis
In order to analyze samples, it is necessary to generate a standard calibration curve (or curves for
multiple detector systems) as described in the Calibration section. Ensure that the MultiTek® has been
assembled and tested according to all guidelines set forth in Sections 1 – 3, and that the system is ready
for operation.
Sample materials are analyzed in the same manner as the calibration materials discussed in Calibration.
If the sample analysis is to be done manually, follow the programming example given in Section 3.
Perform the individual sample material injections desired, and the system will use the resulting
integrated counts to determine the concentration based on the calibration.
If the sample analysis is to be done automatically, see Section 3. When all sample injections are com-
pleted, the sample data may be viewed on the Sample screen.
Calculation and Interpretation of Results

The MultiTek® Software compares the raw data generated from the unknown samples to the calibration
curve(s) calculated internally from the analysis of standards. A concentration is reported for all samples.
The raw data, calibration curve data, and the calculated concentrations can be viewed or printed with the
columns selected in the Display Preferences section of the Edit menu. Reported concentrations will be in
the same units used for calibration standards.

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Operational Hints
The following is a collection of operational hints which are intended to supply the user with practical
information concerning many aspects of the Antek MultiTek®.
General
1. The time required to reach operational status from a cold start-up is approximately 45 minutes.
2. The UV source requires at least 30 minutes for stabilization.
3. Not all glass components of the analytical system are quartz. Some items, such as the cyclone
trap and glass elbow, are made of Pyrex™ and should not be exposed to extreme heat.
4. If the MultiTek® is regularly modified or if accessories are added or removed, the system should
be checked for leaks.
5. Supply gas cylinders should be replaced when the cylinder pressure reaches 200 PSI (13 bar).
This will prevent contamination of the analytical system.
Analytical
1. Always ensure that the gas flows and temperatures are correct before introducing sample
materials into the system.
2. Do not touch any sample introduction device (i.e., syringe needle, quartz sample boat, etc.) with
fingers. This may contaminate the device with nitrogen, sulfur and/or halides.
3. Quartz sample boats, syringes, syringe needles, sample introduction tubes, etc. should be cleaned
on a daily basis to prevent contamination and errant analytical results.
4. Avoid removing the sample introduction device (i.e., syringe, quartz sample boat, etc.) before the
sample material is completely combusted.
5. A wait of at least two to three minutes between sample introductions is recommended. This will
allow the membrane dryer to regenerate.
6. Frequently inspect the inlet and exit portions of the pyrotube for any carbon residue. If residue is
found, immediately clean the residue from the system and check for gas leaks, proper gas flows,
appropriate temperature profile, correct sample introduction technique, and suitable sample size.
7. When entering Timed Events, ensure that the cycle time is long enough to allow all timed events
to be completed before the next analysis is started.
8. When using vials for liquid samples, ensure that the caps are properly seated. This will prevent
evaporation and provide for accurate sampling.
9. When using an autosampler, ensure that at least two rinses are purged through the syringe
assembly during the sample rinse function. The autosampler parameters may need adjustment
when changing from non-viscous to viscous sample materials.
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10. In order to obtain a more stable electronic baseline and better repeatability, it may be necessary
to lower the PMT voltage. This must be considered in relation to sample size with materials of
very low nitrogen/sulfur/halides concentration.
11. If the ambient room temperature changes more than 10°C during a normal work period, the
thermoelectric cooler may allow the PMT temperature to change. The PMT temperature should
periodically be monitored.
12. When using the Model 737-M Temperature Programmable Inlet, ensure that the initial
temperature is low enough to prevent premature evaporation of the sample material. This is
particularly important when using liquid calibration materials for solid sample analysis.
Additionally, the following temperature programming guidelines may be helpful:
a. The initial temperature level (Level 1) should be approximately 25°C below the temperature
of initial detector response.
b. The first temperature ramp (Ramp 1) should begin at a time suitable to provide for smooth
sample volatilization, usually before the detector(s) show a response.
c. The next temperature level (Level 2) should begin before the detector response reaches full
scale, as indicated by the appropriate signal level.
d. The next temperature ramp (Ramp 2) should begin as the detector response begins to
decrease and before the detector response decreases below mid-scale, as indicated by the
appropriate signal level.
e. The final temperature level should be approximately 100°C above the temperature at which
the signal level returns to baseline.
13. Calibrate the MultiTek® only over the range necessary to completely encompass the samples to
be analyzed. If the calibration range is too large, an inaccurate or nonlinear calibration curve may
result. Always operate within the calibrated range, extrapolation is not recommended.
14. Confirm the validity of all calibration curves on a daily basis by analyzing at least one material
of known concentration. The result should be within normal analytical error.
15. Volatile sample matrices may be stabilized by refrigeration or dilution with a higher boiling
point solvent.
16. If integrated areas are too high (flat top peaks) the signal amplifiers and/or integrator may
electronically saturate and produce inaccurate results. Integrated area may be reduced by
changing the PMT Voltage or sample size.
17. When constructing a calibration curve, select a PMT Voltage setting which will yield at least
three times baseline noise for the lowest point on the calibration curve.

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Important Factors for Nitrogen and Sulfur in Certain Sample Types
As an aid to the analyst, a collection of Helpful Hints has been assembled for the various Antek
MultiTek® Configurations. Use these guidelines in accordance with your particular instrument
configuration and sample matrix.
Nitrogen & Sulfur in Liquid Hydrocarbons (Direct Injection)

1. Furnace Temperature: Set to 1050°C. The use of quartz chips in the combustion zone of the
pyrotube is required. The entire sample flow path must be leak free.
2. Needle Tip Position during Injection: The needle tip should be presented fully into the hottest
part of the inlet area of the furnace. Assembly of apparatus to manufacturer's specification and
full insertion of the needle will assure this.
3. Injection Peak/Needle Blank: Avoid integration of any baseline upset caused by the needle
penetration of the septum. After the sample specimen has been measured into the syringe, retract
the plunger to form an air gap up to approximately the 10% scale mark of the syringe barrel.
Insert the syringe needle into the injection inlet and allow the needle/septum blank to dissipate.
Reset the instrument baseline or enable integration, if required, prior to the injection of the
syringe contents.
4. Residence Time of Needle in Furnace: Residence time of the needle in the furnace must be
consistent following the injection of the sample. For direct injections, it is recommended that the
needle remain in the furnace until the instrument returns to baseline and the analysis of the
injected material is complete.
5. Injection Size: As a general rule, larger sample sizes are required for measurement of lower
levels of nitrogen/sulfur. While determining the best sample size, frequently check for evidence
of incomplete combustion (coking or sooting) that may be present in the sample path. Control
coking by slowing the injection rate of the sample from the syringe, and/or increasing the Pyro-
Oxygen or Inlet Oxygen supply. Suggested sample sizes are as follows:
Trace to 5 ppm 10 – 20 µL
5 ppm to 100 ppm 10 – 15 µL
100 ppm to percent 5 – 10 µL
6. Injection Rate and Frequency: Discharge contents of the syringe into the furnace at a slow
rate, approximately 1 µL/second. Frequency of injection can vary depending upon sample and
syringe handling techniques, rate of injection and needle in furnace residence time. Typical
injection frequency allows at least 2.5 minutes between injections.
7. Flowpath, Leak Check and Back Pressure: The sample flowpath must be leak free when
pressure tested per the manufacturer's recommended procedure. Flowpath back pressure during
normal operation can range from 5 – 14 kPa.

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8. Gas Flow Settings: Gas supplies to various points in the sample path must be consistently
controlled to allow for smooth, complete combustion of the sample.
Typical Gas Flows

Inlet Carrier Flowmeter Settings* 120 – 140 mL/min
Inlet Oxygen Flowmeter Setting 10 – 40 mL/min
Furnace Oxygen Flowmeter Setting 400 – 450 mL/min
Ozone Generator Flowmeter Setting** 25 – 35 mL/min
*Helium or argon may be used as a carrier gas.
**Flow to ozone generator (optional)
9. Membrane Dryer Purge: Water produced during the combustion of the sample is removed by
the membrane dryer. This water must then be purged from the membrane dryer. For an apparatus
that utilizes a desiccant scrubber to provide the membrane dryer purge gas, replace the drying
agent when color change (blue to pink) indicates. When an auxiliary gas flow is used, set
membrane dryer purge flow at 200 – 350 mL/minute.
10. Sample Homogeneity/Calibration Response: Prior to analysis, mix samples and calibration
materials well. Minimum response should be no less than 2 – 3 times baseline noise for the
lowest point on the calibration curve. The highest concentration point on the curve must be
below the saturation point of the detector. Use a maximum response of 12 – 14 million counts as
a guideline. Adjust PMT voltage and/or sample size accordingly.
11. Baseline Stability: Prior to analysis, especially when analyzing low levels, be certain that the
detector baselines are stable and noise free. For a given photomultiplier tube, PMT voltage may
be adjusted to insure maximum sensitivity while maintaining a stable, noise-free baseline.
12. Calibration Materials/Standard Curve Construction: Prepare calibration standards with
solvent materials that have minimum or no contamination relative to the concentration
anticipated in the sample unknown. Correct for contribution from solvent materials and impurity
of source material. Use calibration curves that bracket the expected levels in the sample
unknown as a guide to prepare standards. Do not force the calibration curve through the 0,0 axis,
unnecessarily. Construct standard concentrations that will yield a calibration curve that is linear
and that does not exceed the dynamic range of the detector (use a correlation coefficient of 0.999
and 1 – 2 orders of magnitude as a guideline). The curve should yield a value that can be used to
calculate sulfur/nitrogen content in the sample on a mass/mass basis.
Nitrogen & Sulfur in Hydrocarbons (Boat-Inlet)

1. Furnace Temperature: Set to 1050°C. The use of quartz chips in the combustion zone of the
pyrotube is recommended. The entire sample flow path must be leak free.
2. Boat Path: The boat should be presented fully into the inlet area of the furnace. Assembly of
apparatus to manufacturer's specification assures this.

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3. Boat Entry Rate and Residence Time of Sample in Furnace: Insert the boat into the furnace
using a drive rate of 1 µL/second. Additional slowing of boat speed or briefly pausing the boat in
the furnace may be necessary to assure complete sample combustion. The boat should emerge
from the furnace soon after detection is complete. Boat in furnace residence times can vary
depending on sample volatility and levels measured. Typical boat in furnace residence times
range between 15 – 45 seconds.
4. Injection Size: As a general rule, larger sample sizes are required for measurement of lower
levels. While determining the best sample size, frequently check for evidence of incomplete
combustion (coking or sooting) that may be present in the sample path. Control sooting by
slowing the boat speed into the furnace, increasing the length of time the boat is in the furnace,
and/or increasing the Pyro-Oxygen supply. Suggested sample sizes are as follows:
5 ppm to 100 ppm 10 – 15 µL
5. Injection Rate and Frequency: Discharge contents of the syringe into the boat at a slow rate
(approximately 10 µL/second) being careful to discharge the last drop. Use of Cerafelt in the
sample boat to aid quantitative delivery is advised. Frequency of injection can vary depending
upon boat speed, level being determined, furnace residence time, and cooling capacity of the
boat loading area. Typical injection frequency allows at least 2.5 minutes between injections.
6. Boat Temperature at Time of Sample Introduction: Sample volatility must be addressed; be
sure boat temperature has returned to ambient or sub-ambient temperatures prior to introduction
of sample into boat. Let boat rest at least 45 seconds in cooling area between injections. Some
sulfur may be measured as the sample evaporates as the boat approaches the furnace. Sub-
ambient temperature can reduce this evaporation.
7. Sample Flowpath: Leak Check and Back Pressure: The sample flowpath must be leak free
when pressure tested per the manufacturer's recommended procedure. Flowpath back pressure
during normal operation can range from 5 – 14 kPa.
Typical Gas Flows


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materials well. Minimum response should be no less than 2 – 3 times the baseline noise for the
lowest point on the calibration curve. The highest point on the curve must be below the
saturation point of the detector. Use a maximum response of 12 – 14 million counts as a
guideline. Adjust PMT voltage and/or sample size accordingly.
11. Boat Blank/Baseline Stability: Prior to analysis, especially when analyzing low levels, advance
the boat (with Cerafelt) into furnace to assure that no contamination is present in the boat or on
the inside areas of the pyrotube near the injection area. Heat the empty boat and Cerafelt in the
furnace to assure that boat and Cerafelt are clean, and then rapidly move boat out to injection
area.
NOTE
If the hot boat being returned to injection area causes detection, repeat the boat in and out cycle, until
no sulfur/nitrogen is measured.
For a given photomultiplier tube, PMT voltage may be adjusted to ensure maximum sensitivity
while maintaining a stable, noise-free baseline.
solvent materials that have minimum or no contamination relative to the concentration of
anticipated in the sample unknown. Correct for nitrogen/sulfur contribution from solvent
materials and impurity of source material. Use calibration curves that bracket the expected levels
in the sample unknown as a guide to prepare standards. Do not force the calibration curve
through the 0,0 axis, unnecessarily. Construct standard concentrations that will yield a
calibration curve that is linear and that does not exceed the dynamic range of the detector (use a
correlation coefficient of 0.999 and 1 – 2 orders of magnitude as a guideline). The curve should
yield an estimated value that can be used to calculate sulfur/nitrogen content in the sample on a
mass/mass basis.
Nitrogen & Sulfur in Aqueous Samples (Direct Injection)

1. Furnace Temperature: Set to 1050ºC - 1100ºC. The use of quartz chips in the combustion zone
of the pyrotube is required. The entire sample flow path must be leak free.
2. Needle Tip Position during Injection: The needle tip should be presented fully in, or very near,
the hottest area of the furnace. Assembly of apparatus to manufacturer's specification and full
insertion of the needle will assure this.

