SP1 789-0568 3-in-1 GC/MSD DRS Analyzer Installation and

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Agilent SP1 7890-0568

3-in-1 GC/MSD DRS

Analyzer

Installation and Checkout

Guide

Agilent Technologies

Notices

© Agilent Technologies, Inc. 2011

No part of this manual may be reproduced in any form or by any means (including electronic storage and retrieval or translation into a foreign language) without prior agreement and written consent from Agilent

Technologies, Inc. as governed by United

States and international copyright laws.

Manual Part Number

7890-0568

Edition

First edition, November 2011

Printed in USA

Agilent Technologies, Inc.

5301 Stevens Creek Boulevard

Santa Clara, CA 95051 USA

Warranty

The material contained in this document is provided “as is,” and is subject to being changed, without notice, in future editions. Further, to the maximum extent permitted by applicable law, Agilent disclaims all warranties, either express or implied, with regard to this manual and any information contained herein, including but not limited to the implied warranties of merchantability and fitness for a particular purpose. Agilent shall not be liable for errors or for incidental or consequential damages in connection with the furnishing, use, or performance of this document or of any information contained herein. Should

Agilent and the user have a separate written agreement with warranty terms covering the material in this document that conflict with these terms, the warranty terms in the separate agreement shall control.

Technology Licenses

The hardware and/or software described in this document are furnished under a license and may be used or copied only in accordance with the terms of such license.

Restricted Rights Legend

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(Technical Data) and 12.212 (Computer Software) and, for the Department of Defense,

DFARS 252.227-7015 (Technical Data -Commercial Items) and DFARS 227.7202-3

(Rights in Commercial Computer Software or Computer Software Documentation).

Safety Notices

C A U T I O N

A CAUTION notice denotes a hazard. It calls attention to an operating procedure, practice, or the like that, if not correctly performed or adhered to, could result in damage to the product or loss of important data. Do not proceed beyond a CAUTION notice until the indicated conditions are fully understood and met.

W A R N I N G

A WARNING notice denotes a hazard. It calls attention to an operating procedure, practice, or the like that, if not correctly performed or adhered to, could result in personal injury or death. Do not proceed beyond a WARNING notice until the indicated conditions are fully understood and met.

3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide

Contents

1 General Information for the 3-in-1 Analyzer

Objective

6

System Overview

7

Before Getting Started

8

Installation Summary

9

2-way Purged Splitter Plumbing and Operation Specifics

11

Backflushing Parameters

12

Software

13

2 S-VOA Analyzer Specifics

Copying and Pasting S-VOA Files

17

Description of VOA Files

18

Loading and Relocking the S-VOA Method

19

Loading the Acquisition Method

20

Making the Relocking Runs

21

Relocking Sequence

21

Confirming the Lock

22

DRS Analysis of the S-VOA Checkout Mix

24

3 VOA Analyzer Specifics

Copying and Pasting VOA Files

30

Description of VOA Files

31

Loading and Relocking the Headspace VOA Method

32

Standards Preparation for Relocking the VOA Column

34

Loading the VOA Acquisition Method

34

3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide 3

Relocking Sequence

34

Confirming the Lock

36

DRS Analysis of the Solvents-Plus Checkout Mix

37

4 Pesticides Analyzer Specifics

Copying and Pasting Pesticides Files

41

Description of Pesticides Files

42

Loading and Relocking the Pesticides Method

43

RT Locking the Method

45

Relocking Sequence

45

Confirming the Lock

47

DRS Analysis of the Pesticides Checkout Mix

48

5 Allowed 3-in-1 System Configurations

6 Consumables and Supplies

4 3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide

Agilent SP1 7890-0568 3-in-1 GC/MSD DRS Analyzer

Installation and Checkout Guide

1

General Information for the 3-in-1

Analyzer

Objective 6

System Overview 7

Before Getting Started 8

Installation Summary 9

2-way Purged Splitter Plumbing and Operation Specifics 11

Backflushing Parameters 12

Software 13

Agilent Technologies 5

1 General Information for the 3-in-1 Analyzer

Objective

This document will guide you through the process of loading the semivolatiles (S-VOA) acquisition method, relocking the method, running the checkout sample, and analyzing the results using Deconvolution Reporting software (DRS). This process will be repeated for the volatiles (VOA) method. The pesticides method locking and DRS report are also discussed.

Read all sections in this chapter. You can then proceed to any section, depending upon which application will be run first.

Chapter 2 , “S-VOA Analyzer Specifics”

Chapter 3 , “VOA Analyzer Specifics”

Chapter 4 , “Pesticides Analyzer Specifics”

At the end of this document you will find

Chapter 5 , “Allowed

3-in-1 System Configurations” which shows allowed hardware

options and Chapter 6 , “Consumables and Supplies” which lists

the replaceable parts and consumables used for these applications.

6 3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide

General Information for the 3-in-1 Analyzer 1

System Overview

The Agilent 3-in-1 GC/MSD DRS Analyzer, SP 7890-0568, is designed for the analyses of S-VOA, VOA, and pesticides compounds by GC/MSD, with Deconvolution Reporting software (DRS) for data reduction. The system includes an

Agilent 7693A Autosampler, 7697A Headspace Sampler (HS),

7890A GC, and 5975C MSD.

A programmable temperature vaporizing multimode inlet (MMI) is used in hot splitless mode (HSL) for S-VOA and pesticide analyses. Cold splitless (CSL) and solvent vent modes (SV) are also available. A split-splitless (S/SL) inlet can be used in place of the MMI. A post column, 2-way purged splitter enables column backflushing of heavy matrix and column removal, without venting. A second inlet, S/SL, operates in hot split mode (HSP) for HS-VOA analyses.

The 2-way purged splitter operates as a column combiner. It combines the outlet flows from the S-VOA and VOA columns to a

1.1 m × 0.15 mm SilTek treated restrictor into the MSD transfer line. The 2-way purged splitter also provides makeup gas for good peak shapes and backflush flow.

The S-VOA DRS database-library (DBL) includes the single component analytes from USEPA methods 525 and

8270 plus others; 338 total. The Solvents-Plus DRS DBL includes the analytes from USEPA methods 524 and 8260 plus others; 369 total. The pesticides DRS DBL includes 927 pesticides and endocrine disruptors.

A top view schematic of the major components of the 3-in-1

Analyzer is shown in

Figure 1 on page 8.

3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide 7

8

1 General Information for the 3-in-1 Analyzer

Volatiles run on the rear column at 1.2 mL/min CF or

Semi-volatiles or pesticides run on the front column at ~ 1 mL/min CF

~ 7 mL/min bleeder

1 m × 0.254 id (0.010”)

Aux ramp psi

7890A

7693 Tray

S/SL

5975C

EI MSD

Aux = 320 or 310

MMI or

S/SL

2 mL/min to MSD

7693 ALS

7697A

Headspace with or without

Sampler

2-way splitter with make-up acting as a combiner

Figure 1 Top view of the 3-in-1 Analyzer

Before Getting Started

Agilent recommends that you watch the series of DRS training videos (p/n 5973-1731) before you follow these procedures. If you are not familiar with retention time (RT) locking, DRS,

AMDIS Deconvolution software, or the QEdit function in the

Agilent MSD ChemStation, these videos will be very helpful.

3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide

General Information for the 3-in-1 Analyzer 1

Installation Summary

1 Install the GC and MSD.

• Connect all gases using required purifiers, and make sure supply pressures are high enough for the method

(especially for backflushing at 60 psig).

• Connect the AC power.

• Start the GC gases flowing to purge the system.

