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