The Tool Box – Getting More Productivity from Your GC and GC/MSD
Transcript of The Tool Box – Getting More Productivity from Your GC and GC/MSD
Productivity Tool Box for GC & GC/MSOverview 5975C MSDAgilent RestrictedPage 2
The Tool Box – Getting More Productivity from Your GC and GC/MSD
M RameshApplication Engg – GC/GCMSAgilent Technologies India Pvt. Ltd.
Productivity Tool Box for GC & GC/MS
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Defining Productivity
• More analyses per unit time . . . – Faster and more efficient separations
– Shorter analysis cycle time (time from injection to injection)
– Reduced requirement for sample preparation
• with consistently better results . . . – Quantitative: accuracy, precision, detection limits, linear range
– Qualitative: response ratios, confirmatory retention times, library searches (eliminate false negatives and false positives)
• while using less operator time for each analysis.– Less time performing maintenance
– Extensive computer control and data processing
– Simplified operator review/approval
Productivity Tool Box for GC & GC/MS
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Productivity: the Sum of Many Technologies
• Low Thermal Mass GC
• Capillary Flow Technology - Backflush
• Hydrogen carrier gas for GC and GC/MS
• Retention Time Locking (RTL) Editor (& Methods)– With more RTL Databases
• Trace Ion Detection
• Fast Electronic - Synchronous SIM/Scan
• Method Translator
• High signal-to-noise Triple-Axis Detector– Gain Normalization of the EM
– EM Saver
• 2nd Generation Deconvolution Reporting Software (DRS)
Return home(this slide)
Nextslide
Return tosection menu
Productivity Tool Box for GC & GC/MS
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Productivity: Low Thermal Mass GC
• More analyses per unit time . . . – Faster and better separations– Shorter analysis cycle time (time from injection to injection)– Reduced requirement for sample preparation
• with consistently better results . . . – Quantitative: accuracy, precision, detection limits, linear range
– Qualitative: response ratios, confirmatory retention times, library searches (eliminate false negatives and false positives)
• while using less operator time for each analysis.– Less time performing maintenance
– Extensive computer control and data processing
– Simplified operator review/approval
Productivity Tool Box for GC & GC/MS
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“LTM” (L ow Thermal M ass) Technology
•Direct heating of fused silica GC columns
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LTM Cooldown Times (Standard Size)
0
50
100
150
200
250
300
350
400
0 50 100 150 200 250
Time (sec)
Tem
p (o
C) 2m LTM
5m LTM
10m LTM
7890 GC
Additional Cooldown times available on website for LTM column modules up to 30m
Rapid Cooldown
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Low Thermal Mass Technology for 7890/6890 GC
Satisfies the need for high through-put, especially for low margin samples, where analytical cycle times are a critical element in making a profit
Independent and simultaneous temperature programming of:1-2 column modules (fastest cooldown), or 1-4 column modules (small format)
Note: Front thermal shield removed to show LTM column modulesEntire thermal shield should always be in place during operation
LTM Column Modules(standard width shown)
LTM Control System w/ Keypad User Interface… Agilent LTM Control SW now available
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LTM Also Greatly Reduces Cool-Down Times,� 9x Faster Heating/Cooling Cycle Times
40 min + 5.4 min
20 min + 5.4 min
3 min + 2 min
GC Run Time Cool Down
LTM/78909x Faster Cycle Time(200oC/min)
Productivity Tool Box for GC & GC/MS
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Obtaining Faster GC, GC/MS Analytical Cycle Times – A Variety of Approaches to Fit Your Lab and Your N eeds
Post-RunBake-Out
ChromatographicRun
Post-RunCool-Down
Pre-RunALS Set-Up
Included “ALS Sample Overlap” 7890 GCin in ChemStation SW Faster Cool-down
HW/SW
Faster GC Column Selection,Analyses Method Translation
GC Add-Ons Capillary Flow TechnologySignficantly Faster GC (Backflush)Analytical Cycle Times
LTM Technology LTM Technology(Rapid Heating) (Rapid Cooling )
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6.00 8.00 10.00 12.00 14.00 16.00 18.00 20.00 22.00Time-->
3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00Time-->
Reference method – Standard Oven30 m x 0.25 mm ID x 0.25 µm DB-5MS
Fast Analysis - LTM20 m x 0.18 mm ID x 0.18 µm DB-5MS
PAH by LTM/GC/MS
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Column contamination from just one prior run
5.00 5.20 5.40 5.60 5.80 6.00 6.20 6.40 6.60 6.80Time (min)
Contamination free when using backflush
PAH by LTM/GC/MS
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LTM Productivity
• High efficiency temperature programming– Fast cooling
– High throughput
– Fast method development
• High performance chromatography– Utilize commercially available columns (typically < 30 m)
• Easily integrates with conventional GC instruments– Utilize existing injectors, detectors, software
• Multicolumn temperature control
– Independent optimization
– Multidimensional GC
– High throughput parallel systems
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Hydrocarbon Processing Industry (HPI)•HPIShorter analytical cycle times get data back to operations faster, or allow more samples/shift (eg. Simulated Distillation) •Key Sales Tools5990-3174EN Fast Hydrocarbon & Sulfur Simulated Distillation Using the
Agilent Low Thermal Mass (LTM) System on the 7890A GCand 355 Sulfur Chemiluminescence Detector(Wang,Firor,Tripp - Fast Simdist (< 3 mins), 6x faster than conventional Simdist- Dual channel, simultaneous SimDist for hydrocarb’s & sulfur
•Article Multidimensional Gas Chromatography with Capillary Flow(Fall’08) Technology and LTM-GC
J Luong (et. al) Dow Chemical, R Mustacich (RVM)Published:Journal of Separation Science, ISSN 0021-9665,Volume 31, pp. 3385-3394 http://www3.interscience.wiley.com/journal/121406899/abstract- HPI examples 2D LTM/CFT/GC using Deans Switch andLTM’s simultaneous/independent temperature programmingof multiple LTM column modules
•
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Environmental/Food Safety/Forensics
•Need for high through-put, especially for low margin samples, where analytical cycle times are a critical element in making a profit
•Key Sales Tools5990-3201EN Ultra-Fast Total Petroleum Hydrocarbons (TPH) Analysis with
Agilent Low Thermal Mass (LTM) GC and Simultaneous Dual-Tower Injection (Wei & Szelewski)- 9x faster TPH throughput using LTM- 18x faster TPH using LTM and dual simultaneous injection
•Pub No. TBA Polyaromatic Hydrocarbons (PAH) by LTM/GC/MS(~end Jan’09) - 2x faster PAH runs using LTM, even faster with Backflush
- Enviro and Food Safety samples can be dirty. LTM columns cannot be trimmed (not Agilent, not Thermo…)
- LTM uses guard columns…and now Backflush/CFTbackflush delivers multiple benefits for LTM analyses including. reduced potential for carryover, longer column life, shorter analysistime
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Food/Flavor/Fragrance and Pharmaceutical
•Chiral Separations• Chiral GC is most effective at low temperatures, yet complex samples usually require a broad temperature program to separate target compounds from background and to elute highly retained sample components.• LTM/GC/MS uses a traditional column in the GC oven to separate target compounds, then heart-cut of target compounds to a chiral column in LTM module at a lower temp. � optimal chiral separations are achieved while decreasing analysis cycle times and increasing chiral column lifetime.
