Post on 29-Dec-2021
transcript
5975 inert MSD
Chris SandyEuropean GC-MS Product SpecialistAgilent Technologies
Presenter: Chris Sandy
Welcome to our e-Seminar:
Introduction of the new 5975 inert MSD for expanding your application capabilities
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Slide 3Chairperson: John Vis, Audio: +44 207 162 0125
What Has Changed?
What’s the same?
• Reliability
• Quality
• Inertness
But NOT Performance – it’s better!
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Slide 4Chairperson: John Vis, Audio: +44 207 162 0125
What’s Different?
• Functional industrial design
• More efficient vacuum system
• Extended mass range
• AutoCI
• New sensitivity specifications
• Synchronous SIM/Scan
• EI with CI ion source
• 6850 GC control
• QuickSwap MSD interface
• Review of differentiators
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Slide 5Chairperson: John Vis, Audio: +44 207 162 0125
Quick Remove Top Cover
Easy analyzer access
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Slide 6Chairperson: John Vis, Audio: +44 207 162 0125
Functional Front Window
• Wire connections
• Filament operation
• Column insertion
• CI Source identification
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Slide 7Chairperson: John Vis, Audio: +44 207 162 0125
Modified MSD mainframe
for quick/easy turbo pump
maintenance
Modified Mainframe
New turbo and mechanical vacuum pumps are more efficient for Helium
and Hydrogen
• New 70 L/sec standard pump
• New 262 L/sec performance pump
• New 2.5 m3/hour mechanical pump
(67% more capacity)
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Slide 8Chairperson: John Vis, Audio: +44 207 162 0125
G3397A – optional gauge/controller
Integrated Ion Gauge/Controller
• Greater vacuumprecision
• Excellent for trouble shooting small leaks –every system should have one!
Software displayLocal display
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Slide 9Chairperson: John Vis, Audio: +44 207 162 0125
New Sensitivity Specifications –EI Scan
182:1 s/n100:160:1EI1 pg OFN
59755973
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Slide 10Chairperson: John Vis, Audio: +44 207 162 0125
New Sensitivity Specifications –CI Scan
125:175:1PCI100 pg BZP
300:1 (100 fg)
500:1(1 pg)
NCI1 pg/100 fg
OFN
59755973
704:1 s/n (100 fg OFN under NCI)
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Slide 11Chairperson: John Vis, Audio: +44 207 162 0125
Extended Mass Range
• 1050 m/z for 5975 inert MSD
• Quadrupole modified
• New electronics
• 800 m/z for all 5973 MSDs
(Software upgrade does not enable 1050 m/z)
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Slide 12Chairperson: John Vis, Audio: +44 207 162 0125
Extended Mass Range – PBDE 209
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Slide 13Chairperson: John Vis, Audio: +44 207 162 0125
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5975 inert MSD Theoretical
Extended Mass Range –PBDE 209
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Slide 14Chairperson: John Vis, Audio: +44 207 162 0125
AutoCI
• AutoCI – Fully automated setup/tuning
• No external manual control
• CI made as easy as EI!
The new 5975
CI interface
The old 5973 manual CI interface
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Slide 15Chairperson: John Vis, Audio: +44 207 162 0125
Automated EI with CI Source
• March 2004: 5973 MSD
• Application note on EI with CI ion source
5989-0595EN
• Now: 5975 MSD
• Automated switching between EI and CI in a
sequence
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Slide 16Chairperson: John Vis, Audio: +44 207 162 0125
Automated EI with CI Source
Setup steps:
1. Install CI Source
2. Tune instrument in PCI – create PCICH4.u
3. Auto create EI tune file – create ei-cisource.u
4. Tune instrument in NCI – NCICH4.u
5. Assign tune file with method and run in sequence
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Slide 17Chairperson: John Vis, Audio: +44 207 162 0125
6850 GC Control via ChemStation
• 5973N MSD (G2570A)
• 5973 inert MSDs
• 5975 inert MSDs
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Slide 18Chairperson: John Vis, Audio: +44 207 162 0125
Agilent MSD Unique Features
• Inert Ion source
• Hyperbolic quad
• Quad temp
• CI system
• Analyzer modularity
Synchronous SIM/Scan
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Slide 20Chairperson: John Vis, Audio: +44 207 162 0125
Set Up Synchronous SIM/Scan
• SIM/Scan data
analysis requiresmixed mode dataview.