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3. Needle Blank: The septum/needle blank is important. Error due to this can be avoided by
inserting the syringe needle into the hot inlet and allowing the needle septum blank to dissipate
before injecting the sample.
4. Injection Size: As a general rule larger sample sizes may be required for measurement of lower
levels of nitrogen or sulfur. While determining the best sample size, frequently check for
evidence of incomplete combustion (evaporating) that may be present in the sample path. When
sample sizes larger than 5 µL are used, control by slowing the injection rate of the sample from
the syringe, and/or increasing the Pyro-Oxygen or Inlet Oxygen supply. Suggested sample sizes
are as follows:
Trace to 5 ppm 10 - 20 µL
5 ppm to 100 ppm 10 - 15 µL
100 ppm to percent 5 - 10 µL
NOTE
Samples containing high levels of inorganic nitrogen/sulfur compounds may require the use of a Boat
Inlet.
5. Rate of Injection into the Furnace: Discharge contents of the syringe into the furnace at a slow
rate, approximately 1 µL/ second.
6. Residence Time of Needle in Furnace: Residence time of the needle in the furnace must be
consistent following the injection of the sample. For manual direct injections it is recommended
that the needle remain in the furnace until the analysis of the injected material is complete.
7. Analysis Rate/Sample Dilution: Analyze samples 2.5 to 3 minutes apart. Dilution of water
matrix samples is often required. Dissolved solids and salts can often cause the syringe needle to
become plugged as the material is vaporized at the needle tip.
Typical Gas Flows
Inlet Oxygen Flowmeter Setting120 – 140 mL/min
Furnace Oxygen Flowmeter Setting400 – 450 mL/min
Ozone Generator Flowmeter Setting**25 – 35 mL/min
In some aqueous applications inert carrier can be omitted.
9. Standardization Material: Final analytical accuracy will improve as the calibration material
approaches the sample material with respect to nitrogen/sulfur concentration and composition of
the matrix (solvent). Accuracy will also improve as the compounds in the calibration standard
approach the nitrogen/sulfur compounds in the sample material with respect to molecular
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structure. Almost any organic material may be used to construct calibration standards, but greater
care must be used to match inorganic standards.
lowest point on the calibration curve. Maximum response should not be greater than the
guideline. Adjust PMT Voltage and/or sample size accordingly.
11. Baseline Stability: Prior to analysis, especially when analyzing low levels, be certain that the
detector baselines are stable and noise free. For a given photomultiplier tube, PMT voltage may
be adjusted to insure maximum sensitivity while maintaining a stable, noise-free baseline.
Nitrogen & Sulfur in Aqueous Samples (Boat Inlet)

1. Furnace Temperature: Set to 1050ºC - 1100ºC. The use of quartz chips in the combustion zone
of the pyrotube is recommended. The entire sample flow path must be leak free.
2. Boat Path: Sample in boat should be presented fully in, or very near, the hottest area of the
furnace. Assembly of apparatus to manufacturer's specification assures this.
3. Residence Time of Sample in Furnace: Slowing boat speed or briefly pausing the boat in the
furnace may be necessary to assure complete sample combustion. A boat drive rate of 1
µL/second is suggested. The bigger the sample, the slower the speed should be. Samples
containing high levels of inorganic nitrogen/sulfur compounds may require several minutes in
the furnace.
Typical Gas Flows
*Helium or argon may be used as a carrier gas. In some aqueous applications,
inert carrier gas can be omitted
5. Analysis Rate: Analyze samples 2.5 to 3 minutes apart.

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6. Injection Size: As a general rule larger sample sizes may be required for measurement of lower
levels of nitrogen or sulfur. While determining the best sample size, frequently check for
evidence of incomplete combustion (evaporation) that may be present. When sample sizes larger
than 5 µL must be used, control by slowing boat speed into the furnace, increasing the length of
time the boat is in the furnace and/or increasing the pyro-oxygen supply. Suggested sample sizes
are as follows:
Trace to 5 ppm 10 - 20 µL
5 ppm to 100 ppm 10 - 15 µL
100 ppm to percent 5 - 10 µL
7. Rate of Injection into Boat: Discharge contents of the syringe into the boat at a slow rate
(approximately 10 µL/ second) being careful to discharge the last drop. Use of Cerafelt in the
sample boat to aid quantitative delivery is advised.
8. Standardization Material: Final analytical accuracy will improve as the calibration material
approaches the sample material with respect to nitrogen/sulfur concentration and composition of
the matrix (solvent). Accuracy will also improve as the nitrogen/sulfur compounds in the
calibration standard approach the nitrogen/sulfur compounds in the sample material with respect
to molecular structure. Almost any organic material may be used to construct calibration
standards, but greater care must be used to match inorganic standards.
nitrogen or sulfur may be measured as the sample evaporates as it approaches the furnace. Sub-
ambient temperature can reduce or control this evaporation.
lowest point on the calibration curve. Maximum response should not be greater than the
guideline. Adjust PMT Voltage and/or sample size accordingly.
the boat (with Cerafelt) into the furnace to assure that no contamination is present in the boat or
on the inside areas of the pyrotube near the injection area. Heat the boat and Cerafelt in the
furnace to assure that both the boat and Cerafelt are clean, and then rapidly move boat out into
injection area.
NOTE
If the hot boat being returned to injection area causes nitrogen and/or sulfur to be detected, repeat
until empty boat enters furnace and no response is seen.
For a given photomultiplier tube, PMT voltage may be adjusted to insure maximum sensitivity
while maintaining a stable, noise-free baseline.

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Nitrogen & Sulfur in Gaseous & Liquefied Hydrocarbons (Gas/LPG)

1. The Antek MultiTek® must be fully stabilized and in standby condition ready for analysis prior
to sample injection.
2. Sample valves should remain in the load (full counter clockwise on a Model 734 manual gas
sampling system) position except during sample analysis.
3. Once the selected sample valve has been filled and allowed to equilibrate, sample injection
should be accomplished by applying a firm, smooth clockwise rotation to the sample valve. This
function will be performed by the software for the Model 734 automatic gas sampling system.
4. Leave the sampling valve in the inject position until analysis is complete (instrument has
returned to baseline and integration has finished).
5. The length of time required for detector response will depend upon the type of pyrotube utilized,
carrier gas flow rates, sample size, sample introduction line length and nitrogen and/or sulfur
concentration. From 30 seconds to 1.5 minutes can be typical.
6. Model 734 carrier gas flows can be used to manipulate sample combustion and detection
characteristics.
WARNING
Excessive carrier flow rates greater than ≥25 mL/min can cause incomplete sample combustion (sooting
- coking).
7. Allow at least three minutes between injections to allow the membrane dryer to regenerate.
8. Sample cylinders containing liquefied gases must contain sufficient pressure (>200 PSI) to allow
the transfer of sample to the 734 without the formation of "bubbles" in the transfer tubing and
sight glass.
WARNING
Do not exceed the overall pressure rating (900 PSI) of the sample inlet system or the capacity of the
sample transfer cylinder, quick connects, and other transfer lines and fittings.
9. Use standard gas flow conditions for your Antek analyzer.

Typical Gas Flows
Inlet Oxygen Flowmeter Setting** 0 – 20 mL/min
Ozone Generator Flowmeter Setting*** 25 – 35 mL/min
**In some applications, inlet oxygen should be omitted.
***Flow to ozone generator (optional)

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10. The use of a filtering device prior to sample introduction is strongly recommended. This can
greatly extend valve service and prevent transfer line (tubing) plugging.
CAUTION
Particulate matter (debris) contained in samples can obstruct sampler tubing and/or cause damage to
injection valves. An inert filter device can minimize this damage.
11. The use of flowpath components with enhanced metal passivation treatments (Sulfinert™ or
Silicosteel™) can enhance the analysis of low level contaminations.
12. The injection of liquids (iso-octane, toluene, other volatile liquids, etc.) is not advised.
13. Routinely inspect user installed transfer lines and fittings used to connect the sample container to
the sample inlet system for leaks and stress weakening that can be caused by frequent bending,
age or use.

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SECTION 5
IC SAMPLER CONTROL OPERATION
IC Sampler Control Software
Connect to Instrument
Launch the IC Sampler Control software by double clicking the desktop shortcut to
IcSamplerControl.exe. The initial screen is shown below. Note the screen indicates no MultiTek® has
been claimed (connected) by the software. The About screen displays the software version; Firmware
version and Serial number are displayed when connected to an instrument.
Figure 5-1: Software Connection
Window Layout of the IC Sampler Control Software
The main window has the following:
• Title Bar
o Displays “Software Name - Instrument Name <(offline)>”
• Toolbar
o Displays IP address, current State and Warning/Alarm status of the connected instrument
o Frequently used command buttons (connect, instrument configuration, sequence abort,
diagnostics and software screen shrink/restore)

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• Workspace areas for control of the instrument:

o Method : Method version dropdown list and currently applied version box (if checked)
 Buttons to Save or Print the method, Apply (send) the method to the instrument,
or Run sample.
o About button will display Software version; Instrument Firmware version and Serial
number are displayed if connected to an instrument.
o Rinse: Skip initial rinse, Post run rinse cycles, Steam rinse and Steam rinse time
(seconds).
o Controls: System blank run check box allows the user to run functional tests of the
MultiTek® without a sample being loaded into the boat. Save gas check box to reduce
gas flow after a sequence is run. Pump scrubber solution time
o Running Status: Running sample number, Running injection number, Run state and
System pressure (kPa) are displayed.
• Workspace Tabs: For each component of method
 Hardware settings
 Timed events
 Liquid autosampler
 Sequence
 Comments
• Status Bar, contains
o Computer name
o Computer IP address
o Computer physical address (MAC)
To view the available MultiTek® analyzers, click Connect to will bring up the Connect to instrument
window (figure 5-2). The software will automatically search to find all the MultiTek® instruments
connected to the LAN.
Figure 5-2: Connect to Instrument
The Connect to Instrument window will then show all MultiTek® instruments connected on the LAN
plus the status and availability of each analyzer (Figure 5-3).

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Select the desired instrument and then click Connect.
NOTE
If the software has already claimed an instrument (online mode) or the highlighted instrument row
has been claimed by a different PC, the Connect button in the “Connect to Instrument” screen will be
disabled. No password or User ID is required to claim the instrument.
Figure 5-3: Connect to Instrument
The main software screen will load and display the real time information of the claimed instrument
(Figure 5-4). The method version of the software will be displayed as well as the current state and the
alarm status of the instrument. To see the software version, connected instrument firmware version and
serial number click About (Figure 5-5).
Figure 5-4: IC Sampler Control Screen

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Figure 5-5: About Screen (connected)
If the MultiTek® IC interface cable is not properly connected to the IC Analyzer, an error message
notification will appear (Figure 5-6).
Figure 5-6: IC Analyzer Not Connected

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Configuration of the IC Sampler Control Software

Click on the Configure Instrument button in the toolbar (Figure 5-7). Many of the analyzer parameters
have been hard-coded and only a few are available to change. N, S modules (installed or not) are not
available and are not displayed. All hardware components, except GFC1, GFC2, GFC4 and furnace,
have also been disabled. By default, set point of GFC1 is 130mL/min, set point of GFC2 is 450mL/min,
set point of GFC4 is 30mL/min, and set point of the furnace temperature is 1050oC.
Figure 5-7: IC Sampler Control Software
If modification is necessary, follow the instructions for the O/S running (Win XP, Vista, Win7):
For Win XP and Vista go to C:\Program Files\PAC L.P\IcSamplerControl, or (for Win7). Open the file
HalideMethods.xml.
For Win7 apply the following options: Show hidden files and folders is selected, Hide extensions for
known file types is unselected, and Hide protected operating system files is unselected. Be sure to use
Notepad for editing – Explorer cannot be used to edit the file. Go to C:\ProgramData\IcSamplerControl.
Open the file HalideMethods.xml.
At the top of the file look for <HalideConfigure>. Below in the string, bMFC1Type, true is for carrier
gas Argon, false is for carrier gas Helium; lMFC1Tolerance, lMFC2Tolerance, lMFC4Tolerance will
set the tolerance for these gas flow controller in percentage. After modifications are complete, save and
exit the file, launch the MultiTek® IC Sampler Control software, claim the instrument, and click the
Configure Instrument button. The new parameter(s) will be applied to instrument.
<?xml version="1.0" encoding="utf-8"?>

<BufferOfHalideMethods xmlns:xsi="http://www.w3.org/2001/XMLSchema-instance"
xmlns:xsd="http://www.w3.org/2001/XMLSchema">
<sCurrentVersion>1</sCurrentVersion>
<oHalideConfigure>
<bMFC1Type>true</bMFC1Type>
<lMFC1Tolerance>10</lMFC1Tolerance>
</oHalideConfigure>

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Diagnostics
All of the components in the IC subsystem can be tested using the Diagnostics screen. To access the
Diagnostics screen (Figure 5-9) click on the Diagnostics icon (arrow in Figure 5-8).
If a peripheral is not connected the control section will be grayed out.
Change size and location of screen

MultiTek® IC Sampler Control software supports sample analysis by the IC analyzer software, so either
Chromeleon or MagIC should occupy the main part of the PC’s display screen. The MultiTek® IC
Sampler Control screen is placed in the middle of the PC display, on top of all other application software
screens. During operation, the MultiTek® software runs in the background but can still provide the user
with information on sampler control status. The button to shrink the MultiTek® IC window and move its
location to the upper right corner of the display is in the upper right of the screen (arrow in Figure 5-10).
This gives additional space for the IC Sampler Control software. The example below shows the
MultiTek® screen on top of the main MagIC screen (Figure 5-11).

