5975 inert msd - agilent

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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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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Quick Remove Top Cover

Easy analyzer access

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Functional Front Window

• Wire connections

• Filament operation

• Column insertion

• CI Source identification

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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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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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New Sensitivity Specifications –EI Scan

182:1 s/n100:160:1EI1 pg OFN

59755973

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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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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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Extended Mass Range – PBDE 209

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959

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5975 inert MSD Theoretical

Extended Mass Range –PBDE 209

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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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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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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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6850 GC Control via ChemStation

• 5973N MSD (G2570A)

• 5973 inert MSDs

• 5975 inert MSDs

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Agilent MSD Unique Features

• Inert Ion source

• Hyperbolic quad

• Quad temp

• CI system

• Analyzer modularity

Synchronous SIM/Scan

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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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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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• 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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Inject Standard

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AutoSIM

Application note: 5988-4188EN

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Edit SIM Method

AutoSIM automatically creates SIM groups and populates ions in each group

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Synchronous SIM/Scan

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1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.0011.0012.0013.00

10000

30000

50000

70000

90000

110000

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

10000

30000

50000

70000

90000

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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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

1000

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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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Scan

SIM

1

2 3

4 5

6

1

2 3

4 5

6

VOC Gases (1 ppb each)

1. Dichlorodifluoromethane

2. Chloromethane

3. Vinyl chloride

4. Bromomethane

5. Ethyl chloride

6. Trichlorofluoromethane

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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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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

21

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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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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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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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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Allergens analysis in SIM/Scan

After shave1% v/v 1ul Split 20 : 1SCAN

SIM

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Allergens Overlaid SIM/Scan

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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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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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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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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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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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Microfluidic Splitter operating modes (2) Splitter

AUX EPCColumn in

MSD

Detector 1



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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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Microfluidic Splitter – ‘Chromatographically Transparent’

MSD

ECD

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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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AUX EPCColumn 1 / Inlet 1

MSD

Column 2 / Inlet 2

Microfluidic Splitter operating modes :(3) Dual Column Inlet



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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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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


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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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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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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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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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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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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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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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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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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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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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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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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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Explorer Navigation

Explorer navigation

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Interactive Edit Integration

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Right Click Features

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SIM Parameter Table

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QEdit

Reports

Baseline Display

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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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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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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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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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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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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

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5975 inert msd - agilent

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