• SIM/Scan data issaved in the samedata file directory.
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Slide 21Chairperson: John Vis, Audio: +44 207 162 0125
Comparison of SIM/scan Implementations
Implementation (1) – ‘coarse granularity’
Agilent Implementation– ‘fine granularity’ for whole acquisition time
Implementation (2) – ‘fine granularity’ at specific times
11.20 11.40 11.60 11.80 12.00 12.20 12.40 12.60 12.80 13.00 13.20 13.40
Scan SIM
TIME
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Slide 22Chairperson: John Vis, Audio: +44 207 162 0125
• AUTOSIM is a standard feature of G1701DA Software
• AUTOSIM provides rapid and automatic conversion of a Scan method to SIM/Scan
• AUTOSIM creates SIM method based on Calibration table
• The operator has fine control over SIM parameter settings
• The SIM ions/groups/times are saved automatically to the method
Synchronous SIM/Scan –AutoSIM
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Slide 23Chairperson: John Vis, Audio: +44 207 162 0125
Inject Standard
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Slide 24Chairperson: John Vis, Audio: +44 207 162 0125
AutoSIM
Application note: 5988-4188EN
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Slide 25Chairperson: John Vis, Audio: +44 207 162 0125
Edit SIM Method
AutoSIM automatically creates SIM groups and populates ions in each group
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Slide 26Chairperson: John Vis, Audio: +44 207 162 0125
Synchronous SIM/Scan
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Slide 27Chairperson: John Vis, Audio: +44 207 162 0125
1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.0011.0012.0013.00
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130000TIC: 1 ppb 60 VOCs.D\DATA.MS
1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.0011.0012.0013.00
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TIC: 1 ppb 60 VOCs.D\DATASIM.MS
Scan and SIM Chromatograms from SIM/Scan Analysis of 60 VOCs at 1 ppb Each
SIM
Scan
• Velocity XPT/6890N/5975 P&T/GC/MS system• 20-m X 0.18 mm X 1.0 µmDB-VRX column• Scan sampling rate = 2; Dwell =20 ms for SIM
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Slide 28Chairperson: John Vis, Audio: +44 207 162 0125
Synchronous SIM/Scan Analysis of VOC Target Gases at 1 ppb each
1.20 1.30 1.40 1.50 1.60 1.70 1.80 1.90 2.000
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1.151.201.251.301.351.401.451.501.551.601.651.701.751.801.851.901.950
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SIM
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VOC Gases (1 ppb each)
1. Dichlorodifluoromethane
2. Chloromethane
3. Vinyl chloride
4. Bromomethane
5. Ethyl chloride
6. Trichlorofluoromethane
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Slide 29Chairperson: John Vis, Audio: +44 207 162 0125
SIM/Scan and Scan-Only Sensitivity Comparison: 5-mL Purge of 1 ppb Ethyl Chloride (a Low Responding Gas)
2075Scan(SIM/Scan)
1773Scan(Scan only)
254749SIM(SIM/Scan)
Peak/Peak S/N
RMS S/N
• SIM as part of SIM/Scan run gives 10X greater sensitivity
• Still get ≥≥≥≥ 8 scans across peak using same scan rate (n = 2)
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Slide 30Chairperson: John Vis, Audio: +44 207 162 0125
Why Our SIM/Scan is So Good
22
Performance Electronics
Nearly no fall off with increasing scan speed
21100
50
Phenanthrene
20 ~ 6250 amu/sec
23 ~ 781 amu/sec
Nearly no fall off with increasing scan speed
Standard Electronics
Fall off with increasing scan speed
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22
100
50
Phenanthrene
23 ~ 781 amu/sec
Fall off with increasing scan speed
20 ~ 6250 amu/sec
Moving from 23 to 22
doubles scans
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Slide 31Chairperson: John Vis, Audio: +44 207 162 0125
For a 0.25 mm column, a typical peak width (at base) is 6 seconds. Switch from scan at 2^2 mode to SIM/scan@2^1, there will still be the same 15 cycles over the peak, but gets the 4-ion SIM group data for FREE.
