Resolve Your Search for More Ions:The 5977B, 7000D, and 7010B GC/MS Instruments

Stephan Baumann

ASTS Talk

November, 2016

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The Most Powerful EI GC/MS Source Ever Made….

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5977A Extractor Source

More intense electron beam

Longer path length for electron beam/effluent interaction

X

=Up to 30x More Ions Produced

NEW! 5977B High Efficiency Source

5977B High Efficiency Source with Magnet Removed

How the HES works

High emission filaments for more electron current

Powerful cylindrical magnet collimates electrons

Long path length for ionization

The Most Powerful EI GC/MS Source Ever Made….

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Conventional EI source on 7000C and 5977A 4 fg OFN IDL 7000C<10 fg OFN IDL 5977A

High Efficiency Source on Agilent 7010 and 5977B

0.5 fg OFN IDL70101.5 fg OFN IDL 5977B

These values must be met at instrument install

The Most Powerful EI GC/MS Source Ever Made….

In a ultra low noise environment A small noise variation creates a big SNR variation

8 OFN runs Area Noise SNR(Height/noise)

Minimum (for each value) 241 0.001 2480

Maximum (for each value) 255 0.15 244035

Average (for each value) 246 0.054 39996

% RSD 2.0 97.7 207.1

8 consecutive injections of 1 μl, 100fg/μl OFN. The peaks virtually overlap; the signal area and height values are very consistent. The baseline noise is very low for every plot, but the automatically selected RMS noise values vary in a wide range, yielding the values below for the 8 OFN injections:

The area values of the response of the injections would not indicate a factor of 100 fold difference in SNR. But a small difference in the ultra low noise baseline can result in extreme difference in the calculated SNR.

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Detection Limit as Defined by Basic Statistics where

is the detection limit

is the student “t” value, given for the desired • confidence level (99%) and • degree of freedom (# of repeated measurements -1)

SD is the standard deviation of the value measured

Amount measured should be only 5-10X higher than the DL

This can be applied in any discipline, not just analytical chemistry

DL = t * SD

DLt

SD

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Calculating IDL (Instrument Detection Level) on a 5977A

t α, n-1 value for 99% confidence level and 8 injection is 2.998SD is determined from the standard deviation of the area count of 8 consecutive injections of 1 µl of 100fg/µl OFN std.

- This would give us IDL based on area. Much more useful if we express this value based on concentration.

IDL

%RSD

IDL

100fg

Average area count represents 100fg injected amount

IDL (area) = 2.988* SD (area)

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But Wait – Even More Innovation

Outcome

JetClean – self-cleaning ion source technology

Reduces cleaning up to 80%. Run more samples!

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Dramatic visual JetCleandemonstration

Easily removed Sharpie marks

Prevents deposits that would require manual cleaning

JetClean

But Wait – The Proof is in the Pudding!

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• SSL, MMI, GSV, LSV inlets

• FID, TCD, ECD, NPD, FPD, NCD, SCD detectors

• SQ and TQ mass spectrometers

• Headspace, thermal desorption, purge and trap samplers

• 16-, 50-, 150-position auto-injectors and trays

• Software: OpenLAB and MassHunter

But Wait – Even More Innovation with Intuvo

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Reimagine What Can Be Done with Single Quad GC/MS

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Rock Solid Precision

Overlay of 8 injections of 2pg of

pyrene:

Exceptional Science --Analyze and Identify Trace Compounds Previously Unseen with Single Quad GC/MS

Do more with Less Sample – Achieve today’s analytical sensitivity using a fraction of the sample

Minimized Environmental Impact

10 fg OFN injections

LOD = 0.57 fgcalculated from 8 consecutive injections

Extremely Low Limits of Detection

Benefits That Touch Your Entire Operation

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Push past the analytical frontier – do amazing science in new ways

Ship, store and dispose of a fraction of your current, valuable sample volume

Less organic solvent to buy, store, and dispose of

A cleaner system means less downtime for cleaning and maintenance

Less Sample Injected = Cleaner System

Less Frequent Liner Maintenance

Longer Column Life

Faster Sample Prep

1 Liter

100 mL

Decreased Shipping Costs

Decreased Storage Costs

Decreased Disposal Costs

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PAH analyses is one of most common services offered in contract labs

• Extraction out of soil or water requires multi-steps; large volumes of solvent (DCM); silica or florisil gel clean ups

• Analysis is typically performed on a single quadrupole GCMS or GC-FID

Significant pain points

• Sampling volumes of 1L

• Significant costs associated with transport

• Samples break during transit

• Significant usage of solvents for extraction (cost and disposal)