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Figure 5-10: Change Screen Size and Location
By clicking the button again (Figure 5-11), the MultiTek® screen goes back to its original size and
location.
Figure 5-11: IC Sampler Control Software and MultiTek IC Sampler Control Software
Running a Sequence
The MultiTek® IC Sampler Control software differs from the MultiTek® software because there are no
methods, samples, or calibration activities available to the user. Because the function of the MultiTek®
IC Sampler Control software is to prepare a sample and then transfer the sample to the IC Analyzer for
analysis, the MultiTek® IC Sampler Control software support sequences, ranging from one to several
samples. The user must configure all of the sample preparation parameters before running a sequence.
The tabs in the main software window are where the user may access and configure any attached
peripherals as well as set up the sequence table.
The Hardware settings tab provides for setting Furnace temperature and flow rates for Gas Flow
Controllers GFC1 – GFC4. System pressure is also displayed (Figure 5-12).
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Figure 5-12: Main Screen – Hardware Settings
The Timed events tab is used to set up sample burn time and control the timing of activities by the
peripherals (Figure 5-13). Peripherals not available are grayed out. “Sample burn time” is the time
between starting and stopping of DI water to the pyrotube. During this time window, the sample boat
containing the sample will be inserted into the furnace. All of the time stamps in the “Timed events”
table are in absolute time relative to the start of the sample burn time. Do not set any peripheral time
event to greater than or equal to the “Sample burn time”, as this will cause an error in the sample
processing.
Figure 5-13: Main Screen – Timed Events

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When connected, the Liquid autosampler tab will be active (Figure 5-14). If no autosampler is
connected, the user will have to manually load the sample in the sample boat (via 740/735).
Figure 5-14: Main Screen – Liquid Autosampler
The user will set up all the autosampler activities including; syringe washes and flushes before loading
the sample boat, the volume to load into the sample boat, and syringe washes after loading the boat. A
utility is provided to estimate the time required to complete all activities up to the sample being loaded
in the boat. This is to help avoid the “Timed events” table from starting the sample boat moving into the
furnace before the sample has been loaded. If the Autosampler cycle time is greater than the Sample
burn time, an error screen will be displayed (Figure 5-15).
CAUTION
When using the 748 or 758 Liquid Autosampler to load the sample into the boat it is very
important to set enough delay in the 735 table to allow the autosampler to complete
injecting the sample into the sample 740 Multimatrix before the 735 begins to move the boat
into the furnace.
All values in parentheses are input value multipliers used by the software. For example, the multiplier
for the Clean cycle fill volume is 1.0µl. With a parameter input value of 25, the autosampler will fill the
syringe with 25µl. The multiplier for the Pull-up delay time is 0.1s. When multiplied by the input value
of 20 the result is this action has been set to occur at 2s.
Important
Total time until injection done is the minimum time to start moving the sample boat into the furnace.
Autosampler run cycle time is the minimum time for sample burn time.

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Figure 5-15: IC Sampler Control Software Screen – Cycle Time Error
The Sequence tab is for setting up the sequence table, which contains information on the location of the
sample vials, and the number of injections per vial.
Figure 5-16: Sequence Table

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A separate line for each vial must be configured. Additional lines may be added using the Add button.
Lines no longer needed are removed with the Delete button. Lines may be inserted into an existing table
using the Insert button.
Usually the sequence takes full control of all operations including the start of each sample preparation.
If there is a need to perform manual operations with samples, such as loading a solid sample into the
boat before a run, check the “Push button” box. This will pause the sequence and await the user to press
the Start button on the front of the MultiTek® after the preparation of the sample.
Any changes to any parameters in the 4 tabs will require the method to be saved before running the
sequence. Click on the Save button, and a new version of Method will be generated using the current
parameter settings. The HalideMethods.xml file mentioned before will be updated by appending the
new version to the file.
<m_oHalideMethods>
<m_sMethodName>24</m_sMethodName>
<m_oHalideMethod>
<AutoSampler>
<lPreSolvClnCyc>2</lPreSolvClnCyc>
<lClnCycFillVol>20</lClnCycFillVol>
<lSamClnCyc>2</lSamClnCyc>
<lPull-upDly>20</lPull-upDly>
<lPull-upSpd>20</lPull-upSpd>
<lPull-upCnt>2</lPull-upCnt>
<lSamFillVol>20</lSamFillVol>
<lAirFillVol>2</lAirFillVol>
<lInjDly>10</lInjDly>
<lInjSpd>30</lInjSpd>
<lPullOutDly>10</lPullOutDly>
<lPostSolvClnCyc>2</lPostSolvClnCyc>
</AutoSampler>
<Sequence>
<sSequence>1;1;1;</sSequence>
</Sequence>
<HardwareSetPoint>
<fMFC1SetPoint>130</fMFC1SetPoint>
<lPyroTempSetPoint>1050</lPyroTempSetPoint>
<fWaterToPyroTube>0</fWaterToPyroTube>
<fSolutionToScruber>0</fSolutionToScruber>
<lPumpTimeToIc>0</lPumpTimeToIc>
</HardwareSetPoint>
<TimedEvents>
<lSampleBurnTime>0</lSampleBurnTime>
<lAutoSampler>0</lAutoSampler>
<lSyringeDriveForward1TurboOn>0</lSyringeDriveForward1TurboOn>
<lSyringeDriveHold1>0</lSyringeDriveHold1>
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<lSyringeDriveForward2>0</lSyringeDriveForward2>
<lSyringeDriveForward3>0</lSyringeDriveForward3>
<lSyringeDriveReverse>0</lSyringeDriveReverse>
<lGasSamplerInject>0</lGasSamplerInject>
<lGasSamplerLoad>0</lGasSamplerLoad>
<lGasSamplerBypassOn>0</lGasSamplerBypassOn>
<lGasSamplerBypassOff>0</lGasSamplerBypassOff>
</TimedEvents>
</m_oHalideMethod>
</m_oHalideMethods>
There is a drop down combo box which will display all saved method version numbers. The last entry is
the most recently saved method. Make sure to select this version before running the sequence.
Starting the Sequence

Click the Run Sample button to start the sequence. The method information will be transferred to the
MultiTek® and any peripheral. The state of instrument will be changed from “Idle” to “PreRun”. After a
few seconds it will change again to “Ready” if there were no errors detected. If the autosampler in the
“Timed events” tab is enabled, the instrument will automatically move from “Ready” to a “Run” state
and continue running the sequence unless the “Push button” box on the sequence tab was checked. The
user must press the Start button on the front of the MultiTek® at this time to continue operations. The
state LED will blink in orange to remind the user to push the start button.

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As long as the sequence is running, the MultiTek® software will control all functions except for pressing
the Start button. The samples in the sequence will be processed until the sequence is completed. At that
time, the analyzer state will change to “Idle”. If necessary, the sequence can be aborted by clicking the
Abort button (Shown by arrow, Figure 5-18).
Figure 5-18: Abort
If an alarm is triggered during operations, the sequence will be automatically aborted. The software will
perform a cleanup on the IC subsystem before entering an idle state. This operation may take several
minutes to complete. During this clean up the user cannot start any new sequence.
Figure 5-19: Abort In Progress
Flow of Operation
User can create a sequence with multiple samples and multiple injections for each sample. The
following is a brief operation flow for running a sequence.
One time pre-clean (done once at the start of every sequence):

• Pump DI water to container for ~5 minutes for pre-clean
• Pump out cleaning solution from container for ~2.5 minutes

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Steps performed for each injection:

• Pump scrubber solution to container for ~2 minutes
• Pump DI water to pyrotube for sample burn time
• During sample burn time, all events will start to happen in the order of time
• At end of sample burn time wait until IC analyzer is ready, pump the solution from container
to IC analyzer for 20 seconds
• Signal to IC analyzer to change from Load position to Inject position
• Pump out the rest of solution from container (time depends on sample burn time)
• Pump DI water to container for post clean (time depends on sample burn time)
• Pump out cleaning solution from container (time depends on sample burn time)
View Alarms
The alarm trigger in the IC Sampler Control software continuously checks actual parameter values
against setpoint values for all instrument hardware. The alarm trigger point is set in Tolerance field in
the HalideMethods.xml file. If no alarm condition is detected, the Alarm status will be green and display
None. If an alarm is triggered, the status changes to yellow and displays Warning or red and Error. By
clicking the Alarm button on the main toolbar, all alarms detected will be displayed. To clear the
alarms displayed, click the Acknowledge all button. Each alarm has an internal code assigned to it, and
a text message to describe the error.
Figure 5-20: Active Alarms

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Setting up the Dionex ICS2100 with the MultiTek® IC Software
Chromeleon Server Configuration

The user should become familiar with the Chromeleon software in order to set up the IC analytical
method, run the method, collect the chromatographic data from standards and samples, set up
calibrations and data analysis, as well as prepare final reports. These operations are outside the scope of
this manual. Basic information on installing the Chromeleon software and configuring the software to
communicate with the MultiTek® software is provided below.
Install the Chromeleon software from the installation CD. Install the Chromeleon dongle and software
license to activate the software. Run the Server Configuration utility to create and configure the IC
timebase, and perform the following operations:
Add “Remote Inject” to the time base. Right click on the time base of the ICS2000/ICS2100, then click
Add device. A window will appear displaying the available devices that can be added. Click on
Generic, then select “Remote Inject”, and then click the OK button.
Figure 5-21: Server Configuration
Select “Remote Start” from the “Inject Port” dropdown list and then click OK. The Server
configuration screen should be updated to show the Remote Inject has been added.

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Figure 5-22: Remote Inject
Next, right click the timebase and click properties from the list. The Dionex ICS-2000 IC System
window will then load. Click the TTL Inputs tab and change the “TTL Input Mode” to “Inverted
edge”. Configure the “TTL Input Functions” of each channel as in shown below.
Figure 5-23: Inverted Edge
Go to the “General” tab and configure the IC pump by clicking on the pump serial number drop down
box. The serial number of the attached pump will be automatically updated to the dropdown list. Click
on the number to update the timebase.

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Figure 5-24: Dionex System
Go to the “Eluent Generator” tab and click on the serial number drop down box. There will not be an
automatic update for the eluent generator serial number. Manually enter the number which is found on
the body of the KOH bottle. Click OK to accept the serial number.
Figure 5-25: Eluent Generator
After the system loads the serial number, Chromeleon will load the eluent generator into the timebase
and will automatically reset operating parameters for the eluent generator. Accept all four changes by
clicking OK as prompted.

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Click the save icon and save the “timebase configuration”. If no warnings or errors are found by
Chromeleon, close the utility.
Launch the Chromeleon software by clicking on the desktop shortcut. The timebase name should be
displayed. Open the Dionex templates folder and find the ICS-2000_System.pan file. Copy this file
into the MultiTekIC/1_Instrument_Panels folder.
Figure 5-26: Launch Chromeleon Software
Figure 5-27: Software Location
Rename the ICS-2100_System.pan file as MultiTek IC.pan. After renaming the file, double click the
file to launch the instrument panel view.
The instrument panel will show all of the attached system components added to the system during the
configuration of the time base. When first loaded, the system panel will not update any information to

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the screen because the time base has not connected to the analyzer. Click the Control menu and then
click Connect to timebase.
Figure 5-28: Connect to Timebase
After Chromeleon has connected the MultiTekIC timebase to the IC, the instrument panel will be
updated in real time with information from the various system components. The check box “Connected”
will show that the IC is now under computer control. Many of the IC front panel controls will now be
locked out. To restore IC front panel controls, unclick the “Connected” box.