Scan ���� SIM/scan45 to 555 => 510 amu
Scan
45 to 555 amu, Scan only @ 2^2
2.87 scan/sec1563 amu/s
SIM
4 ions, 40 ms
1 sec 2 sec
2^06250 amu/s
3.76 cycle/s
2^13125 amu/s
2.88 cycle/s
2^21563 amu/s
1.94 cycle/s
Same width (SIM)
a cycle
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Slide 32Chairperson: John Vis, Audio: +44 207 162 0125
Synchronous SIM/Scan –Key Features
• Performance Electronics really make the difference
• SIM Improvements – 100 groups and 60 ions per group
• Minimum dwell time is reduced by half to 5 ms
• Even more data points per SIM peak
• Synchronous SIM/Scan available on 5973 MSDs with performance electronics (req. Smart Card 3+)
• Upgrades: G1088A and G1088B AND SW upgrade
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Slide 33Chairperson: John Vis, Audio: +44 207 162 0125
Synchronous SIM/ScanApplication examples
•Allergens analysis: Proposed 5975 method, 26 Targets
SIM/Scan mode
- SIM table built with AUTOSIM
- Quant with SIM target ion
- Confirmation by DRS with Scan data
•Pesticides analysis with microfluidics technology for flexible GC and GC/MS analysis
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Slide 34Chairperson: John Vis, Audio: +44 207 162 0125
Allergens analysis in SIM/Scan
After shave1% v/v 1ul Split 20 : 1SCAN
SIM
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Slide 35Chairperson: John Vis, Audio: +44 207 162 0125
Allergens Overlaid SIM/Scan
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Slide 36Chairperson: John Vis, Audio: +44 207 162 0125
Allergens SIM/Scan analysis and deconvolution with DRS
With courtesy of Chris Sandy and J-F Garnier
Quant based on SIM target ion
Confirmation based on deconvoluted full mass spectrum
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Slide 37Chairperson: John Vis, Audio: +44 207 162 0125
Synchronous SIM/Scan –Summary
• Great for target analysis and identifying unknowns
• SIM data for quantitation
• Scan data for confirmation of unknowns
• Our SIM/Scan delivers real performance based on superior electronics
Overview of MicrofluidicTechnologies
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Slide 39Chairperson: John Vis, Audio: +44 207 162 0125
Connections to Microfluidic Splitter
•Deactivated, very low internal volume to prevent peak tailing orband broadening
•A single, special design metal ferrule
• More inert that graphite/vespel, does not leak at high oven temperatures
To Detector 1To Detector 2
Plate
Metal
Ferrule
Nut
Column
Channel
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Slide 40Chairperson: John Vis, Audio: +44 207 162 0125
Microfluidic Splitter hardware installation
Deactivated microfluidicsplitter operates to 350 C.
Uses metal ferrules to eliminate leaks and
retightening
To MSD
To Det 1
Column in
Makeup from Aux EPC
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Slide 41Chairperson: John Vis, Audio: +44 207 162 0125
AUX EPC
MSD
Column in
Blocked
Microfluidic Splitter operating modes * (1) Single Column
* Aux EPC Flow enables column change-over without venting MSD
* Aux EPC Flow enables inlet / septum maintenance without ingressof air into column.
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Slide 42Chairperson: John Vis, Audio: +44 207 162 0125
Microfluidic Splitter operating modes (2) Splitter
AUX EPCColumn in
MSD
Detector 1
* Aux EPC Flow enables column change-over without venting MSD
* Aux EPC Flow enables inlet / septum maintenance without ingressof air into column.
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Slide 43Chairperson: John Vis, Audio: +44 207 162 0125
Splitting to 2 Detectors
Effluent Splitter
with Makeup
6890N GC
Column
AUX EPC
3.8 psig
0.814 m X 0.18 mm id
1.1 m X 0.18 mm id
15 m X 0.25 mm id X 0.25 um HP-5MS
Configuration for 2:1 Split to MSD
mECD
Auto-sampler
5975 InertMSD
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Slide 44Chairperson: John Vis, Audio: +44 207 162 0125
Microfluidic Splitter – ‘Chromatographically Transparent’
MSD
ECD
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Slide 45Chairperson: John Vis, Audio: +44 207 162 0125
100 ppb VOAs, 100 ppm Gasoline in Water, Ambient Headspace
0 2 4 6 8 10 12
0 2 4 6 8 10 12
0 2 4 6 8 10 12
Scan
ECD
SIM
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Slide 46Chairperson: John Vis, Audio: +44 207 162 0125
AUX EPCColumn 1 / Inlet 1
MSD
Column 2 / Inlet 2
Microfluidic Splitter operating modes :(3) Dual Column Inlet
* Aux EPC Flow enables column change-over without venting MSD
* Aux EPC Flow enables inlet / septum maintenance without ingressof air into column.