2 Reconnect the CFT restrictor tube to the MSD from the plate located in oven.

3 Pump down the MSD with cool zones.

4 Check for leaks.

5 Load the following software:

• MSD ChemStation

• NIST 08 Library and AMDIS

• DRS software

• S-VOA DRS DBL, Solvents-Plus DRS DBL

Copy files from the CD-ROM supplied by the Specials Group:

(Detailed information is supplied in later sections).

• Methods to Methods directory

• Data files to Data directory

• Macros to MSExe directory

• AMDIS, MSSearch, and DRS config files to their respective directories

• Tune file for MSD

6 Edit the msdchem.ini with the method desired for startup, such as S-Voa_3in1_acq_BF.m, to prevent Method Resolution.

7 Load and resolve methods. (Resolution may not be needed.)

8 Autotune the MSD.

9 Run a blank solvent.

10 Run the S-VOA checkout mix twice.

11 Relock the RT of the method on the second run.

3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide 9

1 General Information for the 3-in-1 Analyzer

12 Rerun the checkout sample with the relocked method, if needed.

13 In DA, run Quant + DRS single on the checkout sample data file.

14 Inspect the report to assure all peaks in the checkout mix are found with a match factor above the method default.

15 Run Solvents+ checkout mix, using headspace twice.

16 Relock the RT of method on the second run.

17 Rerun the checkout sample with the relocked method, if needed.

18 In DA, run Quant + DRS single on the checkout sample datafile.

19 Inspect the report to assure all peaks in the checkout mix are found with a match factor above the method default.

20 Archive:

• Stored method(s) with RTL calibration

• Autotune file

• Checkout sample data files

• DRS reports from checkout sample data files

• Any install notes for future service people (for example:

AUX EPC supply pressure too low, so backflushing pressure reduced and time extended)

10 3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide

General Information for the 3-in-1 Analyzer 1

2-way Purged Splitter Plumbing and Operation Specifics

The 2-way purged splitter operates as a column effluent flow combiner. The splitter may be mounted on either side of the

GC oven, as the restrictor is long enough to reach the MSD. The rear VOA column is connected with a SilTite ferrule to the first position closest to the makeup gas line from the Aux EPC module. This minimizes the chance of contamination from heavy matrix that may elute from the S-VOA column. The front

S-VOA column is connected with a SilTite ferrule to the second

(middle) position of the splitter. The restrictor is connected with a SilTite ferrule to the last position of the splitter, furthest from the makeup gas line.

The Aux EPC module is run in ramped pressure (RP) mode.

This is done to maintain a constant 2 mL/min flow to the MSD as the oven temperature increases. It can not be run in constant pressure (CP) mode nor in constant flow (CF) mode. If run in

CP mode, the flow to the MSD will be higher than 2 mL/min when the oven is cold. If run in CF mode, a true 2 mL/min will not be maintained due to the temperature differences between the oven and MSD transfer line.

Each of the three methods, S-VOA, VOA, and pesticides, has a different pressure ramp for the Aux EPC based on both the oven program and the transfer line temperature.

The restrictor (column 3) is a 1.1 m × 0.150 mm id piece of

SilTek treated fused silica tubing (p/n 160-7625-5). It is connected to the splitter with a SilTite ferrule. The other end is connected to the MSD transfer line using either a SilTite or graphite/vespel ferrule with the appropriate nut.

A bleed restrictor is attached to the makeup gas line with a

T connector in between the Aux EPC and the splitter plate. This restrictor is 1 m × 0.010 mm id SS (p/n 0100-2354), and provides over pressure relief for pulsed injections and RT locking.

3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide 11

1 General Information for the 3-in-1 Analyzer

Backflushing Parameters

The S-VOA and pesticides methods include parameters for backflushing. The parameters are based on the MSD pump type.

Agilent recommends that a turbo pump be used as they can handle higher flows and therefore shorter backflush times. A diffusion pump can be used but the backflush time will be at least 10 minutes . The Aux EPC pressure for backflushing with a diffusion pump can not exceed 25 psi, or excessive flow will go to the pump. Experiments have shown that the 10 minute backflush time is necessary to clean heavy hydrocarbons, often found in S-VOA samples, from the column. In all cases when backflushing the front S-VOA-pesticides column, set the rear

VOA column inlet to a lower pressure (15 psi). This step is necessary to prevent the rear column from attempting to maintain a normal forward flow. However, the VOA method itself does not include backflushing due to the overall cleaner nature of the samples introduced. Listed in

Table 1 are the

pressures, flows, and times for backflushing for either the turbo or the diffusion pump. The void volumes for the pesticides method, not shown, are just slightly larger due to the oven temperature difference.

Table 1 Backflush parameters for the front column, using either the S-VOA or pesticides method

Method

S-VOA

Pump

Aux EPC

(psi)

Turbo 60

Diffusion 24

Backflush

(min)

5

10

1

1

Inlet pressure

Front

(psi)

Rear

(psi)

15

15

Column flow Front column

Front S-VOA

(mL/min)

Rear VOA

(mL/min) Void volumes

–1.54

–0.36

–3.3

–0.43

8.6

7.3

12 3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide

General Information for the 3-in-1 Analyzer 1

Software

All acquisition methods were built using the Agilent MSD

Chemstation software E.02.01 or later. Data analysis methods were built using E.02.00. None of the methods are backward compatible. The NIST08 used was version 2.0 f, Oct 8, 2008.

AMDIS version 2.66, create 121.82 was used to create all AMDIS files.

Table 2

lists the methods and files that should be used for each of the 3-in-1 Analyzer modes of operation.

Table 2 Files for use with the 3 modes of the 3-in-1 Analyzer

Acquisition

Checkout DA

Full DA

Checkout msl

Full msl

*.cal

*.csl

Agilent.L

Checkout.D

Onsite.ini

Default.ini

Nistms.ini

S-VOA

S-VOA_3in1_acq_BF.M

S-VOA_3in1_DA-checkout.M

S-VOA_3in1_DA.m

S-VOA_3in1_checkout.msl

S-VOA_1.msl

S-VOA_3in1.cal

S-VOA_3in1.csl

8270_DRS.L, 525_DRS.L

S-VOA_3in1_checkout.D

Onsite.ini

Default.ini

Nistms.ini

AmdisConfig.txt AmdisConfig.txt

VOA

VOA_3in1_acq.M

VOA_3in1_DA-checkout.M

VOA_3in1_DA.m

VOA_3in1_checkout.msl

CF_SOLV.MSL

VOA_3in1.cal

VOA_3in1.csl

CF_SOLV.L

VOA_3in1_checkout.D

Onsite.ini

Default.ini

Nistms.ini

AmdisConfig.txt

Pesticides

Pest_3in1_acq_BF.M

Pest_3in1_DA-checkout.M

Pest_3in1_DA.m

Pest_3in1_checkout.msl

RTLPest3.msl

Pest_3in1.cal

Pest_3in1.csl

RTLPest3.L

Pest_3in1_checkout.D

Onsite.ini

Default.ini

Nistms.ini

AmdisConfig.txt

3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide 13

1 General Information for the 3-in-1 Analyzer

14 3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide

Agilent SP1 7890-0568 3-in-1 GC/MSD DRS Analyzer

Installation and Checkout Guide

2

S-VOA Analyzer Specifics

Copying and Pasting S-VOA Files 17

Description of VOA Files 18

Loading and Relocking the S-VOA Method 19

Loading the Acquisition Method 20

Making the Relocking Runs 21

Relocking Sequence 21

Confirming the Lock 22

DRS Analysis of the S-VOA Checkout Mix 24

The S-VOA portion of the 3-in-1 Analyzer is based on the

SP1 7890-0459 S-VOA analyzer with modifications. The single-taper with glass wool liner, (p/n 5190-2293), introduced in early 2011, is UI deactivated and is used for HSL. CSL injections can be done using a 2 mm dimple liner

(p/n 5190-2296) and conditions in Application Note 5989-7875.

