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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
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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
2-way Purged Splitter Plumbing and Operation Specifics
Backflushing Parameters
Software
2 S-VOA Analyzer Specifics
Copying and Pasting S-VOA Files
Description of VOA Files
18
Loading and Relocking the S-VOA Method
Loading the Acquisition Method
20
Making the Relocking Runs
Relocking Sequence
Confirming the Lock
DRS Analysis of the S-VOA Checkout Mix
3 VOA Analyzer Specifics
Copying and Pasting VOA Files
Description of VOA Files
31
Loading and Relocking the Headspace VOA Method
Standards Preparation for Relocking the VOA Column
Loading the VOA Acquisition Method
3-in-1 GC/MSD DRS Analyzer Installation and Checkout Guide 3
Relocking Sequence
Confirming the Lock
DRS Analysis of the Solvents-Plus Checkout Mix
37
4 Pesticides Analyzer Specifics
Copying and Pasting Pesticides Files
41
Description of Pesticides Files
Loading and Relocking the Pesticides Method
RT Locking the Method
Relocking Sequence
Confirming the Lock
DRS Analysis of the Pesticides Checkout Mix
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
2-way Purged Splitter Plumbing and Operation Specifics 11
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
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
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
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.
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
Loading and Relocking the S-VOA Method 19
Loading the Acquisition Method 20
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.
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
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 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
Loading and Relocking the Headspace VOA Method 32
Loading the VOA Acquisition Method 34
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
. 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)
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
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
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 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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