Pub No. TBA Chiral Separations by LTM/GC/MS(~end Jan’09) - 2D LTM/GC/MS, simultaneous/independent temperature
programming of GC and LTM column module(s)
Article Multidimensional Gas Chromatography with Capillary Flow(Fall’08) Technology and LTM-GC, J Luong (et. al) Dow Chemical,R Mustacich
Published:Journal of Separation Science, ISSN 0021-9665,Volume 31, pp. 3385-3394253-261- Examples 2D LTM/CFT/GC using Deans Switch andLTM’s simultaneous/independent temperature programmingof multiple LTM column modules
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Productivity: CFT Backflush
• More analyses per unit time . . . – Faster and more efficient separations
– Shorter analysis cycle time (time from injection to injection) – Reduced requirement for sample preparation
• with consistently better results . . . – Quantitative: accuracy, precision, detection limits , linear range
– Qualitative: response ratios, confirmatory retention times, libr ary searches (eliminate false negatives and false posit ives)
• while using less operator time for each analysis.– Less time performing maintenance– Extensive computer control and data processing
– Simplified operator review/approval
Productivity Tool Box for GC & GC/MS
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Backflush – Complete Column
1 psi
45 psi
During GC Run
After GC Run
S/S Inlet
QuickSwap or 3-way SplitterColumn
25 psi
4 psi
MSD
Aux EPCSplit Vent Trap
S/S Inlet
QuickSwap or 3-way SplitterColumn
MSD
Aux EPCSplit Vent Trap
performance turbo recommended
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Backflush – Mid-Column (Analysis Mode)
Vent
Pressure / Flow
Controller
15-m HP-5ms (0.25mm id x0.25um)
15-m HP-5ms (0.25mm id x0.25um)
Capillary Flow Technology Device
5975C MSDEI mode
7890A GC
Split/Splitless Injection Port
Y ml/min
Y+Z ml/min
Z ml/min
Z mL/min very low flow; set against column backpressure, not short restrictor as with QuickSwap
Column 1 and 2 could be different phases and different dimensionsPCT available Oct’08
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Backflush – Mid-Column (Backflush Mode)
Vent
Pressure / Flow
Controller
15-m HP-5ms (0.25mm id x0.25um)
15-m HP-5ms (0.25mm id x0.25um)
5975C MSDEI mode
7890A GC
Split/Splitless Injection Port
Decrease inlet pressure during backflush
Pressure Controlled Tee
Productivity Tool Box for GC & GC/MS
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Backflush – Mid-Column (Backflush Mode)
Vent
Pressure / Flow
Controller
15-m HP-5ms (0.25mm id x0.25um)
15-m HP-5ms (0.25mm id x0.25um)
5975C MSDEI mode
7890A GC
Split/Splitless Injection Port
Pressure Controlled Tee
Decrease inlet pressure during backflush
Purged UltimateUnion From 1st
column
To 2nd
Column & MSD
From P control
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9.00 9.50 10.00 10.50 11.00 11.50 12.00
9.00 9.50 10.00 10.50 11.00 11.50 12.00
9.00 9.50 10.00 10.50 11.00 11.50 12.00
a b
Backflush – Mid-Column (Timing Considerations)
a = begin backflush (last peak exits column 1)
b = increase flow 4 mL/min
Sample - no backflush
Sample - with backflush
Solvent blank - no backflush
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Comparison of Backflush Configurations
T=300°C; head pressure =0.5psi
4x faster & lower flow!
* smallest restrictor => best QS case
Backflush (BF) Pressure (psi)
BF flow (mL/min)
1 column vol (min)
MDS flow (mL/min)
BF flow (mL/min)
1 column vol (min)
MSD flow (mL/min)
10.0 0.3 3.82 1.5 0.6 0.94 0.9 4.120.0 0.7 1.89 2.9 1.5 0.47 1.8 4.030.0 1.3 1.28 4.8 2.6 0.32 3.0 4.040.0 2.1 0.98 7.2 4.1 0.25 4.5 3.9
PCT time savings
(N x)
QuickSwap (QS) Pressure Controlled Tee (PCT)30 m column; restrictor (0.092mm*) Two 15 m columns
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Backflush Impact on Data Quality
– Late eluters are more than just a timing problem • Bake-out may push the limits of phase stability
• Matrix may not bake out well even at the upper limit of the column
– For ‘high boiling’ matrices, backflush offers:• Improved retention time precision
• Improved spectra quality
• Consistent detector response
• Increased column lifetime
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GC/MS Industry Standard: Low Bleed Stationary Phase sLow bleed means less background (and background ion s)
DB-35ms
8.00 10.00 12.00 14.00 16.00 18.00 20.00
320°C
DB-35
8.00 10.00 12.00 14.00 16.00 18.00 20.00
300°C
CLP Pesticides Analysis
S/N =10
DB-35ms, 320°C
S/N =3
DB-35, 300°C
51
78 96119
144
207
197
214
250
253
286
315
346
356 377
405
428
455470
498
m/z-->50 100 150 200 250 300 350 400 450 500
0
Primary IonDB-35ms
51
78 96119
144
207
197
214
250
253
286
315
346
356 377
405
428
455470
498
m/z-->50 100 150 200 250 300 350 400 450 500
m/z-->50 100 150 200 250 300 350 400 450 500
0
Primary IonDB-35ms
52
78
96 119
135156
197
207
249
253
281
315331
356
377
405
428
451
470
498
m/z-->50 100 150 200 250 300 350 400 450 500
0
Primary Ion
DB-35
52
78
96 119
135156
197
207
249
253
281
315331
356
377
405
428
451
470
498
m/z-->50 100 150 200 250 300 350 400 450 500
m/z-->50 100 150 200 250 300 350 400 450 500
0
Primary Ion
DB-35
Low bleed column
Standard column
Better detection limits
Better spectra
Column bleed = chemical noise
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Typical GC/MS Separation Sequence
• Injection• Filament ON after the solvent peak• Separation and detection of the analytes• Filament OFF after the last analyte peak and before bake-out
– In an effort to ‘save’ the electron multiplier (EM), the operator is ‘blind’ to the success of bakeout
– Bake-out may NOT be adequate for all samples
This means the typical method will always have a potential for matrix carryover that
the user does not expect.