The 3-in-1 Analyzer uses a 20 m × 0.18 mm × 0.36 um DB-8270D column (p/n 121-9723) which is a more inert version of

DB 5-MS. The system is RT locked to Phenanthrene-d10

at 11.000 min.

The S-VOA acquisition method, S-voa_3-in-1_acq_bf.m, contains both scan and SIM parameters. Scan only acquisitions can be run at a sampling rate of 2^2 or 2^1. The SIM parameters are those for the most common 100+ compounds from USEPA

Method 525. If SIM/scan is run, the rate should be set to 2^1.

With SIM/scan, the SIM signal can be used for quantitation of the most important analytes, and the scan signal can be used for deconvolution and identification of all 338 compounds.

Agilent Technologies 15

2 S-VOA Analyzer Specifics

The 338 compound quant database was taken from Agilent's

G1677AA S-VOA DRS DBL, supplied with this analyzer. The

RTs of the earliest and latest eluters have been slightly modified due to the Aux EPC pressure ramp. It is important to use the

methods and files listed in Table 2 on page

system performance.

13, for the best

The 338 compounds are listed in application note: Semivolatiles

Retention Time Locked (RTL) Deconvolution Databases for

Agilent GC/MSD Systems. Mike Szelewski, Agilent Technologies,

Publication 5989-7875EN, www.agilent.com/chem . A copy of this application note is included on the G1677AA S-VOA DRS

DBL CD that came with this analyzer.

S-voa front column view 20 m × 180 um × 0.36 um DB-8270D (p/n 121-9723)

Semi-volatiles or pesticides run on the front column at ~ 1 to 1.2 mL/min CF,

Method and RTL dependent

7693 Tray

5975C

EI MSD

Aux = 320 °C

7693A

Rear volatiles column at 0.4 mL/min CF

Aux EPC maintains ~0.4 to 0.6 mL/min makeup

Aux ramp psi

MMI or

S/SL front inlet

~1 mL/min CF

7697A

Headspace with or without

Sampler

2 mL/mjn to MSD

CP Restictor 1.1 m × 0.15 mm id

Silcotek deactivated tubing,

Agilent p/n 160-7625-5

Figure 2 Front column view of the 3-in-1 Analyzer

16 3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide

S-VOA Analyzer Specifics 2

Copying and Pasting S-VOA Files

Copy the S-VOA files from the CD supplied by the Specials

Group and paste them into the location listed in

Table 3 . This

CD is not one of the software installation CDs.

Table 3 Copying and pasting S-VOA files

File name

S-VOA_3in1_acq_BF.m

S-VOA_3in1_DA-checkout.m

S-VOA_3in1_DA.m

S-VOA_3in1_checkout.D

S-VOA_3in1_checkout.msl

S-VOA_3in1_checkout.cid

S-VOA_3in1.cal

S-VOA_3in1.csl

Onsite.ini

Default.ini

Nistms.ini

AmdisConfig.txt

Location to paste the copied file

C:\MSDchem\1\Methods

C:\MSDchem\1\Data

C:\NIST08\AMDIS32\Lib

C:\NIST08\AMDIS32\Lib

C:\NIST08\Mssearch

C:\Program Files\Agilent\MSD Deconvolution

Reporting Software

Additional file information

Verify the following files in Table 4 were installed.

Table 4 Additional S-VOA file information

File name

8270_DRS.L, 525_DRS.L

Semivoas_1.msl

Semivoas_1.cid

Location to paste the copied file

These 2 libraries should have installed into

C:\Database when the G1677AA S-VOA DRS database was installed.

These 2 files should have installed into

C:\NIST08\AMDIS32\Lib when the G1677AA

S-VOA DRS database was installed.

3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide 17

2 S-VOA Analyzer Specifics

Description of VOA Files

S-voa_3in1_acq_BF.m

– the method that has been RT locked by the Specials Group using the installed column. This method will be relocked as part of the system installation and will be used for data acquisition of the checkout mix and customer samples in scan. The method includes SIM ions as discussed above.

S-Voa_3in1_DA-checkout.m

–the data analysis method that contains 29 compounds in the quantitation database, that will be used for the DRS analysis of the checkout mix.

S-Voa_3in1_DA.m

–the data analysis method that contains

338 compounds in the quantitation database that can be used for samples.

S-voa_3in1_Checkout.D

–the datafile that was acquired by the

Specials Group as final checkout. It can be used as a reference for the Checkout sample run as part of the system installation.

S-voa_3in1_checkout.msl, S-voa_3in1_checkout.cid,

S-voa_3in1.cal, S-voa_3in1.csl– these are the AMDIS files designed for the S-VOA portion of the 3-in-1 Analyzer.

Semivoas_1.msl, Semivoas_1.cid

–this is the 338 compound

S-VOA DRS Database-Library and associated chemical information directory.

Onsite.ini, Default.ini, Nistms.ini, AmdisConfig.txt

–these are configuration files specific to the analyzer and should over-write the exisiting files in the specified directories.

18 3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide

S-VOA Analyzer Specifics 2

Loading and Relocking the S-VOA Method

The GC/MSD S-VOA checkout mix (p/n 5190-0473) is a solution of 29 compounds, each at 10 ppm (10 ng/µL), in dichloromethane (methylene chloride). The names and CAS

numbers of the compounds in the mix are listed in Table 5 in

RT order.

Table 5 S-VOA checkout mix compound list

Compound

N-Nitrosodimethylamine

Aniline

1,4-Dichlorobenzene-d4

Isophorone

1,3-Dimethyl-2-nitrobenzene

Naphthalene-d8

Hexachlorocyclopentadiene

Mevinphos

Acenaphthene-d10

2,4-Dinitrophenol

4-Nitrophenol

2,4-Dinitrotoluene

Fluorene

4,6-Dinitro-2-methylphenol

Trifluralin

Simazine

Atrazine

Pentachlorophenol

Terbufos

9.016

9.482

9.542

9.574

9.671

10.056

10.078

10.190

RT

3.770

6.190

6.538

7.299

7.707

7.746

8.614

10.654

10.680

10.796

10.820

7786347

15067262

51285

100027

121142

86737

534521

1582098

CAS number

62759

62533

3855821

78591

81209

1146652

77474

122349

1912249

87865

13071799

3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide 19

2 S-VOA Analyzer Specifics

Table 5 S-VOA checkout mix compound list (continued)

Compound

Chlorothalonil

Phenanthrene-d10

Aldrin

Heptachlor epoxide -isomer B

Endrin

4,4'-DDT

3,3'-Dichlorobenzidine

Chrysene-d12

Benzo[b]fluoranthene

Perylene-d12

RT

10.980

11.000

11.816

12.119

12.833

13.158

13.597

13.661

14.840

15.363

CAS number

1897456

1517222

309002

1024573

72208

50293

91941

1719035

205992

1520963

Open one of the vials of the S-VOA checkout mix and transfer it to an autosampler vial. Place the autosampler vial in tray position 1. This will be used for relocking the previously locked method.

The S-VOA method is RTLocked to Phenanthrene-d10 at

11.000 minutes.

Loading the Acquisition Method

Open the ChemStation instrument control software and click

Method > Load Method and choose the method called

S-voa_3in1_acq_BF.m. This method should inject 1 µL, but verify the syringe size and injection volume after loading.