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Figure 5-29: Connection Screen
Loading the Chromeleon method

The Chromeleon method file developed for use with the MultiTek® contains system calls and device
codes to process signals between the IC and the MultiTek® as well as the analytical method to separate
and identify fluoride, chloride, and bromide ions. The default MultiTek® method is found on the
MultiTek® installation disk.
Any new IC method must contain these lines to insure proper operation of the two instruments. An
example IC method is shown below.
Data_Collection_Rate = 5.0 [Hz]

CellTemperature.Nominal = 35.0 [°C]
ColumnTemperature.Nominal = 30.0 [°C]
Suppressor_Type = ASRS_4mm
Suppressor_Current = 99 [mA]
Pressure.LowerLimit = 200 [psi]
Pressure.UpperLimit = 2050 [psi]
%A.Equate = "%A"
CR_TC = On
; Pump_ECD.Hydroxide = 40
; Pump_ECD.Recommended Current = 99
; Pump_ECD.Carbonate = 0.0
; Pump_ECD.Bicarbonate = 0.0
; Pump_ECD.Tetraborate = 0.0
; Pump_ECD.Other eluent = 0.0

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Flow = 1.00 [mL/min]
-1.000 Concentration = 15.00 [mM]
-0.500 Pump_InjectValve.LoadPosition ;Set valve to Load position

Pump_ECD_TTL_2.0v ;inform MultiTek ICS is ready
0.000 Inject ;Wait until the inject signal sent by

MultiTek, then switch valve to Inject position and start analyze
Autozero
ECD_1.AcqOn
Pump_ECD_TTL_2.5v ;inform MultiTek ICS is busy
3.000 Concentration = 15.00 [mM]

ECD_1.AcqOff
Pump_InjectValve.LoadPosition ;set valve to Load again

End
NOTE
If the Remote Inject was not added to the timebase these system calls will not be functional.
Loading the Chromeleon IC sequence

During sample preparation and sample analysis, the IC and the MultiTek® perform different operations.
This requires communications between the two instruments to avoid errors in timing. When running
samples using a sequence, two sequence tables need to be set up, one by the MultiTek® and one by the
IC Sampler Control software. The Chromeleon information must match samples prepared by the
MultiTek®.

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Figure 5-30: Loading the Table
Setting up the Metrohm 881 Compact IC Pro with the MultiTek® IC

Software
The user should become familiar with the MagIC.net software in order to set up the IC analytical
method, run the method and collect the chromatographic data from standards and samples, set up IC
calibrations and data analysis, and as well as prepare final reports. These operations are outside the
scope of these work instructions. Basic information on installing the MagIC.net software and
configuring the software to communicate with the MultiTek® software is provided below.
Install the MagIC.net software from the installation CD. Launch the software. Do not turn on the IC
pump. Go to the “Manual” screen by clicking the Manual tab.
The user settable parameters for all of the components in the “Manual” view can be accessed by either
clicking the component image or the components tab. The “manual configuration” screen shows the
remote communications box, which is the connection point to the MultiTek®. Click the image of the
box to open the configuration screen.

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Figure 5-31: View Parameters
The Metrohm IC communicates with the MultiTek® using a customized 25 pin cable. The configuration
tab allows the user to set the High (1) and Low (0) status of the output lines and to read the state of the
input lines. Each of these lines may be either set or read by the MagIC Net software during an analytical
run.
Figure 5-32: Communications Screen

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To test the communications between the MultiTek® and the 881 Compact IC Pro begin by reducing the
window size of the “Remote” box by 50%. Launch the “Diagnostics” window in the MultiTek®
software. Position the windows as shown such that the MultiTek® and MagIC Net information can be
viewed simultaneously.
“IC connect” should show a green status light indicating that the MultiTek® to Remote box cable is
properly plugged into the MultiTek®. The “IC ready” should show a red status light. Remove the
MultiTek® to Remote box cable from the back of the MultiTek®. The IC “connect” status should
change to red and a warning text box should appear. After confirming the operation, replace the cable.
Figure 5-34: IC Connection Screen

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Move the window slider on the Remote box window to the right. Set the 3rd bit from the right of the
Remote box output to 1 and click Apply. The “IC ready” status should show a green status.
Set the 3rd bit from the right of the Remote box to 0 and click Apply. The “IC status” should show red.
Move the Remote box slider back to the left to display the “Input signals”. Click the MultiTek® IC
inject button on the MultiTek® “Diagnostics” window. The first bit to the right of the Remote box Input
signal should be a 1. Click on the MultiTek® IC load box and the first bit to the right of the Remote box
input signal should change to a 0.
Close the “Diagnostics” screen on the MultiTek® IC software and close the Remote box window.

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Method Editor Screen

Click the MagIC Net Method button to open the method screen. This screen allows the creation and
modification of an analytical method. This screen only displays a loaded method. If no method has been
loaded, then the screen will be empty.
A method for use with the MultiTek® has been provided on the MultiTek® Installation CD. This method
will need to be imported into the MagIC Net database.
Once the method has been imported, the method can be loaded by clicking the “Open Method” icon on
the tool bar and selecting the method from the list. After the method is loaded, it must be configured to
match the Metrohm IC system connected to the MultiTek®.
Several views in the MagIC Net software are composed of multiple smaller windows. Each window can
be expanded to full screen view by clicking the small white square in the upper corner of the window.
Clicking the square again reduces the window to its original size.
Figure 5-37: MagIC Net Software Screens
Once the method is loaded, all relevent method information is displayed using 4 separate windows.

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Sequence Table Configuration

Click the Workplace button then double click to expand the Run window. Click the edit button and
select “load sequence”.
The sequence table editor is available in the lower left corner of the Workplace window. The structure
of the MagIC Net sequence table is similar to the sequence table of the MultiTek® IC software. Each
line represents a single sample with options to name the sample, add comments and multiplicative
factors, and to run the sample once or several times. All the relevant sample information is stored in this
table. The information in the column labeled “Position” is not used during a sequence because the
MultiTek® has this information in its sequence table. For convenience or reference, the MagIC Net
position column can be loaded with the sample vial number on the sample tray. Care must be taken to
exactly match the two sequence tables so the information stored in the MagIC Net data base is correct
for the sample or standard analyzed.
Analysis of Halides on the MultiTek® IC

NOTE
The system is set up, tuned and performance tested before being shipped. A service engineer will set up the
analyzer in the lab and demonstrate proper operation for sign off. Training classes are available at PAC sites to
instruct users in routine maintenance and operation of the equipment.
A working knowledge of operating the IC and its software is required in order to analyze samples.
Results are viewed in the software controlling the IC. Please refer to the documentation provided with

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the IC for details on operation and maintenance. These documents will also have specifics on using
blank correction and regression techniques supported to calibrate the instrument.
The following steps are required before quantitatively analyzing samples:
1. Set up instrument and method.
2. Determine retention times of target compounds, set up identification and integration parameters
in the method.
3. Ensure the system is clean enough to determine the desired concentration levels of components.
4. Calibrate the method for each target compound.
A validation sample should be analyzed periodically to ensure the calibration is still valid. When the
validation sample exceeds the tolerance level, the system should be reviewed for the cause of the
response to change. If the system is believed to be in proper working conditions, it can be recalibrated.
NOTE
PAC provides standards for calibration and performance testing. See the Spares and Consumables overview or
contact PAC for information.
General Guidelines for Sample Analysis

Methods for the IC are provided with the IC Sampler Control software.
The maximum recommended sample size is 100µl for aqueous samples and 40μl for organic samples.
This sample size can be changed by modifying the methods included with the MultiTek® software.
NOTE
Approach the maximum sample size with caution to avoid coking the instrument. Most organic solvent samples
will require a multiple step advancement of the sample boat.
Identification and Integration of Target Compounds

Analyze a standard sample to determine the retention times of the target compounds and set up
identification and integration. Figure 5-39 and Figure 5-40 below show examples on the Metrohm and
Dionex system.

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Figure 5-39: Metrohm IC chromatogram with target compounds at 10 ppm
Figure 5-40: Dionex IC chromatogram with target compounds at 10 ppm
The integration of Bromide needs consideration on the Dionex IC system. On the standard configuration
Bromide elutes the tail of the Carbonate peak; and proper integration settings need to be found to
accurately determine the peak area. Dionex sells a carbonate suppression module to reduce the size of
the carbonate peak and improve bromide results. Contact Dionex for further information on availability
and price.

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Blank Analysis
Analyze a blank sample to verify no components co-elute with the target compounds.
An example of a blank IC chromatogram is shown below in Figure 5-41. Ensure the identification
windows are chosen such that other compounds will not be identified as one of the target compounds if
the target compound is not identified.
Figure 5-41: Blank IC Analysis On Dionex
It is important to ensure a blank run is sufficiently clean in the area of the target compounds. A number
of typical peaks are present besides the target compounds Fluoride, Chloride and Bromide. Those
compounds mostly originate either from impurities of the deionized water, the combustion process, or
from the sample itself. The majority does not interfere with the target compounds and can safely be
ignored.
Fluoride: One component has been found eluting together with Fluoride. This has an effect on the LOD.
The Troubleshooting section contains possible causes and remedies to minimize the interference. Use of
high purity 18Mohm water and correct cleaning procedures for the condenser and scrubber jar glassware
are two important items necessary for achieving low level fluoride results.
Chloride: Higher than anticipated Chloride levels can originate from the scrubber or the water used for
the analyzer.
Bromide: On the Dionex IC, bromide elutes on the tail of the Carbonate peak. Ensure integration
settings result in a correct integration of the peak on the slope.
General: Analysis of samples containing high concentrations of halides (100ppm or more) contaminates
the system. It takes several blank runs to clean the system to the level whereas sub ppm samples can be
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analyzed again. Diluting these samples or using a smaller injection volume for those samples can
minimize these effects.
Calibration
Use several concentration levels including a blank level to determine the response curves. The method
of calibration on the IC depends on the concentration range of interest. Larger concentration ranges may
require higher order calibration curves to accurately represent the response of the system. The IC
software supports these calibrations.
The methods provided are set up to use ISTD calculation. Adjust the concentration of the phosphate to
give a peak with an area corresponding to the middle of the concentration curve.
System and Sample Treatment

Water Quality and Use
Minimum water quality is 16Mohm or better. Recommended is 18Mohm resistively water (Type1) rated
for use with IC analysis. The major contamination in de-ionized water processors is trace chloride.
Proper maintenance of a laboratory water processing system is essential to maintain the quality of the
water. Refer to the equipment manufacturer’s user manual for recommended maintenance.
Bacteria will grow in 18Mohm water given enough time and fluorescent lighting. Water should be
protected by using a bio check such as methanol or hydrogen peroxide. Use of brown glass reduces the
availability of UV light. Water/scrubber solutions should not be stored or used for more than one week.
Pyrotube water can be stabilized with 0.1% methanol as a bio check.
Columns (general)
Over time the IC columns loose separation efficiency and loss of resolution between peaks occurs.
Overpressure can damage the columns and result in quick loss of separation efficiency. Refer to the
column manufacturer’s instructions on column care, storage conditions, and expected lifetimes.
Dionex
A syringe filter should be used to protect the injector system from damage by the silicate particles
generated by the combustion of organic samples.
Dionex supports a carbonate eluent generator that will yield a better bromine detection levels. This can
be used as an alternate to the hydroxide elution in the standard MultiTek® method.
Metrohm
Prepare the carbonate eluent fresh every 2-3 days. The sulfuric acid solution does not need further
treatment (the acid inhibits bacterial growth).

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Analyzing Samples
Start and prepare analyzers and software
1. Start the IC system and load the MultiTek® IC analysis method using the IC software.
2. Launch the IC Sampler Control software and claim the MultiTek® to be used for the sample
analysis.
3. After the MultiTek® has been claimed, and the initial screen has loaded, click on the “Configure
system” icon. Wait for the software to download the operational parameters to the MultiTek®.
4. Check to ensure all required MultiTek® peripherals are acknowledged by the IC Sampler Control
software.
5. If necessary create or modify the IC Sampler Control method for the sample preparation. Check
to ensure the operational parameters and the Timed Events table has been properly set up to
control each of the required MultiTek® peripherals.
6. Initialize IC system and turn on all necessary IC system components. Allow the IC column and
other system components to stabilize for 15-30 minutes before analyzing the first sample.
7. While the IC system is stabilizing, the IC Sampler Control sequence table information should be
synchronized with the IC software sample information and sequence tables.
Prepare sequence
NOTE
The IC Sampler Control software does not store sample specific information. The only information
required by the IC Sampler control software is the number of samples in the sequence, the number
of injections required for each sample, and whether or not the user or the software will start each
sample analysis.
8. If necessary modify or create a new sample table with the IC software and input all relevant
calibration standard and sample information. Ensure the total number of samples and the number
of analyses per sample has been entered into the IC Sampler Control sequence table.
9. Load the samples into the autosampler tray (if present) or prepare the first sample for manual
loading.
Run the sequence

10. Analysis of the first sample may be started when the IC system has reached a stable operational
status and the IC software sequence table information has been synchronized with the IC
Sampler Control sequence table.
11. Initiate the start of the IC sequence table using the IC control software. The IC will set the
injection valve to the LOAD position and send an ‘IC System READY’ signal to the MultiTek®.
The IC system will then enter a “WAIT” loop while the MultiTek® prepares the sample for
analysis.
12. Initiate the start of the IC Sampler Control by clicking on the “Send to instrument button”. After
a few seconds, the “Run state monitor” box will be updated with the operations currently being
conducted by the MultiTek®.