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Without Backflush: A Serious Problem
Abundance
4.00 6.00 8.00 10.00 12.00 14.00 16.00 18.00 20.000
2000000400000060000008000000
1e+071.2e+071.4e+071.6e+071.8e+07
2e+072.2e+072.4e+072.6e+072.8e+07
3e+073.2e+073.4e+073.6e+073.8e+07
4e+074.2e+074.4e+074.6e+07
Time
A: TIC: lettuce_blank.D\data.ms
B: TIC: lettuce_blank3.D\data.ms
B
A
Overlay of two chromatograms of a blank extract inj ected BEFORE (A) and AFTER (B) three injections wit hout backflush
Data provided by MSD user in Almeria, Spain
After only 3 samples , the background is significantly higher (increase chemical noise is every spectrum)
Productivity Tool Box for GC & GC/MS
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Without Backflush: Changes in Retention Time
Overlay of two chromatograms of a blank extract inj ected BEFORE (A) and AFTER (B) three injections wit hout backflush
Abundance
4.00 6.00 8.00 10.00 12.00 14.00 16.00 18.00 20.000
2000000400000060000008000000
1e+071.2e+071.4e+071.6e+071.8e+07
2e+072.2e+072.4e+072.6e+072.8e+07
3e+073.2e+073.4e+073.6e+073.8e+07
4e+074.2e+074.4e+074.6e+07
Time
A: TIC: lettuce_blank.D\data.ms
B: TIC: lettuce_blank3.D\data.ms
B
A
Data provided by MSD user in Almeria, Spain
Highly retained matrix is altering the column selectivity and changing the retention time
After only 3 samples
Productivity Tool Box for GC & GC/MS
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Without Backflush: Increased Background
Abundance
4.00 6.00 8.00 10.00 12.00 14.00 16.00 18.00 20.000
2000000400000060000008000000
1e+071.2e+071.4e+071.6e+071.8e+07
2e+072.2e+072.4e+072.6e+072.8e+07
3e+073.2e+073.4e+073.6e+073.8e+07
4e+074.2e+074.4e+074.6e+07
Time
A: TIC: lettuce_blank.D\data.ms
B: TIC: lettuce_blank3.D\data.ms
B
A
Overlay of two chromatograms of a blank extract inj ected BEFORE (A) and AFTER (B) three injections wit hout backflush
Data provided by MSD user in Almeria, Spain
Increased background due to carryover of concentrated matrix
After only 3 samples
Sample matrix = chemical noise
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With Backflush: Consistent Retention Times and Baselines (No Increase in Spectral Noise)
Stable retention times and baseline . . . less chemical noise
4.00 6.00 8.00 10.00 12.00 14.00 16.00 18.00 20.000
2000000400000060000008000000
1e+071.2e+071.4e+071.6e+071.8e+07
2e+072.2e+072.4e+072.6e+072.8e+07
3e+073.2e+073.4e+073.6e+073.8e+07
4e+074.2e+074.4e+074.6e+07
Time
Abundance
TIC: lettuce_10_ppb.D\data.ms
TIC: lettuce_100_ppb.D\data.ms
TIC: lettuce_5_ppb.D\data.ms
Overlay of three chromatograms of lettuce extract r un with 2 min of back flush
Data provided by user in Almeria, Spain
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What Real Value Does High Performance EPC Have If Matrix Carryover Destroys Rt Precision?
m in5 .3 5 .4 5 .5 5 .6 5 .7 5 .8 5 .9 6 6 . 1
N or m .
0
2 0 0 0
4 0 0 0
6 0 0 0
8 0 0 0
1 0 0 0 0
1 2 0 0 0
1 4 0 0 0
1 6 0 0 0
m in5 .3 5 .4 5 .5 5 . 6 5 .7 5 .8 5 .9 6 6 .1 6 .2
N or m .
2 0 0 0
4 0 0 0
6 0 0 0
8 0 0 0
1 0 0 0 0
1 2 0 0 0
1 4 0 0 0
10 Runs with Backflushing
10 Runs without BackflushingRetention times shift ~4-5 secduring 10 runs
Fish oil analysis
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Backflush with Purged Ultimate Union: Lipid Peroxidation Products in Blood
App Note 5989-9359EN
4-hydroxy-2,3-nonenal (HNE), an indicator of oxidative stress, and its metabolite, 1,4-dihydroxynonene (DHN)
PCI with NH 3
Late eluting peaks were quickly contaminating the source
Productivity Tool Box for GC & GC/MS
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Backflush with Purged Ultimate Union: Loss of Response without Backflush
without backflush
with backflush
These were the first backflush results; the system is getting clearer
App Note 5989-9359EN
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Productivity Benefits of Backflush
• More samples per day per instrument
• Longer column life
• Lower operating costs
• Less frequent and faster GC & MSD maintenance
• Less chemical background– More consistent retention times
– More consistent baselines
– Higher quality spectra (no increase in noise during analysis sequence)
– Higher quality quantitation (no increase in interfering ions during analysis sequence)
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References for Backflush
• 5989-9359EN Capillary Flow Technology for GC/MS: Efficacy of the Simple Tee Configuration for Robust Analysis Using Rapid Backflushing for Matrix Elimination (Prest, Foucault, and Aubut, Aug 08)
• 5989-9341EN Screening for 430 Pesticide Residues in Traditional Chinese Medicine Using GC/MS: From Sample Preparation to Report Generation in One Hour (Luan, Xu, Sept08)
• 5989-8664EN Capillary Flow Technology for GC/MS: a Simple Tee Configuration for Analysis at trace Concentrations with Rapid Backflushing for Matrix Elimination (June 08, Prest)
• 5989-8588EN The Use of Automated Backflush on the 7890A/5975C GC-MS System• 5989-8582EN Improved Forensic Toxicology Screening Using A GC/MS/NPD System with a 725-Compound DRS Database (Quimby, May08)• 5989-7670EN, Replacing Multiple 50-Minute FPD/ELCD/SIM Analyses with One 15-Minute Full-Scan Analysis for 10x Productivity Gain (Meng/Szelewski, Nov07)
Productivity Tool Box for GC & GC/MS
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References for Backflush
• 5989-6460EN Analysis of Suspected Flavor and Fragrance Allergens in Cosmetics Using the 7890A GC and Capillary Column Backflush (March 2007)• 5989-6095EN Direct Injection of Fish Oil for the GC-ECD Analysis of PCBs: Results Using a Dean Switch with Backflushing (Jan 2007)• 5989-6066EN Rapid Forensic Toxicology Screening Using an Agilent 7890A/NPD/5975C/DRS GC/MSD System (Jan 2007)• 5989-6018EN Improving Productivity and Extending Column Life with Backflush (Dec 2006)• 5989-5111EN Simplified Backflush Using Agilent 6890 GC Post Run Command (June 2006)• 5989-1716EN New Tools for Rapid Pesticide Analysis in High Matrix Samples (October 2004)
Productivity Tool Box for GC & GC/MS
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Productivity: Retention Time Locking
• More analyses per unit time . . . – Faster and more efficient separations
– Shorter analysis cycle time (time from injection to injection)
– Reduced requirement for sample preparation
• with consistently better results . . . – Quantitative: accuracy, precision, detection limits, linear range
– Qualitative: response ratios, confirmatory retention times , library searches (eliminate false negatives and false positives)
• while using less operator time for each analysis.– Less time performing maintenance– Extensive computer control and data processing
– Simplified operator review/approval
Productivity Tool Box for GC & GC/MS
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What is Retention Time Locking (RTL)?The ability to precisely match chromatographic retention times in any systems to those in another chromatographic system with the same nominal method and column.