20 3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide

S-VOA Analyzer Specifics 2

Making the Relocking Runs

N O T E

To save time, use the GC keyboard to set the current oven temperature to

250 °C while doing the next step. Do NOT save the method, as this is just temporary. This will preheat the oven and give better time matching in the relock step. As soon as the sequence starts, the oven temperature will return to 40 °C before the injection is made.

Relocking Sequence

1 Go to the Sequence>Load Sequence menu item in the

ChemStation Instrument control software and load the file

Default.s. Edit the sequence table to look like

Figure 3 .

Figure 3 S-VOA sequence table for RTL relocking runs

2 Save the sequence as Semivoas_Relock_Seq.s. Make sure the vial of S-VOA checkout mix (p/n 5190-0473) is located in position

1 of the autosampler tray.

3 Go to the Sequence>Run Sequence menu item and run the sequence.

4 After the sequence is completed, start the Instrument 1 Data

Analysis program.

5 Use the Method>Load Method menu item to load the same

S-voa_3in1_acq_BF.m file that was run in the sequence.

3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide 21

2 S-VOA Analyzer Specifics

N O T E

6 Load the second run from the sequence (the first run was just to clean out the column) named S-voa_3in1_Relock_2.D.

7 Select the View>RTLock Setup menu item to open the RTLock screen. Proceed with relocking the acquisition method,

S-voa_3in1_acq_BF.m, using datafile S-voa_3in1_Relock_2.D.

The new inlet pressure has now been saved to the method.

The new pressure will not be applied to the method nor the GC until the method is reloaded or is run.

8 Select the View>Return to Data Analysis menu item to close the

RTLock Setup View.

9 On the GC keyboard, press the Front Inlet key to view the pressure setpoints for the inlet the method is using.

10 In the Data Acquisition view, re-load your method

S-voa_3in1_acq_BF.m.

You should see the new calculated locking pressure downloaded as the setpoint for the inlet.

Confirming the Lock

If the RT lock time of Phenanthrene-d10 was off by more than ± 0.010 minutes after relocking the method, an optional third run of the checkout mix can be made to verify the locking pressure and time.

The best way to do this is to add a line to the existing sequence, and then use the Sequence > Position and Run menu item.

22 3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide

S-VOA Analyzer Specifics 2

Figure 4 S-VOA checkout mix total ion chromatogram

3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide 23

2 S-VOA Analyzer Specifics

DRS Analysis of the S-VOA Checkout Mix

This step is to confirm that the RTs across the entire elution range of the chromatogram match those in the method closely enough to have all peaks fall in their recognition windows.

1 In Data Analysis, using the Method > Load Method… menu item, load the method S-Voa_3in1_DA-checkout.m.

2 Using the File > Load Data File… menu item, load the last

checkout mix relocking run that was made. Select the menu item DRS > Quant + DRS single file. After a moment, you will see activity on the computer as DRS performs a quantitative analysis, deconvolutes the mass spectra, and searches the

S-voa_3in1_checkout.msl AMDIS database, then searches the

NIST08 library. Depending upon the deconvolution settings chosen, the DRS process will typically take 2–4 minutes. At this point, DRS will generate a report that looks similar to

(but not necessarily identical to) Figure 5 on page

3 Inspect the report and compare it to the list of compounds in the sample.

Also note that the ChemStation Amount column gives only estimated amounts for the compounds that it identified.

These amounts are based on a single point response factor that is supplied with your method. You must calibrate any compounds that you wish to quantify as you do with any other GC/MS method.

The AMDIS amount column is completed after the QEdit process.

The AMDIS column of the DRS report should find all the analytes in the test mix, typically with match factors

> 90 and with RT differences of < 10 seconds.

24 3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide

S-VOA Analyzer Specifics 2

.

MSD Deconvolution Report

Sample Name: S-VOA checkout

Data File: C:\msdchem\1\DATA\S-voa_3in1_checkout.D

Date/Time: 8:52:43 AM Wednesday, May 25, 2011

Adjacent Peak Subtraction = 1

Resolution = Medium

Sensitivity = High

Shape Requirements = Medium

The NIST library was searched for the components that were found in the AMDIS target library.

RT

3.7997

6.1762

6.4935

7.2780

7.6890

7.7469

8.5964

9.0028

Cas number Compound Name

62759

62533

3855821

78591

81209

1146652

77474

7786347

N-Nitrosodimethylamine

Aniline

1,4-Dichlorobenzene-d4

Isophorone

1,3-dimethyl-2-nitrobenzene (ss) 10

Naphthalene-d8 10

Hexachlorocyclopentadiene

Mevinphos

10

10

Amount (ng)

Chem station

AMDIS Match

AMDIS

R.T. Diff sec

6.77

10

10

10

96

99

99

96

2.0

4.7

6.1

4.4

96

100

98

95

3.7

2.3

1.2

0.6

9.4978

15067262 Acenaphthene-d10

9.5359

51285 2,4-Dinitrophenol

9.5676

100027

9.6660

121142

4-Nitrophenol

2,4-dinitrotoluene

10.0484

86737

10.0698

534521

10.1747

1582098

10.6410

122349

Fluorene

4,6-Dinitro-2-methylphenol

Trifluralin

Simazine

10

10

9.48

10

10

10

10

10

98

91

95

96

98

96

95

93

–0.1

0.1

0.3

0.1

0.0

–0.0

–0.1

0.7

10.6642

1912249

10.7841

87865

Atrazine

Pentachlorophenol

10.8089

13071799 Terbufos

10.9678

1897456 Chlorothalonil

10.9973

1517222

11.8117

309002

12.1149

1024573

12.8343

72208

Phenanthrene-d10

Aldrin

Heptachlor epoxide -isomer B

Endrin

13.1563

50293

13.5999

91941

13.6598

1719035

14.8425

205992

15.3696

1520963

4,4'-DDT

3,3'-Dichlorobenzidine

Chrysene-d12

Benzo[b]fluoranthene

Perylene-d12

10.97

10

10

10

10

10

10

10

10

10

10

10

10

96

97

95

100

96

98

97

98

93

96

98

100

98

0.3

–0.0

0.0

0.2

0.0

–0.8

–1.1

–1.7

–2.0

–2.2

–2.2

–3.8

–4.6

Figure 5 Example of S-VOA checkout mix DRS report

90

97

91

95

85

86

92

93

94

91

92

91

95

93

93

93

84

81

91

93

92

95

90

91

90

84

96

91

95

Revers

Match

NIST

Hit

Num.

1

1

1

1

1

1

1

1

1

2

1

1

1

2

1

1

1

1

1

2

1

1

1

1

1

1

2

1

1

3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide 25

2 S-VOA Analyzer Specifics

26 3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide

Agilent SP1 7890-0568 3-in-1 GC/MSD DRS Analyzer

Installation and Checkout Guide

3

VOA Analyzer Specifics

Copying and Pasting VOA Files 30

Description of VOA Files 31

Loading and Relocking the Headspace VOA Method 32

Loading the VOA Acquisition Method 34

Relocking Sequence 34

Confirming the Lock 36

DRS Analysis of the Solvents-Plus Checkout Mix 37

The VOA portion of the 3-in-1 Analyzer is based on the

SP1 7890-0567 HS VOA Analyzer.

The straight bore no taper liner, (p/n 8004-0157), has a

1.2 mm id and gives good peak shapes and sensitivity at a

20:1 split. The liner is inserted upside-down, that is with the counterbore, if present, at the top. This is not the normal position but it helps guide the megabore transfer line into the liner. The column is a 30 m × 0.25 mm × 1.0 um DB-5 MS UI column (p/n 121-5533UI). The column length above the inlet ferrule should be ~ 20 mm.