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Slide 47Chairperson: John Vis, Audio: +44 207 162 0125
Dual Column Configuration*
Back : 30m x 0.25mm ID x 0.25um HP5-MS
Front : 12.4m x 0.25mm ID x 0.25um HP5-MS
25 mins
6 mins
*Requires performance turbo pump
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Slide 48Chairperson: John Vis, Audio: +44 207 162 0125
AUX EPCColumn 1 / Inlet 1
MSD
Column 2 / Inlet 2
Microfluidic Splitter operating modes :(4) Dual Column Inlet + Olfactory Port + MSD
ODO II* Aux EPC Flow enables column change-over without venting MSD
* Aux EPC Flow enables inlet / septum maintenance without ingressof air into column.
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Slide 49Chairperson: John Vis, Audio: +44 207 162 0125
AUX EPC3.8 psig Column inlet
23.73 psig
MSD
Detector 1
Splitter mode – acquiring data
AUX EPC25.0 psig Column inlet
1.0 psig
MSD
Backflush mode
Detector 1
Microfluidic Splitter operating modes *
(5) Splitter mode with Backflush
* Aux EPC Flow enables column
change-over without venting MSD* Aux EPC Flow enables inlet / septum
maintenance without ingress of air into column
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Slide 50Chairperson: John Vis, Audio: +44 207 162 0125
6890N/5975 inert Pesticide Analysiswith 3-Way Splitter
3-way Effluent Splitter with Makeup
Auto-sampler
6890N GC
Column
Phosphorus FPD
30 m X 0.25 mm id X 0.25 um HP-5MS
1X method with 10:10:1 split FPD:MSD:ECD
5975InertMSD
uECDAUX EPC
3.8 psig
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Slide 51Chairperson: John Vis, Audio: +44 207 162 0125
1-injection-4-signal System
• 5975, RTLocked, 30m x 0.25mm x 0.25um HP-5MS
• Samples: pesticide mix at 10, 1, and 0.1 ppm
• Injection: 10:1 split
• At the end of the column, eluent flow is split 3 ways: MSD:FPD:µECD = 10:10:1
10:1 split
SIM/Scan
µECD
FPD
~480 pg
~480 pg
~48 pg
Injection 10 ppm (10000 pg)
1000 pg
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Slide 52Chairperson: John Vis, Audio: +44 207 162 0125
5975 SIM/scan + 3-way splitterUltimate Pesticide System
Scan: ~ 480 pg
SIM: ~ 480 pg
FPD: ~ 480 pg7 peaks
5.00 10.00 15.00 20.00 25.00 30.00 35.00 40.00 45.00
µECD: ~ 48 pg
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Slide 53Chairperson: John Vis, Audio: +44 207 162 0125
QuickSwap MSD interfaceAvailable October 1st, 2005
• Replacement for NoVent
• Remove column w/o venting
• Backflush mode
• Inlet maintenance reverse flow
• Removes heavies from column
• Maintain constant flow to MSD
MS
Transferline
Column
EPC inlet
Microfluidic technology
Requires performance turbo for flow rates > 2 cc/min
Introduction to eMethods and the new MSD Chemstation
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Slide 55Chairperson: John Vis, Audio: +44 207 162 0125
What are eMethods?
• eMethods is short for Electronic Methods.