How is Retention Time Locking Done?By adjusting column head pressure via EPC using interactive ChemStation software.
Retention Time Locking
Productivity Tool Box for GC & GC/MS
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Pesticides on Two Different GCs Before RTL
23 23.5 24 24.5 25 25.5
23 23.5 24 24.5 25 25.5
Productivity Tool Box for GC & GC/MS
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Pesticides on Two Different GCs After RTL
23 23.5 24 24.5 25 25.5
23 23.5 24 24.5 25 25.5
Productivity Tool Box for GC & GC/MS
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RTL Calibration - Done Once for a Given Method
� Make 5 runs at 5 different inlet pressures:� target -20%
� target -10%
� target
� target +10%
� target +20%
� Determine RT of your target compound in each chromatogram� Enter values into the RTL Software
Productivity Tool Box for GC & GC/MS
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Acquire RTLock Calibration Data..
Productivity Tool Box for GC & GC/MS
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RTL Calibration Runs Are Collected Automatically
5 10 15 20 25 30
34 psi
31 psi
28 psi
25 psi
22 psi
Dichlorvos Methyl chlorpyrifos
Mirex
15.192 min
15.771 min
16.433 min
17.201 min
18.121 min
Target Compound for RTL
Productivity Tool Box for GC & GC/MS
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RTL Calibration Runs Are Collected Automatically
And times can be edit manually
Productivity Tool Box for GC & GC/MS
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Productivity Tool Box for GC & GC/MS
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RTL Re-Locking Procedure for Trimmed Column
0
50
100
Original RTL Head pressure 16.00 psi
16.50 min.
16.34 min.Trim front of column
New RTL Head pressure 15.71 psi
0
50
100
0
50
100
16.50 min.
Re-lock method
Productivity Tool Box for GC & GC/MS
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Benefits of Locked Methods
• Faster method transfer & validation
• Faster startup after column maintenance
• Reduces / eliminates need to update RTs in calibration tables
• Easy set up of windows for SIM groups and MS/MS transitions
• Equivalent chromatography for all labs sharing a common method
• More efficient troubleshooting
• Easier review of data
• Faster identification of unknowns
Productivity Tool Box for GC & GC/MS
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Productivity: Trace Ion Detection
• More analyses per unit time . . . – Faster and more efficient separations
– Shorter analysis cycle time (time from injection to injection)
– Reduced requirement for sample preparation
• with consistently better results . . . – Quantitative: accuracy, precision, detection limits , linear range
– Qualitative: response ratios, confirmatory retention times, library searches (eliminate false negatives and false positives)
• while using less operator time for each analysis.– Less time performing maintenance
– Extensive computer control and data processing
– Simplified operator review/approval
Productivity Tool Box for GC & GC/MS
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Trace Ion Detection Technology
• Proprietary algorithm– Digital filtering
• Reduced noise level • Improved peak shape
– Smoothes ‘spikes’ on trace peaks
– Especially under-sampled peaks
• Improved library matchS/N = 92
WithoutTrace Ion Detection
S/N = 53
WithTrace Ion Detection
… better detection at trace levels
Productivity Tool Box for GC & GC/MS
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Improve Library Match QualityFenthion in strawberry extract
Match Quality30
Trace Ion Detection off
Trace Ion Detection on Match Quality92
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Trace Ion Detection Reduces False Negatives
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Literature for Trace Ion Detection
• Technical Overview 5989-6425EN , The 5975C Series MSD: Method Optimization and Trace Ion Detection (Roushall/Prest, Mar 07)
• App Note 5989-7670EN , Replacing Multiple 50-Minute FPD/ELCD/SIM Analyses with One 15-Minute Full-Scan Analysis for 10x Productivity Gain (Meng/Szelewski, Nov07)
Productivity Tool Box for GC & GC/MS
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Productivity: Fast Electronic - SIM/Scan Mode
• More analyses per unit time . . . – Faster and more efficient separations– Shorter analysis cycle time (time from injection to injection)
– Reduced requirement for sample preparation
• with consistently better results . . . – Quantitative: accuracy, precision, detection limits, linear range– Qualitative: response ratios , confirmatory retention times, library
searches (eliminate false negatives and false posit ives)
• while using less operator time for each analysis.– Less time performing maintenance
– Extensive computer control and data processing
– Simplified operator review/approval
Productivity Tool Box for GC & GC/MS
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High Performance, Fast Electronics
Higher percentage of time monitoring ions = more signal
Higher data rate for narrow “fast” peaks = better area precision
Productivity Tool Box for GC & GC/MS
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High Performance Electronics for High Performance Synchronous SIM/Scan
5989-3108EN: Improving Productivity with Synchronous SIM/Scan