The rear inlet top weldment is replaced with the accessory

7890A S/SL MMI Weldment for Headspace, (p/n G3521A). This eliminates splicing the transfer line into the carrier line. The septum purge line exists but the carrier is fed directly from the inlet EPC module to the headspace sampler. The original weldment is included if needed.

The 7697A Headspace sampler is interfaced to the 7890 rear inlet using a length of 530 um SilTek deactivated fused silica tubing through the transfer line. At the GC inlet, the tubing is

Agilent Technologies

27

3 VOA Analyzer Specifics punctured through the septum and trimmed to a length of

~ 30 mm. The tubing is inserted into the liner, using the counterbore in the liner as a lead-in. The standard green septum nut and septum complete the seal.

The system is RT locked to Toluene-d8 at 7.790 minutes.

The VOA acquisition method, VOA_3-in-1_acq.m, contains both scan and SIM parameters. Scan only acquisition, run at a sampling rate of 2^2, is used for RT locking and checkout. The

SIM parameters are those for the 63 most commonly measured compounds from USEPA Method 524. If SIM/scan is run, the rate should be set to 2^1. With SIM/scan, the SIM signal can be used for quantitation of the most important analytes and the scan signal can be used for deconvolution and identification of all 369 compounds.

The 369 compound quant database was taken from Agilent's

G1678AA Solvents-Plus DRS DBL, supplied with this analyzer.

The retention times from the CF methodology with a CP post column splitter were used as a starting point. The retention times of the earliest and latest eluters have been slightly modified due to the Aux EPC pressure ramp. It is important to

use the methods and files listed in Table 2 on page 13, for best

system performance.

Additional information on using a headspace with the

Solvents-Plus DRS DBL can be found in the following application note: Headspace Volatiles using a

Headspace-GC/MSD Analyzer. Mike Szelewski, Agilent

Technologies, Publication 5990-7907EN, www.agilent.com/chem . A copy of this application note is included on the CD that came with this analyzer.

28 3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide

VOA Analyzer Specifics 3

Volatiles rear column view 30 m × 250 um × 1.0 um DB-5MS UI (p/n 122-5533UI)

HS volatiles run on rear column at 1.2 mL/min CF, RTL dependent

Front semi-voas column at 0.4 mL/min CF

Aux maintains 0.4 mL/min make-up

7693A

7693 Tray

Aux ramp psi

S/SL rear inlet,

20:1 split

5975C

EI MSD

Aux = 310 °C

1.2 mL/min CF

7697A

Headspace with or without

Sampler

2 mL/mjn to MSD

CP Restictor 1.1 m × 0.15 mm id

Silcotek deactivated tubing,

Agilent p/n 160-7625-5

Figure 6 Rear column view of the 3-in-1 Analyzer

3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide 29

3 VOA Analyzer Specifics

Copying and Pasting VOA Files

Copy the VOA files from the CD supplied by the Specials Group and paste them into the location listed in

Table 6

. This CD is not one of the software installation CDs.

Table 6 Copying and pasting VOA files

File name

VOA_3in1_acq.m

VOA_3in1_DA-checkout.m

VOA_3in1_DA.m

VOA_3in1_checkout.D

VOA_3in1_checkout.msl

VOA_3in1_checkout.cid

VOA_3in1.cal

VOA_3in1.csl

Onsite.ini

Default.ini

Nistms.ini

AmdisConfig.txt

Location to paste the copied file

C:\MSDchem\1\Methods

C:\MSDchem\1\Data

C:\NIST08\AMDIS32\Lib

C:\NIST08\AMDIS32\Lib

C:\NIST08\Mssearch

C:\Program Files\Agilent\MSD Deconvolution

Reporting Software

Additional file information

Verify the following files in Table 7 were installed.

Table 7 Additional VOA file information

File name

CF_SOLV.L, CP_SOLV.L

CF_SOLV.msl

CF_SOLV.cid

Location to paste the copied file

These 2 libraries should have installed into C:\

Database when the G1678AA Solvents-Plus DRS database was installed.

These 2 files should have installed into C:\

NIST08\AMDIS32\Lib when the G1678AA

Solvents-Plus DRS database was installed.

30 3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide

VOA Analyzer Specifics 3

Description of VOA Files

VOA_3in1_acq.m

–the method that has been RT locked by the

Specials Group using the installed column. This method will be relocked as part of the system installation and will be used for data acquisition of the checkout mix and customer samples in scan. This method includes the SIM ions discussed above.

VOA_3in1_DA-checkout.m

–the data analysis method that contains 20 compounds in the quantitation database, that will be used for the DRS analysis of the checkout mix.

VOA_3in1_DA.m

–the data analysis method that contains

369 compounds in the quantitation database that can be used for samples.

VOA_3in1_Checkout.D

–the datafile that was acquired by the

Specials Group as final checkout. It can be used as a reference for the checkout sample run as part of the system installation.

VOA_3in1_checkout.msl, VOA_3in1_checkout.cid,

VOA_3in1.cal, VOA_3in1.csl

–these are the AMDIS files designed for the VOA portion of the 3-in-1 Analyzer.

CF_SOLV.msl, CF_SOLV.cid

–this is the 369 compound

Solvents-Plus DRS Database-Library and associated chemical information directory file.

Onsite.ini, Default.ini, Nistms.ini, AmdisConfig.txt

–these are configuration files specific to the analyzer and should overwrite the exisiting files in the specified directories.

3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide 31

3 VOA Analyzer Specifics

Loading and Relocking the Headspace VOA Method

The GC/MSD Solvents-Plus checkout mix (p/n G3440-85012) is a solution of 20 compounds, each at 500 ppm (500 ng/µL), in n-propanol. If the checkout mix is unavailable, an alternate mix containing toluene-d8 can be used for relocking, such as Ultra

Scientific (p/n STS-310). The names and CAS numbers of the compounds in the G3440-85012 mix are listed in Table 8 on page 33 in RT order.

32 3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide

VOA Analyzer Specifics 3

Table 8 Solvents-Plus checkout mix compound list

Compound

Pentane

Allyl chloride

Allyl ether

Propyl acetate

Propylene glycol

Toluene-d8 n-Octane

2-Methylbutyl acetate

Diethyl disulfide

Phenol o-Ethyltoluene p-Isopropyltoluene (p-Cymene)

Indene

Nitrobenzene

1-Nonanol

Decanal n-Nitroso-di-n-butylamine

1,8-Octanediol

2,6-Di-tert-butyl-4-methylphenol (BHT) n-Hexadecane

9.857

11.004

11.698

12.054

12.864

13.398

14.108

15.077

RT

3.284

3.718

6.275

6.613

7.045

7.790

8.371

15.702

16.670

17.745

20.111

21.091

CAS number

109660

107051

557404

109604

57556

2037265

111659

624419

110816

108952

611143

99876

95136

98953

143088

112312

924163

629414

128370

544763

The VOA method should be RT locked to toluene-d8 at

7.790 minutes. If a toluene-d8 standard is not available, the system RT lock can be checked with chlorinated tap water.

Chloroform should elute at ~ 5.08 min, bromodichloromethane

3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide 33

3 VOA Analyzer Specifics at ~ 6.80 min, and dibromochloromethane at ~ 8.63 min. These three compounds are commonly found in chlorinated drinking water in the 1–50 ppb range.

Standards Preparation for Relocking the VOA Column

Partially fill two 20 mL headspace vials with 10 mL water.

Spike 2 uL of the Solvents-Plus checkout mix into each of the headspace vials. The resulting concentration is 100 ppb in the water. Place the vials in the first two tray positions. These will be used for relocking the previously locked method.