• Extensive sample cleanup with columns

Agilent’s Programmable Inlet – MultiModeInlet (MMI)

7890 standard pneumatics

7890 turn-top

7890 standard capillary fitting

Uses 7890 S/SL liners, septa and o-rings

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Multimode Inlet Features HardwareTemperature range of -160C to 450C

Heating @ 15C/sec (900C/min)

Injection Modes: Hot S/SL, Cold S/SL, all in pulsed mode, solvent vent mode, residue removal mode

Support for single stroke injections from 0.1 L to 250 L

Able to reduce extractable volumes to 100 mL of water

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Backflush to remove non-volatile residues

MassHunter GC/MS Acquisition for GC/MSD

Unified GC/MS Acquisition and MassHunter Data Analysis; with MSD ChemStation workflow for GC/MSD

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GC/MSD SoftwareMassHunter Qual

MassHunter QuantMH

CS

MassHunter GC/MS Acquisition

And Use EitherMassHunter Data Analysis

ORMSD ChemStation Data AnalysisMSD ChemStation DA

G1701FA

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The Value of G1701FA SoftwareAll Inclusive G1701FA Software Package

• MassHunter GC/MS Acquisition

• MassHunter Quantitative Analysis

• MassHunter Qualitative Analysis

• MSD ChemStation Data Analysis

• 21CFR11 Compliance tools (Acquisition and MH Quantitative Analysis)

• GC/MS and LC/MS Translators

Collated User Information• Workflow guides, Video Tutorials, all in one

location

Support• 1yr Upgrade, Updates, and Phone Support• Training and Familiarization options

MSD ChemStation DA

MassHunter Qual

MassHunter Quant

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Other Powerful Software Tools

Target Deconvolution

- Lower limits of detection of target compounds in complex matrix

Unknown Analysis

- Quick screening, deconvolution and identification tool

Enviroquant

- Dedicated package for EPA regulated environmental analysis

Versatile Reporting Options

- Excel based reports- Powerful- User customizable templates

- Fast PDF Reports- Very fast report generation- Templates are not user customizable

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Migrate MSD ChemStation Data to MassHunter

Data

Data

Data

MassHunter Quant

MassHunter Qual

MSD ChemStation (.D)

WorkStation (.SMS)

Generic (.CDF)

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Migrate MSD ChemStation Quantitative Methods to MassHunter

MSD ChemStation (QDB.MTH)

WorkStation (.mth)

MassHunter Quant

Method

Method

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Data file review - Mass Hunter Quant Compounds-at-a-Glance

Review / compare multiple samples / compoundsin a fully customizable UI

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Quant ion EIC

Overlayed Quant EIC and Qualifier EICs

‘Head to Tail’ Deconvoluted component spectrum (top)

and reference library spectrum(bottom)

Expected RT

Recognition Window

EIC Window

Library Match Score from TD

Targeted Deconvolution Compound Information Mass Hunter Quant Batch at a Glance

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Example Mass Hunter TD Report

The Agilent 7010B Triple Quadrupole GC/MS SystemMore Ions Than Ever Before

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• Features a completely new EI source design –produces 20-30X more ions

• Instrument Detection Limit:0.5 fg OFN8X better than 7000D

• Joins the 7000D, the best selling GC/MS/MS system ever

New Features added to the 7000 Series InstrumentsDynamic MRM (dMRM)

Compound 1

Compound 2Compound

35 min.

6 min.

Compound 1

Compound 2

Compound 3

5 min.

6 min.

…Or…

dMRMTime Segment (TS)

• Create and edit methods more easily – no need to constantly change time segment boundaries• Obtain greater measurement efficiency – measure fewer compounds simultaneously; dwell

times automatically increase whenever possible• Continue to use existing TS-based methods, or convert them to dMRM at your own pace

Retention time

Retention window

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New Features added to the 7000 Series InstrumentsDynamic MRM (dMRM)

Select desired data rate here…

…dwell times automatically adjust here

Easily find and fix highly “congested”

spots by decreasing retention windows –Agilent RT locking makes it possible

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New Features added to the 7000 Series InstrumentsSIM/Scan: It’s Like Having Another Single Quad Whenever You Need One!

It’s this easy…

Simultaneous SIM/scan capability, of course!

SQ SIM table automatically recreated, so you measure the same compounds at the same time, with the same dwell times as on your SQ

Works for scan methods, too…

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The 7010B doesn’t just look different

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The 7010B doesn’t just look different

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Low ppb quantitation of Captan and Folpet!