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Liquid samples using autosampler or automatic gas sample box

Samples will be automatically injected and analyzed on the system. Use of the “Push Button” check box
in the sequence table is not needed.
Liquid or solid samples, manual injection

Ensure to check the “Push button” option in the IC Sampler Control sequence table. The MultiTek® will
wait for the user to manually load the sample into the sample boat and then press the START button on
the front of the MultiTek®.
Important Factors for Halides in Certain Sample Types
As an aid to the analyst, this has been assembled for the Antek MultiTek® IC Configuration. Use these
guidelines in accordance with your particular instrument configuration and sample matrix.
Halides in Liquid Hydrocarbons (Direct Injection)
1. The analysis of halides in liquid hydrocarbon solvents using direct injection can be done, but is
not recommended due to higher RSDs. The boat inlet described below is the recommended
sample introduction for halides in liquid hydrocarbon solvents.
Halides in Hydrocarbons (Boat-Inlet)

1. Furnace Temperature: 1050°C. The use of quartz chips in the combustion zone of the pyrotube
is recommended.
from the furnace soon after sample combustion is complete. Boat in furnace residence times can
vary depending on sample volatility and levels measured. Typical boat in furnace residence times
4. Injection Size: As a general rule larger sample sizes are required for measurement of lower
combustion (coking or sooting) that may be present in the sample path. Control sooting by
5 ppm to 100 ppm 10 – 20 µL

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(approximately 10 µL/second) being careful to discharge the last drop. Use of Cerafelt in the
boat loading area. Typical injection frequency allows at least 5 minutes between injections.
halides may be vaporized as the boat approaches the furnace. Sub-ambient temperature can
reduce this evaporation.
Typical Gas Flows

Inlet Oxygen Flowmeter Settings 10 – 40 mL/min
9. Pyrotube Water Introduction Rate: Water vapor is required during the combustion of the
sample to generate the acid halides. The recommended water introduction rate using the pyrotube
water peristaltic pump is 0.7-0.9 mL/minute.
saturation point of the detector.
the inside areas of the pyrotube near the injection area. Heat the boat and Cerafelt in the furnace
to assure that boat and Cerafelt are clean, and then rapidly move boat out to injection area.
solvents that have minimum or no contamination relative to the concentration of anticipated in
the sample unknown. Correct for halide contribution from solvent materials and impurity of
source material. Use calibration curves that bracket the expected levels in the sample unknown
as a guide to prepare standards. Do not force the calibration curve through the 0,0 axis. Construct
standard concentrations that will yield a calibration curve that is a best linear (0-10ppm) or
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second order (0-100ppm). The curve should yield an estimated value that can be used to
calculate halides content in the sample on a mass/mass basis.
Halides in Aqueous Samples (Direct Injection)

1. The analysis of halides in aqueous solvents using direct injection can be done, but is not
recommended due to high RSDs. The boat inlet described below is the recommended sample
introduction for halides in aqueous solvents.
Halides in Aqueous Samples (Boat Inlet)

1. Furnace Temperature: 1050°C. The use of quartz chips in the combustion zone of the pyrotube
is recommended.
from the furnace soon after sample combustion is complete. Boat in furnace residence times can
vary depending on sample volatility and levels measured. Typical boat in furnace residence times
4. Injection Size: As a general rule larger sample sizes are required for measurement of lower
combustion (coking – sooting) that may be present in the sample path. Control coking by
5 ppm to 100 ppm 10 – 40 µL
(approximately 1-3 µL/second) being careful to discharge the last drop. Use of Cerafelt in the
boat loading area. Typical injection frequency allows at least 5 minutes between injections.
halides may be vaporized as the boat approaches the furnace. Sub-ambient temperature can
reduce this evaporation.

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Typical Gas Flows

9. Pyrotube Water Introduction Rate: Water vapor is required during the combustion of the
sample to generate the acid halides. The recommended water introduction rate using the pyrotube
water peristaltic pump is 0.7-0.9 mL/minute.
saturation point of the detector.
the inside areas of the pyrotube near the injection area. Heat the boat and Cerafelt in the furnace
to assure both are clean, then rapidly move boat out to injection area.
solvents that have minimum or no contamination relative to the concentration of anticipated in
the sample unknown. Correct for halide contribution from solvent materials and impurity of
source material. Use calibration curves that bracket the expected levels in the sample unknown
as a guide to prepare standards. Do not force the calibration curve through the 0,0 axis. Construct
standard concentrations that will yield a calibration curve that is a best linear (0-10ppm) or
second order (0-100ppm). The curve should yield an estimated value that can be used to
calculate halides content in the sample on a mass/mass basis.
Halides in Gaseous & Liquefied Hydrocarbons (Gas/LPG)

1. The Antek MultiTek® must be fully stabilized and in standby condition ready for analysis prior
to sample injection.
2. Sample valves should remain in the load (full counter clockwise on a Model 734 manual gas
sampling system) position except during sample analysis.

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3. Once the selected sample valve has been filled and allowed to equilibrate, sample injection
should be accomplished by applying a firm, smooth clockwise rotation to the sample valve. This
function will be performed by the software for the Model 734 automatic gas sampling system.
4. Leave the sampling valve in the inject position until analysis is complete (instrument has
returned to baseline and integration has finished).
5. The length of time required for detector response will depend upon the type of pyrotube utilized,
carrier gas flow rates, sample size, sample introduction line length and nitrogen and/or sulfur
concentration. From 60 seconds to 3 minutes can be typical.
6. Model 734 carrier gas flows can be used to manipulate sample combustion and detection
characteristics.
WARNING
Excessive carrier flow rates greater than ≥25 mL/min can cause incomplete sample
combustion (coking – sooting).
7. Sample cylinders containing liquefied gases must contain sufficient pressure (>200 PSI) to allow
the transfer of sample to the 734 without the formation of "bubbles" in the transfer tubing and
sight glass.
WARNING
Do not exceed the overall pressure rating (900 PSI) of the sample inlet system or the capacity of
the sample transfer cylinder, quick connects, and other transfer lines and fittings.
8. Use standard gas flow conditions for your Antek analyzer.
Typical Gas Flows

Inlet Oxygen Flowmeter Setting** 0 – 20 mL/min
**In some applications, inlet oxygen should be omitted.
9. The use of a filtering device prior to sample introduction is strongly recommended. This can
greatly extend valve service and prevent transfer line (tubing) plugging.
CAUTION
Particulate matter (debris) contained in samples can obstruct sampler tubing and/or cause
damage to injection valves. An inert filter device can minimize this damage.
10. The use of flowpath components with enhanced metal passivation treatments (Sulfinert™ or
Silicosteel™) can enhance the analysis of low level contaminations.

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11. The injection of liquids (iso-octane, toluene, other volatile liquids, etc.) is not advised.
12. Routinely inspect user installed transfer lines and fittings used to connect the sample container to
the sample inlet system for leaks and stress weakening that can be caused by frequent bending,
age or use.

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SECTION 6
MAINTENANCE / TROUBLESHOOTING
Introduction
This section provides information for troubleshooting and maintenance of the Antek MultiTek® system.
For more detailed maintenance and troubleshooting information, please contact a PAC service
representative.
Routine Maintenance
The Antek MultiTek® System is a relatively maintenance free analyzer. Regular care of a few items
should keep the system operating at peak level. The following is a recommended routine maintenance
schedule:
Daily
1. Check cylinder supply pressure for all supply gases.
2. Check all gas flows.
3. Check all analytical parameters including temperatures, detector settings, timed events, etc.
4. Check the validity (within normal analytical error) of any calibration curve(s) being used by analyzing
check standards and comparing them to the existing curve and previous check standard data.
Monthly
1. If the system is equipped with a MoleculiteTM/DrieriteTM scrubber, empty and recharge the
MoleculiteTM/DrieriteTM scrubber with fresh material. Refill kits (P/N 71028 and 72001) are available
from PAC. A properly charged scrubber should contain approximately 50% MoleculiteTM and 50%
DrieriteTM.
NOTE
If the indicating DrieriteTM should turn pink before the one-month period is complete, this is an indication that
the scrubber is wet and the Drierite should be recharged or replaced.
NOTE
If the indicating Drierite should turn black, this is an indication of ozone getting through the catalyst and both
the DrieriteTM and MoleculiteTM should be replaced. The Ozone Generator should also be checked for leaks.
With proper maintenance and use of quality gases, MoleculiteTM can typically last up to 2 years without
needing replacement. DrieriteTM can be regenerated in a low temperature oven which will drive off the
absorbed moisture as indicated by a pink color and turn the material back to a blue color.

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Preventive Maintenance
1. Septa are to be replaced on an as needed basis. Generally, a septum is good for more than 100
injections. When the septum becomes soft or brittle and no longer presents resistance to the syringe
needle upon insertion, it should be replaced.
2. Teflon® ferrules have a tendency to “cold flow” and may need to be tightened or replaced
periodically.
3. Detector Lenses may need to be cleaned periodically. Residue may accumulate on the lenses of the
reaction chamber and fluorescence chamber. Generally, this is only performed on a yearly basis, but
if response decreases steadily or the system exhibits poor repeatability, the lenses may need cleaning.
4. Clean any residue that may accumulate at the inlet or outlet of the pyrotube.
5. Replace any items in the analytical flow path which have degraded with use (i.e., pyrotube, membrane
dryer, interconnect tubing, o-rings, etc.).
6. Application review via internet. PAC service and application personnel can review instrument status
from remote locations if the instrument is accessible through the internet.
Changing the UV Lamp

WARNING
Never look into ultra-violet light from the (UV) Lamp when it is powered on.
Permanent retinal damage may occur to your eyes.
IMPORTANT
Do not touch the glass of the UV Lamp. Fingerprints and oils from your hands will become
permanently etched into the glass, reducing the lamp’s performance.
Clean the UV Lamp with alcohol solvent to remove any dirt or oils from the lamp.
Locate the “Max Output Port” stamped on the glass of the lamp to identify the maximum output port of
the UV Lamp.
Figure 6-1: UV Lamp Max Output Port Output Port

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Loosen the two set screws at the base of the UV Lamp Holder Bracket.
Figure 6-2: UV Lamp and UV Lamp Holder Bracket
Position the lamp so the maximum output port is parallel to the lamp holder bracket window.
Figure 6-3: UV Lamp Positioning
Insert the UV Lamp all the way into the UV Lamp Holder Bracket. Tighten the two set screws to secure
the lamp. Do not over-tighten the screws – damage to the lamp may occur otherwise.
Power the MultiTek® on. Make sure the UV Lamp turns on. If necessary go to Instrument Parameters to
enable the UV Lamp. Allow 30 – 45 minutes for the lamp to warm up.
Loosen the two set screws in the center of the UV Lamp Holder Bracket (Figure 6-5) that keep the
holder in position.
IMPORTANT
Take extra care to make sure the holder does not come off the slide mount
attached to the collimating lens housing.
WARNING
Never look into ultra-violet light from the (UV) Lamp when it is powered on.
Permanent retinal damage may occur to your eyes.
Slide the lamp holder up and down to maximize the Sulfur baseline (Figure 6-4) on the Main screen
(Figure 3-6).
After changing the UV lamp go to the “Service Counter” screen in “Setup” and click Change Lamp.

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Figure 6-4: Adjusting UV Lamp
Figure 6-5: UV Lamp Mounted in MultiTek®
Lamp to Lens Holder Bracket UV Lamp Holder Bracket
Holder Set Screw (1 of 2) Lamp Set Screw (1 of 2)
Note: There are two Set Screws, one on each side of the Lamp to Lens Holder Bracket.

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Backing up the Database

Open Microsoft SQL server management studio, connect to the server where the database is stored.
Figure 6-6: Connect to Server

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Highlight “PAC MultiTek” under the Database folder, right click mouse, click Tasks -> Back Up…
Figure 6-7: Microsoft SQL Server Management Studio
Select “Backup type Full”, then click the Add button

Figure 6-8: Back Up Database

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Select the backup destination, and then type the name for the backup. Click OK.
Figure 6-9: Back Up Destination

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Click OK. The database will be successfully backed-up.
Figure 6-10: Back Up Database

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Restoring the Database

Open Microsoft SQL server management studio, connect to the server where the database is to be stored.
Figure 6-11: Connect to Server
Highlight “PAC MultiTek” under “Database folder”, right the click mouse, and click Tasks -> Restore -
> Database.
Figure 6-12: Microsoft SQL Server Management Studio

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Select “From device”, then click browse button.
Figure 6-13: Restore Database

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Click Add, and then browse to the folder where the backup database is saved. Double click the backup
database then click OK.
Figure 6-14: Specify Backup

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Go to “Database Restore Options” and check “Overwrite the existing database”.
Ensure to check the “Restore” checkbox, and then click OK. The database will be fully restored.