Loading the VOA Acquisition Method

Open the ChemStation instrument control software and click

Method > Load Method and choose the method called

VOA_3in1_acq.m.

Relocking Sequence

The process here is similar to that used for relocking the S-VOA method.

1 Set up a two line sequence using the method VOA_3in1_acq.m.

Name the datafiles VOA_3in1_Relock_1 and VOA_3in1_Relock_2.

2 Save the sequence as VOA_Relock_Seq.s and run the sequence.

3 After the sequence is completed, start the Instrument 1 Data

Analysis program.

4 Use the Method > Load Method menu item to load the same

VOA_3in1_acq.m file that was run in the sequence.

5 Load the second run from the sequence (the first run was just to clean out the column) named VOA_3in1_Relock_2.D.

34 3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide

N O T E

VOA Analyzer Specifics 3

6 Select the View > RTLock Setup menu item to open the RTLock screen. Proceed with relocking the acquisition method,

VOA_3in1_acq.m, using datafile VOA_3in1_Relock_2.D. The new inlet pressure has now been saved to the method.

The new pressure will not be applied to the method or to the GC until the method is reloaded or is run.

7 Select the View > Return to Data Analysis menu item to close the

RTLock Setup View.

8 On the GC keyboard, press the Back Inlet key to view the pressure setpoints for the inlet the method is using. In the

Data Acquisition view, re-load your method VOA_3in1_acq.m.

You should see the new calculated locking pressure downloaded as the setpoint for the inlet.

3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide 35

3 VOA Analyzer Specifics

Confirming the Lock

After relocking the method, a third run (optional) of the checkout mix can be made to verify the locking pressure and time, if the RT lock time of toleune-d8 was off by more than ± 0.010 minutes.

The best way to do this is to add a line to the existing sequence and then use the Sequence > Position and Run menu item.

4.00

6.00

8.00

10.00

12.00

14.00

Figure 7 Solvents-Plus checkout mix total ion chromatogram

16.00

18.00

20.00

22.00

When run using headspace, some compounds may have a much lower response, such as propylene glycol, phenol, or

1,8-octanediol, due to their solubility in water.

36 3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide

VOA Analyzer Specifics 3

DRS Analysis of the Solvents-Plus Checkout Mix

This step is to confirm that the retention times across the entire elution range of the chromatogram match those in the method closely enough to have all peaks fall in their recognition windows.

1 In Data Analysis using the Method > Load Method… menu item, load the method VOA_3in1_DA-checkout.m.

2 Using the File > Load Data File… menu item, load the last checkout mix relocking run that was made. Select the menu item DRS > Quant + DRS single file. After a moment, you will see activity on the computer as DRS performs a quantitative analysis, deconvolutes the mass spectra and searches the

VOA_3in1_checkout.msl AMDIS database. Depending upon the deconvolution settings chosen, the DRS process will typically take 2 to 4 minutes. At this point, DRS will generate a report that looks similar to (but not necessarily identical to)

Figure 7 on page

3 Inspect the report and compare it to the list of compounds in the sample.

Also note that the ChemStation Amount column gives only estimated amounts for the compounds that it identified.

These amounts are based on a single point response factor that is supplied with your method. You must calibrate any compounds that you wish to quantify as you do with any other GC/MS method.

The AMDIS amount column is completed after the QEdit process.

The AMDIS column of the DRS report should find all the analytes in the test mix, typically with match factors > 80 and with RT differences of < 10 seconds.

3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide 37

3 VOA Analyzer Specifics

MSD Deconvolution Report

Sample Name: 2 uL 500ppm VOA COM

Data File: C:\msdchem\1\DATA\VOA_3in1_Relock_2.D

Date/Time: 2:31:01 PM Thursday, May 26, 2011

Adjacent Peak Subtraction = 1

Resolution = Medium

Sensitivity = High

Shape Requirements = Medium

The NIST library was not searched for the components that were found in the AMDIS target library.

RT

3.2976

3.7269

6.2628

6.5954

7.7893

8.375

9.8501

10.9992

12.0524

12.8663

13.3979

14.1014

15.079

15.7087

16.670

20.1332

21.1227

Cas number Compound Name

109660

107051

557404

109604

2037265

111659

624419

110816

611143

99876

95136

98953

143088

112312

924163

128370

544763

Pentane

Allyl chloride

Allyl ether

Propyl acetate

Toluene-d8 n-Octane

2-Methylbutyl acetate

Diethyl disulfide o-Ethyltoluene p-Isopropyltoluene (p-Cymene)

Indene

Nitrobenzene

1-Nonanol

Decanal n-Hexadecane

10.17

10 n-Nitroso-di-n-butylamine 10

2,6-Di-tert-butyl-4-methylphenol (BHT) 10

10

10

10

10

10.01

10

10

10

9.46

Amount (ppb)

Chem station

AMDIS

AMDIS Match R.T. Diff sec

10

9.97

10

10

100

100

98

98

–0.0

–0.0

0.0

0.1

NIST

Reverse

Match

Hit

Num.

100

84

99

100

100

100

100

76

83

97

99

97

–0.0

0.0

0.0

–0.0

0.0

–0.0

–0.0

–0.5

0.1

–0.0

0.0

–0.2

Figure 8 Example of Solvents-Plus checkout mix DRS report

38 3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide

Agilent SP1 7890-0568 3-in-1 GC/MSD DRS Analyzer

Installation and Checkout Guide

4

Pesticides Analyzer Specifics

Copying and Pasting Pesticides Files 41

Description of Pesticides Files 42

Loading and Relocking the Pesticides Method 43

RT Locking the Method 45

Relocking Sequence 45

Confirming the Lock 47

DRS Analysis of the Pesticides Checkout Mix 48

The pesticide portion of the 3-in-1 Analyzer uses the S-VOA hardware and column with method modifications, see

Figure 2 on page 16. The pesticides method is not RT locked by the

Specials Group, and should be done on site by the user after the

S-VOA Analyzer section is completed.

The single-taper with glass wool liner, (p/n 5190-2293), introduced in early 2011, is UI deactivated and is used for HSL.

CSL injections can be done using a 2 mm dimple liner

(p/n 5190-2296) and conditions in Application Note 5989-7875.

The 3-in-1 Analyzer uses a 20 m × 0.18 mm × 0.36 um DB-8270D column (p/n 121-9723) which is a more inert version of

DB 5-MS. The Pesticide Analyzer should be RT locked to lindane at 9.100 minutes.

The pesticides acquisition method, Pest_3in1_acq_bf.m, is scan only and can be run at a sampling rate of 2^2 or 2^1. Users may want to run SIM for some compounds, and if SIM/scan is run, the rate should be set to 2^1. With SIM/scan, the SIM signal can be used for quantitation of the most important analytes and the scan signal can be used for deconvolution and identification of the remaining pesticides.

Agilent Technologies 39

4 Pesticides Analyzer Specifics

The 927 compound quant database was taken from Agilent's

G1672AA pesticides DRS DBL, but has been modified.

The original pesticides DRS DBL was built using a

30 m × 250 um × 0.25 um column running in constant pressure mode. The 3-in-1 Analyzer pesticides column is a

20 m × 180 um × 0.36 um column running in constant flow mode.

The original 927 pesticides DBL was mapped to the

3-in-1 Analyzer column running in CF mode. More than

50 index peaks were used with a 6th order curve fit to translate the RTs. All of the 927 pesticides were not rerun on the

3-in-1 Analyzer column. The translated RTs should be

± 0.10 minutes from actual, with some outliers, as shown in

Figure 9 on page 47. Because all of the RTs are not precise, this

modified pesticides database will be provided at no charge, only as part of the 3-in-1 Environmental Analyzer.