• Can now package existingGC/MSD methods
• Export them to other 5973 MSDs
• Export them to 5975 inert MSDs
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Slide 56Chairperson: John Vis, Audio: +44 207 162 0125
eMethod Benefits
• Fast setup of new 5975 inertMSD
• Method sharing between5973 and 5975 MSDs
• Download apps from websiteand import entire method intoMSD ChemStation
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Slide 57Chairperson: John Vis, Audio: +44 207 162 0125
New 5975 inert eMethods
• PBDE Flame Retardants
• SIM/Scan – Pesticides in Water and Food
• VOCs via Headspace – European method
• Residual Solvents via Headspace
• NIDA Drugs
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Slide 58Chairperson: John Vis, Audio: +44 207 162 0125
MSD ChemStation Software
• Two GC/MS perChemStation
• GC and GC/MS control
• Retention time locking
• Custom reports
• eMethods
• Four configurations
• Enhanced mode
• EnviroQuant
• DrugQuant
• Reformulated Gas
Most popular GC/MS software in the world
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Slide 59Chairperson: John Vis, Audio: +44 207 162 0125
Instrument Control Enhancements
• Combined Top/Instrument Control Screen
• New icons for quick access to tune, EMF and print
• Configurable sequence table
• More right mouse click functions in editing sequences
• Printing selected sections of method and sequence
• Import of GC ChemStation method parameters(excluding 5890 GC)
• Display of IP address(s) of GC and MSD instruments
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Slide 60Chairperson: John Vis, Audio: +44 207 162 0125
Data Analysis Enhancements
• Explorer-style navigation tool
• Interactive editing of Integration Parameters
• Switchable right mouse click functions
• Spreadsheet-like SIM Parameters Table
• Icons for custom tools, DA options, variable watch
• Toolbar on/off capabiity
• Selectable DA color themes
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Slide 61Chairperson: John Vis, Audio: +44 207 162 0125
Data Analysis Enhancements
•QEdit functionality is improved:
• Separate window for Baseline Display
• Generating reports directly from QEdit
• Custom configuring X-axis
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Slide 62Chairperson: John Vis, Audio: +44 207 162 0125
Explorer Navigation
Explorer navigation
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Slide 63Chairperson: John Vis, Audio: +44 207 162 0125
Interactive Edit Integration
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Slide 64Chairperson: John Vis, Audio: +44 207 162 0125
Right Click Features
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Slide 65Chairperson: John Vis, Audio: +44 207 162 0125
SIM Parameter Table
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Slide 66Chairperson: John Vis, Audio: +44 207 162 0125
QEdit
Reports
Baseline Display
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Slide 67Chairperson: John Vis, Audio: +44 207 162 0125
Library Options
• NIST05
• Wiley 7th ed
• Stan pesticide
• Pfleger/Maurer/Weber MS Drug Library, 3rd ed
• NIST Chemical Structures Library
NEW
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Slide 68Chairperson: John Vis, Audio: +44 207 162 0125
Other Software Options
• Deconvolution Reporting Software
- New Revison A.02 released Aug 1, 2005
• Security ChemStation
• Headspace software
• RTL Pesticide Database : FAMES, Flavors, Volatiles Organics, Organotin derivatives, PCB congeners, Forensic toxicology
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Slide 69Chairperson: John Vis, Audio: +44 207 162 0125
Expanding the portfolio of RTL / DRS Databases
• Updated RTL Pesticides Database, Nov 2005
Adding ~ 200 new compounds
• TIC Toxic Industrial Chemicals Database, Nov 2005
~ 800 compounds (VOC, SVOC, Dioxins, PCBs andPesticides)
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Slide 70Chairperson: John Vis, Audio: +44 207 162 0125
GC/MS Configurations
• 5973N EI with diffusion pump
• 5975 inert EI with standard turbo pump
• 5975 inert EI with performance turbo pump
• 5975 XL EI/PCI/NCI with performance turbo pump
All systems available with choice of either 6850 or 6890 GCs
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Slide 71Chairperson: John Vis, Audio: +44 207 162 0125
Summary
Agilent 5975Inert MSD
• Better reliability and quality
• Enhanced performance
• eMethods
• AutoSIM and SIM/scan
• Higher mass range
• AutoCI
• Sensitivity
• Software improvements
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Slide 72Chairperson: John Vis, Audio: +44 207 162 0125
Thank you for attending today’s Agilent e-Seminar.
Our e-Seminar schedule is expanding regularly.
Please check our web site frequently at:
www.agilent.com/chem
If you would like to receive regular updates please
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