Productivity Tool Box for GC & GC/MS
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Fast Electronics: Synchronous SIM/Scan
• The best of both modes in a single run– SIM = maximum sensitivity for target compounds– Scan = best identification of non-targets (unknowns )
• High speed electronics is an Agilent strength
… maximum information from a single run
Scan data points
SIM data points
Chromatographic peak time
Scan time SIM time
Tech Overview 5989-3108EN
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Under-Sampled Peaks Acceptable for MS
• Acceptable precision can be achieved with fewer poi nt per peak
– 6 samples/peak width for area; 8 samples/peak width for height
• Compromises to evaluate
– Affect of a slower data rate on quant precision
– Affect of shorter dwell time decrease SIM S/N
– Affect of faster scan rates decrease scan S/N
For many applications . . . thedecrease in precision and S/N are small compared to the benefits of SIM sensitivity andscan library searches
Productivity Tool Box for GC & GC/MS
Page 59
Literature for Synchronous SIM/Scan (slide 1 of 2 )
• Tech Note 5989-3108EN, Improving Productivity with Synchronous SIM/Scan (Meng, May’05 )• Tech Note 5989-5669EN, Strategies for Developing Optimal Synchronous SIM-Scan Acquisition Methods—AutoSIM/Sca n Setup and Rapid SIM ( Sept’06 )• App Note 5989-6066EN , Rapid Forensic Toxicology Screening Using an Agilent 7890A/NPD/5975C/DRS GC/MSD System (Quim by, Jan’07)• App Note 5989-4184EN , Synchronous SIM/Scan Low-Level PAH Analysis Using the Agilent Technologies 6890/5975 i nert GC/MSD (Szelewski, Nov’05 )• App Note 5989-3571EN, Determination of Trace Levels of Aromatic and Chlorinated Hydrocarbons in Water Using the G18 88 Headspace Sample/6890N and 5975 inert MSD ( Firor, Oct’05 )
Productivity Tool Box for GC & GC/MS
Page 60
Literature for Synchronous SIM/Scan (slide 2 of 2 )
• App Note 5989-3196EN, The Determination of Residual Solvents in Pharmaceuticals Using the Agilent G1888 Headspace/6 890N GC/5975 inert MSD system ( Firor/Gudat, June’05 )• App Note 5989-5494EN, The Determination of Extractables and Leachables in Pharmaceutical Packaging Material Usi ng Headspace GC/MS (Gudat/Firor, Aug’06 )•App Note 5989-4834EN , Screening for Hazardous Chemicals in Homeland Security and Environmental Samples Using a GC/MS/ECD/FPD with a 731 Compound DRS Database (Quimby/Szelewski, Feb’06 )• App Note 5989-3299EN, Identifying Pesticides with Full Scan, SIM, uECD, and FPD from a Single Injection ( Meng/Quimby, July’05 )• Tech Note 5988-4188EN (AutoSIM), New Approaches to the Development of GC/MS Selected Ion Monitoring Acquis ition and Quantitation Methods ( Prest/Peterson, Nov’01 )
Productivity Tool Box for GC & GC/MS
Page 61
Productivity – Method Translator
• More analyses per unit time . . . – Faster and more efficient separations– Shorter analysis cycle time (time from injection to injection) – Reduced requirement for sample preparation
• with consistently better results . . .– Quantitative: accuracy, precision, MDL, linearity, consistent sensitivity
– Qualitative: response ratios, confirmatory retention times, library searches (eliminate false negatives and false positives)
• while using less operator time for each analysis.– Less time performing maintenance
– Extensive computer control and data processing
– Simplified operator review/approval
Productivity Tool Box for GC & GC/MS
Page 62
What is Method Translation?
MTL is a freeware program that determines new method conditions such that relative elution order is constant, and relative run time is known.
MTL works:
g when changing column outlet pressure (e.g., from FID to MSD)
g when changing carrier gas type (e.g., from He to H2) or flow rate
g when changing column dimensions (same phase, different diameter, length, or phase ratio)
Productivity Tool Box for GC & GC/MS
Page 63
Screen capture showing the Method Translation (MTL) Software data entry used in a 4X speed gain translation.
Method Translator
Productivity Tool Box for GC & GC/MS
Page 64
250 µm(X1)30250
0.25018.0
01.970
2.0025.01500.003.02000.008.0280
10.00
100 µm(X2)10100
0.10036.55
00.470
1.0050.01500.006.02000.0016.02805.00
100 µm(X3)10100
0.10063.17
00.870
0.6775.01500.009.02000.0024.02803.30
100 µm(X4)10100
0.10090.00
01.5700.51001500.0012.02000.0032.02802.50
Length (m)I.D. (µm)D.F. (µm)Inlet P (psig)Outlet P (psia)Flow (mL/min)Init Temp (°C) Init Hold (min)Ramp 1 (°C/min)Final Temp1 (°C)Final Time 1 (min)Ramp 2 (°C/min)Final Temp 2 (°C)Final Time 2 (min)Ramp 3 (°C/min)Final Temp 3 (°C)Final Time 3 (min)
Speed GainColumn id.
Method Translations to 100 um Column
Productivity Tool Box for GC & GC/MS
Page 65
Method Translations to 15 m Column
30 m(X1)
19091S-4332500.2518.0
01.970
2.0025.01500.003.02000.008.0280
10.00
Part NumberI.D. (µm)D.F. (µm)Inlet P (psig)Outlet P (psia)Flow (mL/min)Init Temp (°C) Init Hold (min)Ramp 1 (°C/min)Final Temp1 (°C)Final Time 1 (min)Ramp 2 (°C/min)Final Temp 2 (°C)Final Time 2 (min)Ramp 3 (°C/min)Final Temp 3 (°C)Final Time 3 (min)
Speed GainColumn Length (m) 15 m
(X2.5)
2500.255.74
01.4970
0.8062.51500.007.52000.00202804.00
19091S-431
15 m(X4)
2500.2518.0
03.870
0.501001500.00122000.00322802.5
19091S-431
Productivity Tool Box for GC & GC/MS
Page 66
Productivity – Triple Axis Detector with Gain Normalization and EM Saver• More analyses per unit time . . .