For best system performance, it is important to use the methods

and files listed in Table 2 on page 13.

40 3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide

Pesticides Analyzer Specifics 4

Copying and Pasting Pesticides Files

Copy the pestidides files from the CD supplied by the Specials

Group and paste them into the location listed in

Table 9 . This

CD is not one of the software installation CDs.

Table 9 Copying-pasting pesticides files

File name

Pest_3in1_acq_BF.m

Pest_3in1_DA-checkout.m

Pest_3in1_DA.m

Pest_3in1_checkout.D

Pest_3in1_checkout.msl

Pest_3in1_checkout.cid

Pest_3in1.cal

Pest_3in1.csl

RTLPest3.msl

RTLpest3.cid

Onsite.ini

Default.ini

Nistms.ini

AmdisConfig.txt

RTLPest3.L

Location to paste the copied file

C:\MSDchem\1\Methods

C:\MSDchem\1\Data

C:\NIST08\AMDIS32\Lib

C:\NIST08\AMDIS32\Lib

C:\NIST08\Mssearch

C:\Program Files\Agilent\MSD Deconvolution

Reporting Software

C:\Database

3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide 41

4 Pesticides Analyzer Specifics

Description of Pesticides Files

Pest_3in1_acq_BF.m– the method has not been RT locked by the

Specials Group. This method should be RT locked by the user for data acquisition of the checkout mix and samples. On loading the method, Method Resolution will be required.

Pest_3in1_DA-checkout.m

–the data analysis method that contains 20 compounds in the quantitation database, and will be used for the DRS analysis of the checkout mix.

Pest_3in1_DA.m

–the data analysis method that contains

927 compounds in the quantitation database that can be used for samples. The RTs have been translated as described earlier and can be updated by users, if needed, after running standards.

Pest_3in1_Checkout.D

–an example datafile that can be used as a reference for the checkout sample run.

Pest_3in1_checkout.msl, Pest_3in1_checkout.cid,

Pest_3in1.cal, Pest_3in1.csl

–these are the AMDIS files designed for the pesticides portion of the 3-in-1 Analyzer.

RTLPest.msl, RTLPest3.cid

–this is the 927 compound pesticides DRS Database-Library and associated directory file, provided at no charge. The G1672AA pesticides DBL product should not be purchased nor installed.

Nistms.ini, AmdisConfig.txt, Default.ini

–these are configuration files specific to the Analyzer and should overwrite the exisiting files in the specified directories.

Onsite.ini

–this is an AMDIS configuration file specific to the

Analyzer and should overwrite the exisiting file in the specified directory. When running Pesticides, the RI Window in AMDIS should be changed to 45. This can be found under the Analyze >

Settings… Identification tab in AMDIS.

42 3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide

Pesticides Analyzer Specifics 4

Loading and Relocking the Pesticides Method

The GC/MSD pesticides checkout mix (p/n 5190-0468) is a solution of 20 compounds, each at 10 ppm (10 ng/µL), in acetone. The names and CAS numbers of the compounds in the mix are listed in

Table 10 in RT order.

Table 10 Pesticides checkout mix compound list

Compounds

Dichlorvos

Mevinphos

Ethalfluralin

Trifluralin

Atrazine

Lindane

Chlorpyrifos methyl

Heptachlor

Malathion

Chlorpyrifos p,p'-DDE

Dieldrin

Hexazinone

Propargite

Leptophos

Fenarimol

Mirex

Coumaphos

Ethofenprox

Deltamethrin

10.448

10.706

10.890

12.838

13.059

14.406

14.564

15.896

16.444

16.483

17.107

18.146

19.793

RT

4.892

6.006

7.750

7.862

8.786

9.100

10.055

76448

121755

2921882

72559

60571

51235042

2312358

21609905

CAS number

62737

7786347

55283686

1582098

1912249

58899

5598130

60168889

2385855

56724

80844071

52918635

3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide 43

4 Pesticides Analyzer Specifics

Open one of the vials of the pesticides checkout mix and transfer it to an autosampler vial. Place the autosampler vial in tray position one. This will be used for RT locking the method.

The method, PEST_3in1_acq_BF.m, should be RTLocked to Lindane

at 9.100 minutes.

44 3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide

Pesticides Analyzer Specifics 4

RT Locking the Method

The method, PEST_3in1_acq_BF.m, should be RT locked in Data

Acquisition. The procedure for this is found in the MSD

Chemstation Help, by Searching rtlocking and then select To lock

an MS method. An outline of the steps is as follows:

1 Load the acqusition method, PEST_3in1_acq_BF.m, in the Data

Acqusition View and Resolve if necessary.

2 Place a vial of the pesticides checkout mix in position one of the autosampler.

3 Acquire the initial 5 RT locking runs.

4 A new Data Analysis session will start after completion of the 5 runs.

5 Select the peak for locking. Lindane should elute close to

9 minutes.

6 Complete the remaining dialogue box inputs.

7 Reload the method in Data Acquisition.

Relocking Sequence

The process here is similar to that used for relocking the S-VOA method.

1 Set up a two-line sequence using the method

PEST_3in1_acq_BF.m. Name the datafiles PEST_3in1_Relock_1 and PEST_3in1_Relock_2.

2 Save the sequence as PEST_Relock_Seq.s and run the sequence.

3 After the sequence is completed, start the Instrument 1 Data

Analysis program.

4 Use the Method > Load Method menu item to load the same

PEST_3in1_acq_BF.m file that was run in the sequence.

5 Load the second run from the sequence (the first run was just to clean out the column) named PEST_3in1_Relock_2.D.

3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide 45

4 Pesticides Analyzer Specifics

N O T E

6 Select the View > RTLock Setup menu item to open the RTLock screen.

7 Proceed with relocking the acquisition method,

PEST_3in1_acq_BF.m, using datafile PEST_3in1_Relock_2.D. The new inlet pressure has now been saved to the method.

[

The new pressure will not be applied to the method until the method is reloaded or is run.

8 Select the View > Return to Data Analysis menu item to close the

RTLock Setup View.

9 On the GC keyboard, press the Front Inlet key to view the pressure setpoints for the inlet the method is using.

10 In the Data Acquisition view, re-load your method

PEST_3in1_acq_BF.m.

You should see the new calculated locking pressure downloaded as the setpoint for the inlet.

46 3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide

Pesticides Analyzer Specifics 4

Confirming the Lock

After relocking the method, a third run (optional) of the checkout mix can be made to verify the locking pressure and time, if the RT lock time of lindane was off by more than

± 0.010 minutes from the expected 9.100 minutes.

The best way to do this is to add a line to the existing sequence and then use the Sequence > Position and Run menu item.

Figure 9 Pesticides checkout mix total ion chromatogram

3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide 47

4 Pesticides Analyzer Specifics

DRS Analysis of the Pesticides Checkout Mix

This step is to confirm that the retention times across the entire elution range of the chromatogram match those in the method closely enough to have all peaks fall in their recognition windows.

1 In Data Analysis, using the Method > Load Method… menu item, load the method Pest_3in1_DA-checkout.m.

2 Using the File > Load Data File… menu item, load the last checkout mix relocking run that was made. Select the menu item DRS > Quant + DRS single file. After a moment, you will see activity on the computer as DRS performs a quantitative analysis, deconvolutes the mass spectra and searches the

Pest_3in1_checkout.msl AMDIS database, then searches the

NIST08 library. Depending upon the deconvolution settings chosen, the DRS process will typically take 2–4 minutes. At this point, DRS will generate a report that looks similar to

(but not necessarily identical to) Figure 49.