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Troubleshooting and Service Guide

This section is a guide for isolating and correcting problems that may arise while operating the Antek
MultiTek® system. These problems may be grouped into three categories: (1) analytical troubleshooting.
(2) IC module troubleshooting and (3) electrical, electronic, and mechanical troubleshooting. These
three situations will be discussed separately below.
To use this guide, simply locate the symptom in the left column and follow suggestions for probable
cause and remedy. Some symptoms may be addressed in each section. For detailed drawings of
component location, electronic schematics, flow diagrams, parts lists, and servicing guidelines, please
contact a PAC service representative.
Analytical Troubleshooting
Before attempting to perform any troubleshooting and before taking any action to remedy an apparent
problem, ensure all components of the analytical system and any accessories are properly assembled.
Solutions that are denoted with an * (asterisk) should only be performed by an advanced user or a
qualified Technician. If further assistance is needed, please feel free to contact PAC Service at 1-800-
444-TEST (8378).
Nitrogen / Sulfur Module Troubleshooting

SYMPTOMS PROBABLE CAUSE SOLUTION
Baseline too high or at PMT voltage too high Adjust voltage

maximum voltage
Contaminated gas supply Change gas supply
Contaminated septum Replace septum
Contaminated pyrotube, *Clean pyrotube, tubing,
transfer tubing, or or transfer reaction
reaction chamber chamber
Light leak, detector Repair light leak,
detector
Baseline too low or at Restricted flow Check for flow

zero value restrictions
UV lamp off, low Repair UV lamp/supply
intensity
No ozone *Restore ozone flow
Faulty PMT or module *Replace PMT and/or
board module board
Gas leak Repair gas leak

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Baseline drift Contaminated gas supply Change gas supply

Contaminated pyrotube, *Clean pyrotube, tubing,
transfer tubing, or or reaction chamber
reaction chamber
PMT cooler not stable *Repair cooler
UV lamp not stable Repair UV lamp/supply
Baseline shift-before Change in inlet gas flow *Check for leak during
peak obstruction or sample introduction
inlet
Sample size too large Reduce sample size
Septum leak Replace septum
Baseline shift-during Change in inlet gas flow *Check for obstruction

analysis or leak in sample inlet during sample
introduction
Baseline shift- after Change in inlet gas flow *Check for obstruction
analysis in sample inlet or leak during sample
introduction

Incomplete combustion Ensure that sample
of the sample flows, temperature,
injection rate, and gas
flows are correct
Baseline noise- high Unstable power source Stabilize power

frequency
Unstable power supply *Replace power supply
Faulty signal/power Replace signal/power
cable cable
Dirty printed circuit *Clean printed circuit
board contacts board contacts
Faulty PMT *Replace PMT

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Faulty PMT board *Replace PMT board

Faulty N-S module board *Replace N-S module
board
Baseline noise- low Unstable power source Stabilize power

frequency
Unstable gas regulator Replace regulator
Light leak Repair light leak
Baseline noise- cycling Unstable power source Stabilize power

Faulty PMT cooler * Replace PMT cooler
Abnormal ambient Stabilize ambient
temperature changes temperature
Baseline noise- spikes Unstable power source Stabilize power

Faulty signal/power *Replace signal/power
cable cable
Faulty PMT/N-S module *Replace PMT/N-S
boards module boards
Faulty gas regulator Replace regulator
Faulty ozone generator *Repair generator
No response Gas leak Repair gas leak

No ozone (nitrogen) *Check ozone generator
No UV source (sulfur) *Check UV source
No sample introduction *Check sample injector
Defective pyrotube Check pyrotube
No PMT voltage *Check PMT voltage
Loose cable Secure all cables
board
Integrate time too short Lengthen integration
time
Integration start/stop Correct start/stop times
time not correct
Negative response Gas leak Repair gas leak

Change in inlet gas flow Check for obstruction in
sample inlet
Unusually large Contaminated gas supply Change gas supply

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response
Contaminated pyrotube *Clean or replace tube
Tailing response Gas leak Repair gas leak

Change in inlet gas flow Check for obstruction
in sample inlet during sample
introduction
Incomplete combustion *Ensure that furnace
of sample in furnace temperature is correct
and needle or sample
boat remains in furnace
long enough
Poor sample introduction *Check injection/boat
insertion profile
Split response Gas Leak Repair gas leak

Change in inlet gas flow *Check for obstruction
during sample in sample inlet
introduction
Incomplete combustion Ensure that sample
of sample in furnace furnace temperature is
correct
Poor sample introduction Check injection/boat
insertion profile
Low response Gas leak Repair gas leak

Change in inlet gas flow *Check for obstruction
obstruction in sample during sample
inlet introduction
Incomplete combustion *Ensure that sample
of sample furnace temperature is
correct
Poor sample introduction *Check injection/boat
insertion profile
Faulty membrane dryer *Replace membrane
dryer
Change in response Gas leak *Repair gas leak

Unstable power source Stabilize power
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Poor sample introduction Check injection
No sample introduction Check sample injector
Incomplete combustion Ensure that furnace
of sample temperature is correct
Change in ozone Check ozone generator
production (nitrogen) performance
Change in UV source *Adjust UV lamp sulfur
intensity (sulfur) and check for
contamination in
fluorescence chamber
Change in PMT voltage *Check PMT voltage
temperature change temperature
Faulty PMT cooler *Replace PMT cooler
Faulty N-S board *Replace N-S module
board
Nonlinear curve Saturation of electronicsReduce sample size or

concentration
Change in ozone *Check ozone generator
production (nitrogen) performance
Change in UV source *Replace UV lamp
intensity (sulfur) source
Flat top peaks Saturation of electronics Reduce sample size,

concentration or run
Autofit
Small linear range Saturation of electronicsReduce sample size or

concentration
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Change in ozone *Check ozone generator
production performance
Reduction in UV source *Replace UV source
lamp radiation (sulfur)
Nonrepeatable results Saturation of electronicsReduce sample size or

concentration
Flow path restrictions *Check fittings, ferrules,
pyrotube, and vents for
restrictions
Injection rate too fast Slow injection rate
Faulty membrane dryer *Replace dryer
Sample frequency too Reduce sample
fast frequency
Change in ozone *Check ozone
(nitrogen) performance production generator
lamp radiation (sulfur)
temperature temperature change
Faulty PM cooler *Replace PMT cooler
Faulty pre-amp printed *Replace pre-amp
circuit board printed circuit board
Faulty amplifier printed *Replace amplifier
circuit board printed circuit board
Improper sample size Adjust sample size
Inaccurate results Inaccurate calibration Re-calibrate the system

curve
Inaccurate calibration Construct new
standards calibration standards
Saturation of electronics Reduce sample size or
concentration
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Poor sample introduction *Check injector
Incomplete combustion Ensure the temperature is
of sample correct
(sulfur) radiation (sulfur)
temperature change temperature
Light leak, detector Repair light leak
Faulty PMT cooler *Replace PMT cooler
board
Improper injection rate Adjust injection rate
Coking Improper injection speed Slow injection speed

Low pyro oxygen or *Correct pyro oxygen or
argon flow rate argon flow rate
Incomplete combustion Ensure that the furnace
of sample temperature is correct
Gas leak Repair leak

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IC Module Troubleshooting
High blank response, Buildup in flow path: Clean flow path using
decreasing over time pyrotube, glass elbow, steam by turning on
condenser and/or pyrowater and running
scrubber jar for several hours
Clean pyrotube and glass
elbow by using torch to
burn out contamination
Clean inlet to pyrotube
and 740 glass tube
Replace sample boat and
cerafelt or glass wool in
boat
Replace glass elbow,
condenser and scrubber
jar
Replace gas solenoid
Replace pyrotube
Remove scrubber jar and
clean out any residue
then flush with high
purity water
Remove scrubber jar
bubbler and replace with
new bubbler
Sample not transferred Sample flow to IC Replace filter at IC

to IC Analyzer Analyzer blocked Analyzer inlet (if used)
Replace column(s) in IC
Analyzer
Siphon tube (from Reposition siphon tube
transfer pump) in in scrubber jar
scrubber jar not at the
bottom of the jar
Sample flow path leak Check flow path from
scrubber jar through
transfer pump to IC
Analyzer
MultiTek-IC interface Make sure correct cable
cable loose or not is firmly plugged into
connected both the MultiTek® and
IC Analyzer
Sample not in pyrotube Check sample
introduction accessories’
operation

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Sample not loaded at

input
Wrong sample selected
Flow path directed to N- Make sure IC Sampler
S modules Control Software has
been selected, is running
and the instrument
claimed
Make sure settings
written to MultiTek®
Check connector for gas
solenoid is not loose or
unplugged
Replace gas solenoid
Transfer pump did not Check transfer pump
operate function via diagnostics
screen
Check connection to
control board
Check transfer pump
jumpers: only jumper #4
should be set; all others
should be open.
Replace transfer pump
No response to tested Sample not transferred to Check fluid transfer path

sample IC Analyzer and IC Analyzer for
leaks.
Check transfer pump for
proper operation
Ensure fluid path not
blocked
IC Analyzer did not Verify IC Sample
process transferred Controller SW and IC
sample Analyzer SW are
running and configured
properly
Check IC Analyzer
vendor’s documentation
for troubleshooting guide
Autosampler or user Check autosampler
failed to load sample operation
boat at start of run Check autosampler
information in timed
events table

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Carry-over: increasing No DI water rinse in Check DI water pump

or decreasing response scrubber between sample
to same sample runs
Check DI water solenoid
Check DI water level
Lower overall response IC cooling unit failure Check power to IC

to Halides cooling unit
Check IC cooling unit is
powered on and
circulating fluid
Check cooling fluid level
Very low Fluoride No steam when sample Check DI water pump

response with lower in pyrotube – DI water
Chloride and Bromide not injected into
response pyrotube
Check DI water solenoid
Check DI water level
No reference peak Scrubber solution not Check scrubber solution

response pumped into scrubber jar pump
Check connector for
pump
Check level of scrubber
solution
Water on floor near IC waste container full Empty waste container

Instrument

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Electrical, Electronic, & Mechanical Troubleshooting

No power Power cord not plugged Plug power cord into

in proper power source
Input power relays have *Reset power relay in
opened or fuse blown power switch and/or
replace fuses
Faulty power source *Check receptacle for
proper voltage
No power – Ozone Power switch OFF Turn power switch ON

Generator
Nitrogen Module not Select Nitrogen module
active or Ozone via MultiTek®software
generator disabled and ensure ozone
generator is active
Nitrogen Module not Ensure module fully
fully seated seated
Faulty 5 VDC power Replace 5 VDC power
supply supply
Faulty ozone generator *Replace ozone
printed circuit board generator printed circuit
board
Jumpers on PCB no set Set jumpers correctly
correctly
No power – UV power Power switch OFF Turn power switch ON

supply
Sulfur Module not active Select Sulfur module via
MultiTek® software
Sulfur Module not fully Ensure module fully
seated seated
Faulty main power Restore main power
supply supply
Faulty UV power supply Replace UV power
supply
No fans running Fuse blown *Replace fuse

No power Check power source
Faulty fan(s) *Replace fan(s)
No LED’s No power Check power source

Loose ribbon cable *Secure ribbon cable
Faulty Controller Board *Replace controller
board
Faulty LED Board *Replace LED board
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No temp readout for Loose ribbon cable. Secure ribbon cable

existing zone
Loose thermocouple *Secure thermocouple
connector connector
Faulty thermocouple *Replace thermocouple
No heat – Pyro zone No power Check power source

Invalid or no set point Ensure proper value
programmed programmed
Circuit breaker open Reset circuit breaker
Faulty heater element Replace heater element
Faulty solid state relay Replace solid state relay
(SSR) (SSR)
No heat – Model 737 No power Check power source

Invalid or no set point Ensure proper value
programmed programmed
Loose control cable *Secure control cable
Circuit breaker open *Reset circuit breaker
Faulty heater element *Replace heater element
Faulty solid state relay *Replace solid state
(SSR) relay (SSR)
Overheating of temp Shorted thermocouple *Replace thermocouple

zone
Faulty solid state relay *Replace solid state
(SSR) relay (SSR)
No cooling – Faulty 12 VDC power *Replace or repair 12

thermoelectric cooler supply VDC power supply
Faulty sensor Replace sensor
Faulty thermoelectric *Replace thermoelectric
cooler cooler
No or slow cool down of Invalid or no set point Ensure proper value

Model 737 programmed programmed
Cool down doors not *Check stepper motor,
opening chain, and doors
Faulty cool down fan *Replace cool down fan

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No gas flow No supply pressure Check supply gas

Closed control valve Adjust control valve
Loose or leaking septum Replace septum
Loose gas fitting Tighten fitting
Restricted pyrotube *Clean pyrotube
Restricted gas line *Clean gas line
No ozone Power supply OFF Turn power switch ON

Power supply connector Plug power connector
not plugged in into supply line
Faulty 5 VDC power *Replace 5 VDC power
supply supply
printed circuit board generator printed circuit
board
transformer generator transformer
Faulty generator cell *Replace ozone
generator cell
O2 gas flow rate to Correct O2 gas flow rate
ozone generator too low