– Faster and more efficient separations
– Shorter analysis cycle time (time from injection to injection)
– Reduced requirement for sample preparation
• with consistently better results . . . – Quantitative: accuracy, precision, MDL, linearity, consistent sensitivity– Qualitative: response ratios, confirmatory retention times, library
searches (eliminate false negatives and false positives)
• while using less operator time for each analysis.– Less time performing maintenance– Extensive computer control and data processing
– Simplified operator review/approval
Productivity Tool Box for GC & GC/MS
Page 67
Conventional Off-Axis Detector
hyperbolic quartztransmission
quadrupoleanalyzer
ion beam
energetic neutrals
Although not directly striking the HED-EM, excited helium neutrals can ionize other molecules and create secondary particles from collisions with surfaces (sputtered ions from surface contamination, ions from the surface, photons and electrons)
high energy dynode (high voltage pulls the ions away from the neutrals)
electron multiplier
Productivity Tool Box for GC & GC/MS
Page 68
Triple-Axis Detector
ion beam X
Y
OffsetZ
With a combination of three axes and appropriate shielding, noise from metastable helium, photons, etc. can be reduced to a minimum
This aperture is larger than the off-axis detector which means more ions and energetic neutrals pass to the detector shield blocking
secondary ions formed by metastable helium after the analyzer
Productivity Tool Box for GC & GC/MS
Page 69
Triple-Axis Detector: Higher Signal – Lower MDL
Lower detection limits !
Tech Overview 5989-7655EN
Increased slope = higher sensitivity
Dashed line show 95% confidence limits
fg
Productivity Tool Box for GC & GC/MS
Page 70
Triple Channel EM
•Triple channels improve signal amplification
– Lower initial EM voltage required
•Triple channels increase life– Lower cost of operation
Exit of the triple channels
Collector removed to show exit passages
Collector
Productivity Tool Box for GC & GC/MS
Page 71
Tuning – Optimization of Multiple Components
• Tuning ion transmission characteristics– Optimize potentials on lens and analyzer
– Effects the relative abundance of ions WITHIN a spectrum
• For example, the intensity ratio of m/z 100 to 200 or 100 to 300
– Effects the absolute number of ions entering the EM
– Improves spectra comparisons between instruments
– US EPA standards made this a critical issue in many areas of the world
• Gain Normalization of ion amplification (EM only)– Effect the ion ‘count’ or absolute abundance of each ion
– Does NOT affect the number of ions entering the EM
– Changes the amplification of charge passing through the EM
Productivity Tool Box for GC & GC/MS
Page 72
Gain Normalized EM Adjustment for Sensitivity
I
EMV: 1kV to 3kV
High Energy Dynode (10kV)QuadrupoleIon source
EMVElectron Multiplier (EM)
Ii
GAIN
Amplification of signalnow, user-selectable!!!
i
Tuning EM voltage changes sensitivity for all ions -- NOT the relative abundances
Tech Overview 5989-7654EN
Productivity Tool Box for GC & GC/MS
Page 73
S igna l vs E MV
0
50000
100000
150000
200000
250000
300000
1000 1200 1400 1600 1800 2000 2200 2400EM V
Sig
nal
Sensitivity Limitation of ATUNE + nV•During aging, the same EMV setting will not give the same signal!
ATUNE (new) ATUNE (aged)
ATUNE+400VATUNE + 400V
“New” detector “Aged” detector
Decreasingsignal with age
+ 600V
Tech Overview 5989-7654EN
As signal decreases, it appears the MS has lost sensitivity In reality, the
MS was OK, but the EMV was too low
Productivity Tool Box for GC & GC/MS
Page 74
Sensitivity Advantage of Gain Normalization
Sign a l v s G AIN
0
5000
10000
15000
20000
25000
30000
35000
40000
0 2 4 6 8 10 12 14 16 18 20
G ain Facto r as GA IN x 10^ 5
Sig
nal
“New”
“Aged”
•During aging, the same GAIN setting will give the same signal!
Tech Overview 5989-7654EN
With Gain Normalization, the operation does not have to think about aging, sensitivity is the same for a new or aged EM at any Gain setting – simple!
Productivity Tool Box for GC & GC/MS
Page 75
“ATune + nV” versus Gain Normalized Methods
9.80 9.90 10.00 10.10 10.20 10.30
1000
9.80 9.90 10.00 10.10 10.20 10.30
1000
“New” “Aged”
Consistent sensitivity over the life of the electron multiplier!Consistent sensitivity from MSD to MSD and lab to lab!
Tech Overview 5989-7654EN
GAIN Tune GAIN TuneATUNE+ n V
ATUNE+ n V
New triple channel EM ages more slowly
Productivity Tool Box for GC & GC/MS
Page 76
Benefits of Gain Normalization (EM Optimization)
New Option: GAIN Normalized methods
Gain Factors are set & saved as a method parameter !
Finer Gain Adjustment for better optimization
Greater reproducibility over time
Greater consistency -for any instrument, or -between a group of instruments
No linearity errors with new EM
Easier tuning & system troubleshooting
Six excellent reasons to use Gain Factors!!
Productivity Tool Box for GC & GC/MS
Page 77
Literature for Gain Normalization
• Technical Overview 5989-7654EN , Enhancements to Gain Normalized Instrument Tuning: Understanding the Benefits and Features• Technical Overview 5989-7655EN , The Triple-Axis Detector: Attributes and Operating Advice• Technical Overview 5989-6050EN , The 5975C Series MSD: Normalized Instrument Tuning
Productivity Tool Box for GC & GC/MS
Page 78
EM Saver
• When too many ions are striking the EM, the response saturates and the overload can damage the EM• EM Saver and fast electronics quickly alters the analyzer voltages to decrease ion transmission
• A simple concept with real benefits to EM life– Highly concentrated peaks cannot damage the Agilent EM
Productivity Tool Box for GC & GC/MS
Page 79
Productivity – Hydrogen Carrier Gas
• More analyses per unit time . . . – Faster and more efficient separations– Shorter analysis cycle time (time from injection to injection) – Reduced requirement for sample preparation
• with consistently better results . . . – Quantitative: accuracy, precision, detection limits, linear range
– Qualitative: response ratios, confirmatory retention times, library searches (eliminate false negatives and false positives)
• while using less operator time for each analysis.– Less time performing maintenance
– Extensive computer control and data processing
– Simplified operator review/approval
Productivity Tool Box for GC & GC/MS
Page 80
Helium Shortage Means Higher Operating Costs
www.cen-online.orgPg 31October 8, 2007
Productivity Tool Box for GC & GC/MS
Page 81
H2 Requires Different Setup and Extra Care
• Lower column head pressure experienced with H2– H2 is upwards of 100% faster than with helium; the column internal diameter may
need to decrease to have optimal pressure control – There is a downloadable Method Translation Software to guide the customer
• H2 is reactive towards some compounds. – This can be an advantage or a disadvantage depending on the application – Sometimes very reactive compounds can be measured as their hydrogenated
counterparts • Diffusion is much faster in H2
– The van Deemter curve will shift and the HETP (height equivalent of a theoretical plate; column efficiency) will be different compared to helium
– GC resolution can be improved under optimal conditions• H2 is explosive
– Auto-ignition temperature is 400ºC and the LEL/UEL are very wide– Special cautions may be required for safety– Hydrogen generators can greatly reduce safety concerns
Productivity Tool Box for GC & GC/MS
Page 82
Agilent Tests for Hydrogen Safety
Productivity Tool Box for GC & GC/MS
Page 83
Hydrogen Generators Make the Cost Very Low and Ensure High Quality Gas
Productivity Tool Box for GC & GC/MS
Page 84
Literature for Hydrogen Carrier Gas
• Manual G3170-90010 , 5975C MSD Hydrogen Safety (Oct ’05)• Technical Overview 5988-4971EN , A Complete Solution for Chlorinated Pesticides and Herbicides Using DB-35ms and DB-XLB Columns (hydrogen and helium comparison) (Dec ’01)
Productivity Tool Box for GC & GC/MS
Page 85
Productivity – Deconvolution Reporting Software
• More analyses per unit time . . . – Faster and more efficient separations
– Shorter analysis cycle time (time from injection to injection)
– Reduced requirement for sample preparation
• with consistently better results . . . – Quantitative: accuracy , precision, detection limits , linear range
– Qualitative: response ratios, confirmatory retention times, library searches (eliminate false negatives and false posit ives)
• while using less operator time for each analysis.– Less time performing maintenance
– Extensive computer control and data processing– Simplified operator review/approval
Productivity Tool Box for GC & GC/MS
Page 86
What is Deconvolution Reporting Software (DRS)?