3 The DRS Report for the pesticides checkout mix shows two compounds, dieldrin and mirex, with RT differences of > 30 sec with respect to the AMDIS database RTLPest3.msl.

Differences such as these can be expected for a subset of the database due to the translation that was described earlier.

The GC/MSD Chemstation quantitation database (qdb.mth) time were translated using the index compounds. The expected RTs in the RTLPest3.msl were not changed from the original values. Instead a modified RT calibration file,

Pest_3in1.cal is used to translate the retention times.

Also note that the ChemStation Amount column gives only estimated amounts for the compounds that it identified.

These amounts are based on a single point response factor that is supplied with your method. You must calibrate any compounds that you wish to quantify as you do with any other GC/MS method.

The AMDIS Amount column is completed after the QEdit process.

48 3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide

Pesticides Analyzer Specifics 4

MSD Deconvolution Report

Sample Name: Pesticides Checkout

Data File: C:\msdchem\1\DATA\Pest_3in1_checkout.D

Date/Time: 9:31:29 AM Tuesday, June 07, 2011

Adjacent Peak Subtraction = 1

Resolution = Medium

Sensitivity = High

Shape Requirements = Medium

The NIST library was searched for the components that were found in the AMDIS target library.

RT Cas number Compound Name

4.8939

62737

6.0058

7786347

Dichlorvos

Mevinphos

7.752

55283686 Ethalfluralin

7.8602

1582098 Trifluralin

8.7850

1912249

9.1017

58899

10.0547

5598130

10.4477

76448

Atrazine

Lindane

Chlorpyrifos Methyl

Heptachlor

10.7060

121755

10.8886

2921882

12.8357

72559

13.058

60571

Malathion

Chlorpyrifos p,p'-DDE

Dieldrin

14.407

51235042 Hexazinone

14.532

2312358 Propargite

15.8956

21609905 Leptophos

16.447

60168889 Fenarimol

16.486

2385855

17.1035

56724

Mirex

Coumaphos

18.1467

80844071 Ethofenprox

19.7897

52918635 Deltamethrin

10

10

10

10

10

10

10

10

10

10

10

10

Chem station

10

10

10

10

10

10

10

10

Figure 10 Example of pesticides checkout mix DRS report

AMDIS Match

99

100

AMDIS

R.T. Diff sec.

0.0

–0.0

99

98

98

99

0.1

–0.0

–0.0

–0.0

99

100

99

100

100

99

99

84

–0.0

0.0

0.0

–0.1

–0.0

37.7

0.3

0.0

100

90

98

99

95

86

–0.0

0.4

38.9

–0.1

–0.0

0.5

94

94

93

92

88

86

78

88

93

93

96

96

93

94

90

95

NIST

Reverse

Match

Hit

Num.

94

91

95

93

1

2

1

1

1

2

1

1

1

1

1

1

1

1

1

1

1

1

1

1

3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide 49

4 Pesticides Analyzer Specifics

50 3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide

Agilent SP1 7890-0568 3-in-1 GC/MSD DRS Analyzer

Installation and Checkout Guide

5

Allowed 3-in-1 System Configurations

GC

Oven

Front inlet

7890A

120V or 240V

S/SL or MMI for S-VOA–checkout is hot splitless

S/SL for VOAs Rear inlet

Splitter

Aux EPC

Aux Temp

Headspace

Software

Purged 2-way acting as a column effluent combiner

3 channel

MSD aux heater option

Autosampler

MSD

Pump type

7693 with tray is recommended, but an

Injector only is allowed

Inlet weldment Rear inlet top weldment replaced with

G3521A for interfacing the headspace sampler

5975C

Either a turbo or a diffusion pump is allowed, however, Agilent strongly recommends the turbo pump

7697A with 111 sample capacity is recommended, but the 12 position headspace is allowed

GC/MSD Chemstation

NIST08

DRS base product G1716AA

S-VOA DRS DBL G1677AA

Solvents-Plus DRS DBL G1678AA

Agilent Technologies 51

5 Allowed 3-in-1 System Configurations

Pesticides DRS DBL included on the Specials CD at no charge.

Do not order.

52 3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide

Agilent SP1 7890-0568 3-in-1 GC/MSD DRS Analyzer

Installation and Checkout Guide

6

Consumables and Supplies

Below is a list of consumables and parts that are used with the

Agilent 3-in-1 Analyzer.

Table 11 Agilent 3-in-1 Analyzer consumables and parts

3-in-1 Columns and column accessories

S-VOA-Pesticide Column,

Agilent J&W DB-8270D GC Column,

20 m × 0.18 mm × 0.36 um

VOA Column,

Agilent J&W DB-5 MSUI GC Column,

30 m × 0.25 mm × 1.0 um

Restrictor tubing, 0.15 mm SilTek deactivated,

5 m 1.1 m × 0.15 mm used in oven from 2-way splitter to

MSD transfer line

Column ferrule, MMI, graphite (10/pk), for inlets

Column nut, GC capillary (2/pkg), for inlets

MSD Transfer line ferrule,

0.4 mm graphite/vespel, long 10pk

Column nut for MSD tranfer line when using p/n 5062-3508

Restrictor tubing, 0.53 mm SilTek deactivated,

5 m for headspace

Part number

121-9723

121-5533UI

160-7625-5

5080-8853

5181-8830

5062-3508

05988-20066

Restek p/n

10028

Agilent Technologies 53

6 Consumables and Supplies

Table 11 Agilent 3-in-1 Analyzer consumables and parts (continued)

GC inlet and instrument supplies

S-VOA Inlet liner, MMI or S/SL,

4 mm id with UI deactivated wool

S-VOA Inlet liner, MMI, cold splitless only, 2 mm id

VOA inlet liner, 1.2 mm straight for interfacing headspace 5pk

Septum, advanced green (50/pkg)

O-ring, inlet liner non-stick (10/pkg)

ALS syringe, 10 µL tapered fixed needle, PTFE-tipped plunger,

6pk

ALS syringe, 10 µL tapered fixed needle, PTFE-tipped plunger

Capillary flow parts

Internal nut for capillary flow devices

SilTite ferrule for 0.25 mm and smaller columns (10/pkg)

2-Way purged splitter, plate only

Bleed line, 0.0625 in OD × 0.010 in id × 100 cm,

316SS tubing

1/16 in Brass Swagelok tee

Bleed tee ferrule, 1/16 in Vespel (10/pkg)

Useful tools

MSD column installation tool

Ferrule pre-swage tool for capillary flow devices

Chemical standards

S-VOA Locking-Checkout Standard,

3 ampoules, 1 mL

Pesticides Locking-Checkout Standard,

3 ampoules, 1 mL

VOA (Solvent+) Locking-Checkout Standard

Part number

5190-2293

5190-2296

8004-0157

5183-4759

5188-5365

G4513-80208

G4513-80200

G2855-20530

5188-5361

G3180-61500

0100-2354

0100-0680

0100-1329

G1099-20030

G2855-60200

5190-0473

5190-0468

G3440-85012

54 3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide

Consumables and Supplies 6

Table 11 Agilent 3-in-1 Analyzer consumables and parts (continued)

CDs

DRS video CD “DRS Familiarization Videos”

CD disk (Installation guide, Methods, Autotune file, AMDIS settings, configured DRS methods, checkout datafiles and DRS report)

5973-1731 not a replaceable part

3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide 55

6 Consumables and Supplies

56 3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide

Agilent Technologies

© Agilent Technologies, Inc.

Printed in USA, November 2011

*7890-0568*

7890-0568

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