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0

20

40

60

80

100

120

140

1601‐1

1‐2

1‐3

1‐4

1‐5

1‐6

5‐1

5‐2

5‐3

5‐4

5‐5

5‐6

10‐1

10‐2

10‐3

10‐4

10‐5

10‐6

50‐1

50‐2

50‐3

50‐4

50‐5

50‐6

Captan

Folpet100

1 ng/g 10 ng/g5 ng/g

%RSD captan =  12folpet =  10

%RSD captan =  11folpet =   5

%RSD captan =  7folpet =   2

50 ng/g

%RSD captan =  5folpet =  3

Individual Recoveries of Captan and Folpet Spiked in Celery, 2g sample with a 0.5 µL injection. Captan and folpet are base-sensitive compounds and often present issues in terms of recovery and precision.

The 7010B doesn’t just look different

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Sample Preparation Cost/Sample

CentrifugeTube

ACN Salts Internal Standards: Captan-d6, Folpet-d4

dSPEGeneral F&V or

Universal

Total Cost/Sample

Cost Savings

QuEChERS $0.43 $1.50 $2.96 $0.30 $1.32/$1.96 $6.51/$7.15 -

Mini-QuEChERS $0.42 $0.20 $0.80 $0.04 $1.32/$1.96 $2.78/$3.42 43% 48%

Cost Breakdown and Cost Savings for Sample Preparation with QuEChERS and Mini-QuEChERS Technique

LOQs for the majority of challenging pesticides in foods are 1 ng/g despite injecting lesssample from a smaller aliquot in order to improve method robustness. Cost savings arerealized through both scaled down sample prep and decreased instrument maintenance.This was made possible by using a miniaturized QuEChERS method and a High EfficiencySource for GC/MS/MS analysis.

Benefits of new design – ability to inject less!64 injections of a

QuEChERS extract of apple

2 µl 0.5 µl

• More “up time”• Fewer liner changes• Column lasts longer• Less source cleaning• Still get more sensitivity

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Easier sample prep Start with less sample Avoid Concentration step

Ship smaller samples from field to lab

Benefits of new design – ability to aliquot less!

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Benefits of new design – shorter dwell times!

• More transitions percompound

• Weaker transitionscan be used for betterselectivity

Ultra-short Dwell Times

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Benefits of new design – more transitions to choose from!

Propargite @ 0.5 ppb in Plum

+ MRM (135.0 -> 107.0) 0pt5ppb_PU_4-10-14_04.D Smooth

Acquisition Time (min)13.5 13.55 13.6 13.65 13.7

Cou

nts 5x10

1.9

2

2.1

2.2

2.3

2.4

2.5

2.6

2.7

2.8

2.9

3

3.1

3.2

3.3

3.4

3.5

3.6

3.7

13.559 min.

+ MRM (201.0 -> 137.0) 0pt5ppb_PU_4-10-14_04.D Smooth

Acquisition Time (min)13.5 13.55 13.6 13.65 13.7

Cou

nts 3x10

-0.05

0

0.05

0.1

0.15

0.2

0.25

0.3

0.35

0.4

0.45

0.5

0.55

0.6

0.65

0.7

0.75

0.8

0.85

0.9

0.95

1

1.05

1.1

13.575 min.

1.1%Area 3936

+ MRM (201.0 -> 137.0) FLAG_Inst1_PU_0pt5ppb_70…

Acquisition Time (min)13.5 13.55 13.6

1x10

-0.5-0.25

00.25

0.50.75

11.25

1.51.75

22.25

2.52.75

33.25

3.53.75

44.25

4.54.75

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13.566 min.

0.6%Area 102

7010 7000C2nd most abundant transition measured on:Quant transition

shows interference

Use of Alternate TransitionsBetter Selectivity Against Interferences

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Conclusions

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5977B• Improves performance with high sensitivity Extractor Ion Source – 1.5 fg OFN EI

specification• More ecological – reduce sample aliquot size to reduce consumption of solvents,

sample prep materials, disposal costs, etc. • MassHunter GC/MS Acquisition• MassHunter and MSD ChemStation data analysis OPTIONS! • Targeted Deconvolution

• 7000D• RoHS (Restriction of Hazardous Substances) compliance• Dynamic MRM• SIM/Scan mode

7010B• Improves performance with high efficiency source• 20 x increase in ion flux• 0.5 fg OFN EI specification• MassHunter Acquisition, Qualitative, and Quantitative