• A second opportunity for accurate result without another analysis
– A post-run calculation based on the NIST algorithm
– A solution to the unpredictable matrix interferences
• DRS makes optimal use of both GC and MS information– Combines peak profiles and spectra
– Extract ‘pure component’ information from the coeluting peaks
– Uses RTL database spectra to filter analytes of interest from vast number of matrix peaks
– Confirms against complete NIST library spectra
– ChemStation QEdit summary of standard and deconvoluted data
Productivity Tool Box for GC & GC/MS
Page 87
Component 2
Component 3
Deconvolution
Deconvoluted peaks and spectra
matrix
target
interference
TIC & Spectrum
TIC
Peak detected with Trace Ion Detection
How Does AMDIS Work?
Some m/z values “ pure ”Some m/z values mixed
m/z
Mathematical “Separation”
Component 1
Uses Difference in Spectra, Retention Time and Peak Shape
Productivity Tool Box for GC & GC/MS
Page 88
Pulling a Useable Spectrum Out of a Mess
Analyte ions are buried in the matrix ions!!
‘Cleaned’ analyte spectrum is easy to match!
Productivity Tool Box for GC & GC/MS
Page 89
NISTConfirm+
ChemStationfor Quant
+AMDIS 32Deconvolute and ID
What is the Agilent DRS?
CONSOLIDATED QUANTITATIVEand
QUALITATIVE HTML REPORT
Productivity Tool Box for GC & GC/MS
Page 90
Reduced Errors and Less Faster Results
32 minutes~ 8 hoursProcessing Time
01False Positives
Same 37+ 99 additional
37Targets Found
Agilent DRS*CDFA
*CDFA is the California Department of Food and AgricultureData files courtesy of Dr. Mark Lee and Steve Siegel
Save about 7.5 hours to do other jobs
Summary of Pesticide Analysis in 17 Surface Water S amples
Productivity Tool Box for GC & GC/MS
Page 91
QEdit Summary of Qual and Quant (DRS A.04)
Overlay of target(s) and Deconvolutedion plots
Spectral review: Before AMDISAfter AMDISAMDIS Library
Areas & amounts from target ion andDeconvoluted ion
Deconvoluted ion plot
Target ion plot
Hits X = MSDA = AMDIS
Productivity Tool Box for GC & GC/MS
Page 92
Summary Report with MSD and AMDIS Results
partial report
Productivity Tool Box for GC & GC/MS
Page 93
Graphics Report
MSD and AMDIS 5-ion overlay
Raw, deconvoluted and library spectra
MSD and AMDIS areas and amounts
Productivity Tool Box for GC & GC/MS
Page 94
Supporting Literature for DRS (slide 1 of 3)
• App Note 5989-8582EN , Improved Forensic Toxicology Screening Using a GC/MS/NPD System with a 725-Compound DRS Database (Quimby, May08)– Capillary Flow Technology for ‘solvent vent’ and NPD– Backflush to shorten analysis time and increase column lifetime– Synchronous SIM/scan (max sensitivity and max information)– Trace Ion Detection to reduce noise before DRS– Next generation of DRS with AMDIS results in QEdit and Agilent database– Real blood extracts from NMS Lab, Willow Grove, PA, USA
• App Note 5989-7670EN , Replacing Multiple 50-Minute FPD/ELCD/SIM Analyses with One 15-Minute Full-Scan Analysis for 10x Productivity Gain (Meng/Szelewski, Nov07)– Capillary Flow Technology for multiple detectors (3-way splitter)– Backflush to shorten analysis time and increase column lifetime– Trace Ion Detection to reduce noise before DRS– Next generation of DRS with AMDIS results in QEdit and Agilent database– Real results from US Food and Drug Administration/Center for Food Safety and
Applied Nutrition (FDA/CFSAN)
Productivity Tool Box for GC & GC/MS
Page 95
Supporting Literature for DRS (slide 2 of 3)
• App Note 5989-7436EN , Screening for Pesticides in Food Using the Japanese Positive List Pesticide Method: Benefits of Using GC/MS with Deconvolution Reporting Software and a Retention Time Locked Mass Spectral Database (Wylie, Sept07)
• App Note 5989-6677EN , Reducing Analysis Time Using GC/MSD and Deconvolution Reporting Software (May07)
• App Note 5989-6066EN , Rapid Forensic Toxicology Screening Using an Agilent 7890A/NPD/5975/DRS GC/MSD System (Quimby, Jan07)
• App Note 5989-5435EN , Screening for 171 Volatile Organic Air Pollutants Using GC/MS with Deconvolution Reporting Software and a New Indoor Air Toxics Library (Wylie, Aug06)
• App Note 5989-5076EN , Screening for 926 Pesticides and Endocrine Disruptors by GC/Ms with Deconvolution Reporting Software and a New Pesticide Library (Wylie, Apr06)
Productivity Tool Box for GC & GC/MS
Page 96
Supporting Literature for DRS (slide 3 of 3)
• App Note 5989-4834EN , Screening for Hazardous Chemicals in Homeland Security and Environmental Samples Using a GC/MS/ECD/FPD with a 731 Compound DRS Database (Quimby, Szelewski, Feb06)
• App Note 5989-1716EN , New Tools for Rapid Pesticide Analysis in High Matrix Samples, (Szelewski, Quimby, Oct04)
• App Note 5989-1654EN , A Blind Study of Pesticide Residues in Spiked and Unspiked Fruit Extracts Using Deconvolution Reporting Software