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APPENDIX A
STANDARDS FOR ANALYSIS
Common Conversions
Name weight/weight weight/volume volume/volume
parts per hundred 10 mg/g 10 mg/ml 10 ml/L
% 1 mg/100 mg 1 mg/100 ml 1 ml/100 ml
parts per thousand 1 mg/g 1 mg/mL 1 mL/L

ppt 1 g/L 1 g/L 1 μL/mL
parts per million 1 μg/g 1 ng/ μL 1 nL/mL

ppm 1 mg/kg 1 μg/mL 1 μL/L
parts per billion 1 ng/g 1 ng/mL 1 nL/L

ppb 1 μg/kg 1 μg/L
Exponential Form
Exponential Prefix Name Symbol
1012 tera- T-
109 giga- G-
106 mega- M-
103 kilo- k-
10-1 deci- d-
10-2 centi- c-
10-3 milli- m-
10-6 micro- μ-
10-9 nano- n-
10-12 pico- p-
10-15 femto- f-
Making Standards
Overview
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(a)(b)(c)(d) = G
(e)(f)
a: actual weight of compound (g)
b: nitrogen/sulfur content in compound (g/g)
c: ng conversion (ng/g)
d: purity of compound (g/g)
e: volume of dilution (mL)
f: μL conversion (μL/mL)
G: standard concentration (ng/μL – ppm)
Example
Pyridine (99.9% pure) contains 17.71% nitrogen. 0.5713 grams of pyridine is diluted to 100 mL with
isooctane.
a b c d
( 0.5713g )(0.1771g / 1g )(
1 x 109ng / 1g)( 0.999g / 1g ) = G = _1011_ ppm
( 100mL
e
)(1000μL / 1mL
f
)
TARGET: Convert 1000 ppm (w/v) to a weight/weight relationship
To derive a weight/weight relationship from a weight/volume concentration,
simply divide by the density of the solvent.
Materials
Nitrogen and sulfur in isooctane solvent (density = 0.6919 mg/mL)
Math
1000 ppm (W/V) = (1000μg)x( 1ml ) = 1000μg = 1445μg
1ml 0.6919g 0.6919g 1g
= 1445 ppm (W/W)
TARGET: Convert 1000 ppm (w/w) to a weight/volume relationship

To derive a weight/volume relationship from a weight/weight relationship concentration, simply
multiply by the density of the solvent.
Materials
Nitrogen and sulfur in isooctane solvent (density = 0.6919 mg/mL)
Math
1000 ppm (W/w) = (1000μg) x (0.6919g) = 691.9μg = 691.9 ppm (W/v)
1g 1mL 1mL

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Chemicals for Nitrogen and Sulfur Standard Preparation

Nitrogen & Sulfur Standards
Name Mol Wt %N %S Structure Solvents
%
Dimethylthiourea 104.18 25.89% 30.78% H2O,
Alcohol,
Acetone
Phenothiazine 199.25 7.03% 16.09% Benzene,
Ether,
slightly in
Alcohol
and mineral
oil
Thiourea 76.12 36.80% 42.12% H2O,
slightly in
Alcohol
P- 171.15 8.18% 18.73% Benzene,

Toluenesulfonamide Toluene,
Xylene
Nitrogen Standards
Name Mol Wt %N Structure Solvents
Acetonilide 135.10 10.37% Alcohol, Methanol,
Acetone,
Chloroform,
1g/185mL H2O,
1g/18mL Ether,
1g/47mL Benzene
3-Alanine 85.04 16.47% H20, slightly in

Alcohol
Carbazole 167.20 8.38% Acetone, 1g/mL

Ether
Creatinine 167.20 8.38% H20, slightly in

alcohol
N,N-Dimethyl 121.181 1.56% Alcohol,

Aniline Chloroform, Ether
Glycine 75.07 18.66% H20

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Nicotinamide 122.13 22.94% Ether
Nicotinic Acid 123.11 11.38% Propylene Glycol,

H2O, Alcohol
Urea 60.00 46.65% H20, Alcohol
Erucamide 337.59 4.15% CH3(CH2)7CH = Glycerol

CH(CH2)11CONH2 Chloroform
Pyridine 79.1 17.71% H2O, Alcohol,
Benzene, Toluene,
Xylene, Iso-octane
Fatty Oils
Acridine 179.2 7.81% Xylene, Alcohol
Sulfur Standards
Name Mol Wt %S Structure Solvents
n-Butyl Sulfide 146.29 21.92% Alcohol,
Ether, Iso-octane,
Benzene, Toluene,
Xylene
Dibenzothiophene 184.26 17.4% H20, Alcohol,

Acetone, Ether,
Benzene,
Toluene, Xylene,
Iso-octane
Dimethyl Sulfoxide 78.13 41.03% H2O, Alcohol,

Ether
Benzene, Toluene,
Xylene
P -Toluenesulfonic 172.20 18.62% Benzene, Toluene,

Acid Xylene
Thianaphthene 134.20 23.90% Iso-octane,

(Benzo[b]thiophene) Benzene,
Toluene, Xylene

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Chemicals for Halides Standard Preparation
Halide Standards, inorganic compound, water solvent

Name Mol Wt %F %Cl %Br Solvents
Sodium Fluoride 41.99 45.25 0 0 H2O
Sodium Chloride 58.44 0 60.66 0 H2O
Sodium Bromide 102.89 0 0 77.66 H2O
Halide Standards, organic compound, water solvent

Name Mol Wt %F %Cl %Br Solvents
Trifluoroacetic 114.02 49.99 0 0 H2O
acid
Trichloroacetic 163.39 0 65.09 0 H2O
acid
Tribromoacetic 296.74 0 0 80.78 H2O
acid
Halide Standards, organic compound, hydrocarbon solvent

Name Mol %F %Cl %Br Solvents
Wt
4-fluorobenzoic 140.11 21.92% 0 0 Isooctane,
acid Toluene
1,4-difluorobenzene 114.09 17.4% 0 0 Isooctane,
Toluene
Chlorocyclohexane 118.6 0 29.89 0 Isooctane,
Toluene
2,4,5- 197.45 0 53.86 0 Isooctane,
trichlorophenol Toluene
Bromobenzene 157.01 0 0 50.89 Isooctane,
Toluene
4-bromoacetanilide 214.06 0 0 37.33 Isooctane,
Toluene

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APPENDIX B
MATERIAL SAFETY DATA SHEETS – MSDS
MATERIAL SAFETY DATA SHEET
INDICATING DRIERITE™
Section I - General Information
Product Name: Indicating DrieriteTM

Manufacturer’s Name: W.A. Hammond Drierite Company
Emergency Phone Number: 937-376-2927, www.drierite.com
Telephone Number for Information: 1-937-376-2927
Address: 138 Dayton Avenue, P.O. Box 460, Xenia, Ohio 45385
Date Prepared: March 15, 2006
Contents: Calcium Sulfate 98%, Cobalt Chloride 2%
Trade Name: DrieriteTM
Section II - Hazardous Ingredients
Hazardous Ingredients: Cobalt chloride

CAS No.: 7646-79-9
%: 2
OSHA/PEL: 0.05 mg/m3
ACGIH/TLV: 0.05* mg/m3
*recommended
Section III - Physical Data
Melting Point: 1450 0C (decomposes)

Boiling Point: n/a
Water Solubility: 0.25 g/L
Specific Gravity (H2O = 1): 1.87
Vapor Pressure (mm Hg): n/a
Evaporation Rate (Butyl acetate = 1): n/a
Odor: none
Appearance: blue granules
Section IV - Fire and Explosion Hazard Data
Flash Point: n/a

Flammability Limits: LEL n/a, UEL n/a
Extinguishing Media: Not Combustible
Special Fire Fighting Procedures: n/a
Unusual Fire and Explosion Hazard: n/a

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Section V - Health Hazard Data
Route of Exposure: Inhalation, skin, ingestion

Carcinogenicity: NTP: No IARC Monographs: No OSHA Regulated: No
OSHA PEL: T.W.A. 200 μg/M3
Health Hazards: (Acute & Chronic)/Signs & Symptoms of Exposure: This product contains 2% cobalt
chloride which causes eye irritation and may cause skin and upper respiratory tract irritation. Overexposure to
cobalt compounds may cause nose and throat irritation and an allergic skin rash. They are mildly irritating to
the eyes and if ingested, may cause vomiting, diarrhea, and a sensation of hotness. Excessive inhalation and/or
ingestion of cobalt salts may affect the kidneys, lungs, and thyroid.
Medical Conditions Generally Aggravated by Exposure: Pre-existing respiratory and lung diseases.
First Aid Procedures

Inhalation: Remove to fresh air. If not breathing, give artificial respiration, preferably mouth-to-mouth. If
breathing is difficult, give oxygen. Call a physician as needed.
Ingestion: If patient is conscious, induce vomiting immediately. Obtain medical attention.
Eyes: Immediately flush eyes with plenty of water for at least 15 minutes. If irritation continues, obtain medical
guidance.
Section VI - Reactivity Data
Stability: Stable Conditions to avoid: n/a

Hazardous Polymerization: n/a Conditions to avoid: n/a
Incompatibilities (Materials to Avoid): Strong oxidizing agents.
Hazardous Decomposition or By-Products: Thermal decomposition may produce chlorine at 318 0C and
sulfurtrioxide@1450 0C.
Section VII - Special Protection Information
Respirator Protection: NIOSH/OSHA approved mask for dust.

Ventilation: Sufficient to meet TLV requirements.
Protective Clothing: Gloves or protective clothing not usually necessary, but may be desirable in specific
work situations.
Eye Protection: Side shield safety glasses or goggles.
Other Protective Equipment: Safety showers & eye washes.
Work/Hygienic Practices: Good housekeeping procedures should be followed to minimize dust.
Spilled or Released: Ventilate area of spill. Collect material into appropriate containers for disposal.
Waste Disposal Method: Dispose in closed containers, at an approved landfill, in accordance with local, state,
and federal regulations. Material may also be flushed with water to a waste water treatment system.
Precautions to be Taken in Handling & Storing: Keep in closed containers. Avoid generating dust.
Other Precautions: Avoid contact with eyes, skin, and clothing. Avoid breathing dust. Wash thoroughly after
handling.
The information contained herein is furnished without warranty of any kind. Users should consider these
data only as a supplement to other information gathered by them and must make independent
determinations of the suitability and completeness of the information from all sources to assure proper
use and disposal of these materials and the safety and health of employees and customers.

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OZONE (O3)
Product Name: Ozone

Manufacturer’s Name: PAC, L.P.
Manufacturer of Analytical Instrumentation
Emergency Phone Number: 800-365-2143, 281-580-0339
Address: 8824 Fallbrook Dr., Houston, TX 77064
Chemical Family: Gaseous Oxidant
Chemical Formula: 03
Trade Name/Synonyms: Ozone, Triatomic Oxygen
Issue Date: December 15, 2006
Product ID: UN
Section II - Hazardous Ingredients
Hazardous Ingredients: Ozone < 5% by weight in oxygen within detector.
Section III- Physical Data
Melting Point: -192.5°C

Boiling Point: -111.9°C
Water Solubility: 14 mg/L from 2% ozone in air.
Percent Volatile by Volume: 100
Absolute Density (Gas) at 101.325 KPa at 25°C: 1.964 kg/L
Relative Density gas at 25°C at 101.325 KPa Air: 1 - 1.66
Density of Solid Ozone at -195.6°C: 1.728
Material at Normal Conditions: Gas
Appearance and Odor at Ambient Temperature & Pressure: Clear, colorless gas (bluish at very high
concentrations) with pungent odor.
Section IV- Fire and Explosion Hazard Data
In the chemiluminescent detector, ozone is generated from oxygen at concentrations of less than 5%. At these
concentrations, the ozone/oxygen mixture is non-explosive, and will support combustion only slightly better
than oxygen. Suitable fire fighting equipment would be any that is useful for other hazards, such as electrical or
chemical. If high concentrations of ozone are present, self-contained breathing apparatus should be used.
Flash Point: NA
Flammability Limits in Air (%by volume): Lower NA, Upper NA.
Extinguishing Media: Shut off ozone gas, if possible, and use the appropriate media for the surrounding fire.
Special Fire Fighting Procedures: Though not flammable itself, ozone vigorously accelerates combustion.
Unusual Fire and Explosion Hazard: Materials which do not burn in air, may burn in ozone enriched
atmosphere.

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MULTITEK ANALYZER
Section V - Health Hazard Data
Threshold Limit Value: TWA 0.1 ppm STEL 0.3 ppm

OSHA PEL: T.W.A. 200 μg/M3
Acute Toxicity: Symptoms appear at a concentration of about 1 ppm by volume. Severity depends upon
concentration and length of exposure. Irritation or burning of the eyes, nose, or throat, lassitude, frontal
headache.
Route of Exposure: Inhalation
Emergency and First Aid Procedure: Remove from environment containing ozone. Most symptoms
disappear after leaving exposure. Severe cases may require oxygen and the need to seek medical help.
Section VI - Reactivity Data
Stability: Powerful oxidizing agent.