• App Note 5989-1157EN , Comprehensive Pesticide Screening by GC/MSD using Deconvolution Reporting Software (Wylie/Szelewski/Meng, May04)
Productivity Tool Box for GC & GC/MS
Page 97
RTL is more flexible now…
GC/MSD user can manually edit these times
Productivity Tool Box for GC & GC/MS
Page 98
Largest Selection of Industry Specific Retention Ti me Locked Databases
modify a library to meet your need… or create your o wn
Product No. RTL DBL Description CompoundsG1671AA Hazardous Chemical 730G1672AA Pesticide 926G1673AA Indoor Air Toxics 171G1674AA Forensic Toxicology 723G1675AA JPN Positive List Pesticide 431G1676AA Fiehn Metabolomics 665G1677AA Environmental Semi-voas 273
Free Volatile Organic Compounds 65Free PCB Congeners 209Free Forensic Toxicology 277Free Fatty Acid Methyl Ester 37Free Flavors 409Free Organotin Derivatives Methyl, Ethyl, Pentyl
Library include GC method details, Getting Started manual, application notes, and HELP files
Productivity Tool Box for GC & GC/MS
Page 99
Supporting Literature for RTL (slide 1 of 4)
• App Note 5989-7875EN, Semivolatiles Retention Time Locked (RTL) Deconvolution Databases for Agilent GC/MSD Systems (Szelewski, Feb’08) G1677AA
• App Note 5989-7670EN , Replacing Multiple 50-Minute FPD/ELCD/SIM Analyses with One 15-Minute Full-Scan Analysis for 10x Productivity Gain (Meng/Szelewski, Nov07) G1672AA
• App Note 5989-7436EN , Screening for Pesticides in Food Using the Japanese Positive List Pesticide Method: Benefits of Using GC/MS with Deconvolution Reporting Software and a Retention Time Locked Mass Spectral Database (Wylie, Sept07) G1675AA
• App Note 5989-6677EN , Reducing Analysis Time Using GC/MSD and Deconvolution Reporting Software (May07)
• App Note 5989-6066EN , Rapid Forensic Toxicology Screening Using an Agilent 7890A/NPD/5975/DRS GC/MSD System (Quimby, Jan07) free DBL
Productivity Tool Box for GC & GC/MS
Page 100
Supporting Literature for RTL (slide 2 of 4)
• App Note 5989-5435EN , Screening for 171 Volatile Organic Air Pollutants Using GC/MS with Deconvolution Reporting Software and a New Indoor Air Toxics Library (Wylie, Aug06) G1673AA
• App Note 5989-5076EN , Screening for 926 Pesticides and Endocrine Disruptors by GC/Ms with Deconvolution Reporting Software and a New Pesticide Library (Wylie, Apr06) G1672AA
• App Note 5989-4834EN , Screening for Hazardous Chemicals in Homeland Security and Environmental Samples Using a GC/MS/ECD/FPD with a 731 Compound DRS Database (Quimby/Szelewski, Feb06) G1671AA
• App Note 5989-3347EN , Developing an eMethod for the Analysis of Volatile Organic Compounds in Water Using Purge and Trap/GC with Agilent’s New 5973 inert Mass Spectrometer (Wylie, Jul’05)
• App Note 5989-2850EN , Determination of Polybrominated Diphenyl Ethers in Polymeric Materials Using the 6890 GC/5973N inert MSD with Electron Impact Ionization (Tu/Prest, Apr05)
Productivity Tool Box for GC & GC/MS
Page 101
Supporting Literature for RTL (slide 3 of 4)
• App Note 5989-1716EN , New Tools for Rapid Pesticide Analysis in High Matrix Samples, (Szelewski/Quimby, Oct04)
• App Note 5989-1654EN , A Blind Study of Pesticide Residues in Spiked and Unspiked Fruit Extracts Using Deconvolution Reporting Software (Sandy, Oct04)
• Tech Overview 5989-0916EN , Building and Editing RTL Screener/Quant Databases and Libraries (Szelewski/Weiner/Meng, June04)
• App Note 5989-1157EN , Comprehensive Pesticide Screening by GC/MSD using Deconvolution Reporting Software (Wylie/Szelewski/Meng, May04)
• App Note 5968-5871EN , Improving the Analysis of Fatty Acid Methyl Esters Using Retention Time Locked Methods and Retention Time Databases (David/Sandra/Wylie, Sept’03)
• App Note 5988-9256EN , Improving the Analysis of Organtin Compounds Using Retention Time Locked Methods and Retention Time Databases (David/Sandra/Wylie, Apr03)
Productivity Tool Box for GC & GC/MS
Page 102
Supporting Literature for RTL (slide 4 of 4)
• App Note 5988-7150EN , Solid-phase Extraction and Retention Time Locked GC/MS Analysis of Selected Polycyclic Aromatic Hydrocarbons (PAHs) (Prest, July’02)
• App Note 5988-3934EN , Retention Time Locked GC-MS Analysis of Phenols (Reese/Prest, Apr02)
• App Note 5988-4392EN , Identification and Quantitation of Pesticides in the Part-per-Trillion Range Using Retention Time Locking and GC/MS (Meng, Nov’01)
• Tech Note 5988-4188EN (AutoSIM), New Approaches to the Development of GC/MS Selected Ion Monitoring Acquisition and Quantitation Methods (Prest/Peterson, Nov’01)
• App Note 5988-2244EN , A New Approach to the Analysis of Phthalate Esters by GC/MS (George/Prest, Mar’01)
• App Note 5988-9455EN , Ambient Headspace GC and GC-MSD Analysis of Non-Polar Volatiles in Water (Szelewski/Quimby, Feb’00)
• App Note 5968-8657E , Retention Time Locking: Creating Custom Retention Time Locked Screener Libraries (Weiner/Prest, Dec’99 )