Incompatibilities: Anilines, Benzene, Oil and Grease, Rubber, Alkenes, Bromine, aromatic compounds,
dicyanogen, diethyl ether, dinitrogen tetraoxide, hydrogen bromide, 4-hydroxy-methyl-1, 6-heptadiene,
nitrogen trichloride, stibine, tetrafluorohydrazine.
Hazardous Decomposition Products: None
Section VI - Leak Procedures
The Chemiluminescence Detector contains an ozone generator which produces ozone from an external oxygen
supply. The outflow of the detector is passed through a scrubber or a high temperature zone before being
vented to atmosphere. For systems with a scrubber: the scrubber contains indicating DrieriteTM. Prolonged or
excessive ozone flow through the scrubber will cause the indicating DrieriteTM to turn black. This could be
due to ozone channeling through the MoleculiteTM, or as a result of a leak in the ozone generator. In the first
case, the scrubber should be recharged with fresh MoleculiteTM (see Section IX - Special Precautions) and
DrieriteTM; in the second, the ozone generator should be checked for leaks.
Ozone Generator Leak Check Procedure: Turn off power switch to ozone generator. Decrease incoming
oxygen pressure to two to five pounds. Turn off flow meters for all other gases, open ozone flow meter (ball
indicator should move to top of scale). Plug exit to scrubber. If no leaks are present, flow meter ball will drop to
zero. If leaks are present, ball will not drop, and all system components (O- rings, fittings, flow cell) should be
thoroughly checked and replaced if necessary.
Section VIII - Personal Protection Information
Respirator Protection: Self-contained breathing apparatus approved by U.S. Bureau of Mines is Adequate, if
used for a short period of time.
Ventilation: Use in well ventilated area. Clear area of personnel and ventilate area well if leak occurs.
Protective Gloves: N/A
Eye Protection: Safety glasses are required when working in the laboratory environment.
Other Protective Equipment: None.

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MULTITEK ANALYZER
Section IX - Special Precautions
Do not attempt to produce high or pure concentrations of ozone. Oxygen flows to the ozone generator should
be kept at a recommended rate of 30 mL/min and should not exceed 100 mL/min. In recharging the scrubber
tube, care should be exercised when removing or discarding the spent MoleculiteTM, since it may contain
ozone or shock sensitive compounds, and could pose an explosion or fire hazard. To minimize these hazards:
a) change the MoleculiteTM regularly;
b) if the MoleculiteTM is “caked” or “packed” do not forcibly remove while dry;
c) once the spent MoleculiteTM has been removed, it should be placed in a tray or other flat container
inside a safety hood to allow the ozone to dissipate before disposal.
The odor threshold of ozone for the normal person is 0.01 – 0.015 ppm by volume in air. Concentrations of 1
ppm produce an unpleasant sulfur-like odor.
The safe level for short term human exposure to concentrations of ozone in excess of 0.1 ppm (the TLV) is not
known with certainty. Probably 2 ppm is safe for several minutes, provided that no respiratory infection is
present. The atmospheric concentration immediately hazardous to life is likewise not known, but inhalation of
50 ppm for thirty minutes would probably be fatal.

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MULTITEK ANALYZER

MOLECULITE™
Product Name: MoleculiteTM Oxidation Catalyst

Manufacturer’s Name: Molecular Products Ltd.
Emergency Phone Number: +44 1371 830676
Address: Mill End, Thaxted Essex CM6 2LT, United Kingdom
Date Prepared: July 3, 2002
Chemical Name: Transition Metal Oxides
Composition: Manganese dioxide concentration in mixture does not exceed 90 weight % and copper oxide
concentration in mixture does not exceed 45 weight %.
Section II - Toxicity Hazards
DOT Hazard Class: Not a hazardous material.

CAS No: Manganese Dioxide, 1313-13-9, and copper oxide, 1317-38-0.
Hazards Identification: Harmful by inhalation and if swallowed.
Section III - Physical Data
Solubility in water: slight

Appearance: Black solid, odorless
Relative Density: 2-3 g/cm3
Stability & Reactivity: Material is stable but can react violently with hydrogen peroxide, inorganic chlorates,
and aluminum powder.
Other: strong oxidizing substance
Section IV- Fire and Explosion Hazard Data
Unusual Fire and Explosion Hazard: MoleculiteTM Catalyst is noncombustible. Packaging may be
combustible.
Flash Point: NA
Extinguishing Media: Water, foam, CO2, powder are all suitable.
Protective Measures: Breathing apparatus may be needed.
Section V - First Aid Measure
Inhalation: Remove from exposure. Obtain medical attention

Skin: Drench with clean water. Obtain medical attention if skin becomes inflamed.
Eyes: Irrigate thoroughly with clean water. Obtain medical attention
Ingestion: Wash out mouth thoroughly. Obtain medical attention.
Section VI - Accidental Release
Personal Precautions: Avoid inhaling dust. Avoid skin and eye contact.
Environmental Precautions: No hazard
Recovery: Contain material. Sweep or vacuum up.

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MULTITEK ANALYZER
Section VII - Handling & Storage
Store in a clean dry environment. Avoid direct sunlight or heat sources. Keep containers closed. Keep away
from organic material and strong reducing agents.
Section VIII - Control Measures
Occupational Exposure Limits: Manganese Dioxide - TWA/8h: 5 mg (Mn)/m3

Waste Disposal: Dispose of according to local, state, and federal regulations.
Personal Protective Equipment: Classified dust mask recommended; general purpose rubber gloves, glasses
to protect eyes against dust, wash skin after contact.

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MULTITEK ANALYZER

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MULTITEK ANALYZER
APPENDIX C
STATIC AND DYNAMIC IPADDRESSING
MultiTek® IP Address Configuration
The MultiTek® Analyzer default communication with the PC is via a network router using dynamic IP
Block Diagram (Section 2, Figure 2-8). Static IP addressing is also supported, but can only be done
once the initial setup has been completed. MultiTek® Software must be running on a Windows PC in
order to operate the MultiTek® analyzer. All the settings and results data are stored on the PC.
NOTE
DHCP must be enabled in the router. After initial setup is complete, a static IP address and subnet can be
set.
Set Static IP Addressing

To set the IP address to a static address, open the MultiTek® Software, enter the user ID and
password, select the instrument desired and click on the Config IP button (Figure C-1), instead of the
Logon button. The instrument must be online and available or the Config IP button will not be
active. Before entering the static IP address, the IP address and subnet mask should be determined by
your company’s IT personnel or the individual setting up the network and PC. The IP address and
subnet mask of the PC should also be determined. Both the instrument and PC must have the same
sub network address.
Figure C-1: Instrument Logon

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MULTITEK ANALYZER
Configure IP Address
Select Use the following IP address, then type in the assigned IP address and subnet mask (Figure C-
2b). Click on Write to instrument to set the new IP address in the instrument, click OK in the
Confirmation screen (Figure C-3), and Close. Turn off the power to the MultiTek®. Repeat this
process for each instrument to be connected to the network with a static IP address; exit the Logon
screen when complete.
Figure C-2 Configure IP Address
a) Dynamic IP Address b) Static IP Address
Figure C-3 IP Configuration Complete
After the static IP address is set in the instrument, set the PC’s IP address to an address within the
same sub network as the MultiTek® or network switch attached to the instrument(s) (figure C-4). Go
to Network Connections in Control Panel and select and right-click on the Ethernet controller and
click on Properties.
Highlight Internet Properties (TCP/IP), click on Properties. When the Internet Protocol Properties
screen appears select “Use the following IP address, then enter the IP address and subnet mask
(Figure C-4). Using the example above, 192.168.1.10 with a subnet mask of 255.255.255.0 would be
work as long as no other device on the network had the same address. If duplicate IP addresses are
used, the PC/MultiTek® will not be able to communicate over the network. Click on OK and close
the IP Properties, Network Properties and Control Panel screens.

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MULTITEK ANALYZER
Figure C-4 PC Static IP Configuration
Connect the PC and instrument(s) directly, or through a network switch. Make sure the PC and
network switch are turned on and running, then power on the instrument(s). Start the MultiTek®
Software and verify the IP address for the instrument is correct. Log onto the MultiTek®.
Set Dynamic IP Addressing

For dynamic IP addressing, open the MultiTek® Software, enter the user ID and password, select the
instrument desired and click on the Config IP button (Figure C-1), instead of the Logon button. The
instrument must be connected to the PC and available, or the Config IP button will not be active.
Select “Obtain an IP address automatically” (Figure C-2a). Click on Write to instrument to set the
new IP addressing in the instrument, click OK in the Confirmation screen (Figure C-3), and Close.
Turn off the power to the MultiTek®. Repeat this process for each instrument to be connected to the
network with a dynamic IP address; exit the Logon screen when complete.
After the dynamic IP address is set in the instrument, set the PC’s IP address to dynamic (figure C-5).
Go to Network Connections in Control Panel and select and right-click on the Ethernet controller
and click on Properties.
Highlight Internet Properties (TCP/IP), click on Properties. When the Internet Protocol Properties
screen appears select “Use Obtain an IP address automatically and click on OK. Close the IP
Properties, Network Properties and Control Panel screens.

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MULTITEK ANALYZER
Figure C-5 PC Dynamic IP Configuration
Connect the PC and instrument(s) through a network router (with DHCP is enabled). Make sure the
PC and network router are turned on and running, then power on the instrument(s). Start the
MultiTek® Software and verify the IP address for the instrument appears in the Logon screen. Log
onto the MultiTek®.

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MULTITEK ANALYZER
INSTALLATION PROBLEM
REPORT
Company: Installation Date:

Contact: Installed By:
Address: PAC Representative:
Sales Order #:
City: St: Zip:
Country: Territory: Fax or e-mail complete report to Service
Manager
Phone: Fax: fax: 281-580-0719  e-mail:
service@paclp.com
E-mail:
Purchase Date S/N Model # Install Date
Problem(s)
Model: S/N:
Part # Description of Problem
Model: S/N:
Model: S/N:
Type of Problem: Appearance Broken Electronic Missing Off Spec Wrong

Assembly Electric Leak Mechanical Non-function

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MULTITEK ANALYZER
END OF DOCUMENT

MultiTek Operation

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MultiTek ®

8824 Fallbrook Dr.• Houston, Texas 77064 • USA

© 2012 by Petroleum Analyzer Company, L.P.

MS Windows, MS Windows XP, and MS Windows Professional are registered

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

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

MAN MULTITEK-1 OPERATION Page i

This manual contains confidential and proprietary information…

Page ii MAN MULTITEK-1 OPERATION

Rev A First release September 2009

Rev B Diagrams and Software Updates April 2010

Rev C Software Updates, Corrections November 2010

Rev D Software Updates and Corrections August 2011

Rev E Software v2.0.0.0 Updates January 2012

Copyright ©2012, by PAC L.P., Houston, Texas.

MAN MULTITEK-1 OPERATION Page iii

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Page iv MAN MULTITEK-1 OPERATION

Warrants and Representations

MAN MULTITEK-1 OPERATION Page v

Page vi MAN MULTITEK-1 OPERATION

STANDARD LIMITED WARRANTY

MAN MULTITEK-1 OPERATION Page vii

5. Exclusive Remedy. THE FOREGOING LIMITED WARRANTY CONSTITUTES BUYER’S EXCLUSIVE

II. Limitations on PAC Liability

8824 Fallbrook Dr. • Houston, Texas • 77064 - 9912 • USA

Page viii MAN MULTITEK-1 OPERATION

 EN 55022: 1994, Class A/B – “Information Technology Equipment - Radio Disturbance

 EN 550082-1: “Electromagnetic compatibility – Generic Immunity Standard,” “Generic

Correct disposal of Waste Electrical and Electronic

MAN MULTITEK-1 OPERATION Page ix

RETURNED PRODUCT WARRANTY DETERMINATION

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

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

Record of Serial Number and Purchase Date

Purchase Date: _________________________

Page x MAN MULTITEK-1 OPERATION

Visible Loss or Damage

Concealed Loss or Damage

MAN MULTITEK-1 OPERATION Page xi

Phone Number: (800) 444-TEST or (281) 580-0339

Fax Number: (281) 580-0719

Email Support: sales@paclp.com

Page xii MAN MULTITEK-1 OPERATION

MAN MULTITEK-1 OPERATION Page xiii

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MAN MULTITEK-1 OPERATION Page 1

Page 2 MAN MULTITEK-1 OPERATION

General Guidelines for Sample Analysis ..............................................................158

SECTION 6 MAINTENANCE / TROUBLESHOOTING ........................................169

APPENDIX B MATERIAL SAFETY DATA SHEETS – MSDS .............................201

MAN MULTITEK-1 OPERATION Page 3

BURN HOT SURFACE HAZARD

ELECTROCUTION VOLTAGE HAZARD

BURN HAZARD HOT SURFACE

ELECTRIC GROUND HAZARD

RELEASE OF PRESSURE HAZARD

Page 4 MAN MULTITEK-1 OPERATION

 Section 1 – Introduction: Gives a description of the MultiTek® Analyzer, product components,

 Section 6 – Troubleshooting & Maintenance: A guide to troubleshooting and regular maintenance of

MAN MULTITEK-1 OPERATION Page 5

1. Click Start > Programs > PAC.

The following terms are used in this guide: