Resolve Your Search for More Ions: The 5977B, 7000D, and 7010B GC/MS Instruments. Stephan Baumann ASTS Talk November, 2016

Transcription

1 Resolve Your Search for More Ions: The 5977B, 7000D, and 7010B GC/MS Instruments Stephan Baumann ASTS Talk November,

2 The Most Powerful EI GC/MS Source Ever Made. More intense electron beam NEW! 5977B High Efficiency Source X Longer path length for electron beam/effluent interaction = Up to 30x More Ions Produced 5977A Extractor Source 5977B High Efficiency Source with Magnet Removed 2

3 The Most Powerful EI GC/MS Source Ever Made. How the HES works High emission filaments for more electron current Powerful cylindrical magnet collimates electrons Long path length for ionization 3

4 The Most Powerful EI GC/MS Source Ever Made. These values must be met at instrument install 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 IDL fg OFN IDL 5977B 4

5 In a ultra low noise environment A small noise variation creates a big SNR variation 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: 8 OFN runs Area Noise Minimum (for each value) Maximum (for each value) Average (for each value) SNR (Height/noise) % RSD 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. 5

6 Detection Limit as Defined by Basic Statistics DL = t * SD where DL t 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 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 6

7 Calculating IDL (Instrument Detection Level) on a 5977A t α, n-1 value for 99% confidence level and 8 injection is SD 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 (area) = 2.988* SD (area) %RSD Average area count represents 100fg injected amount IDL 100fg IDL 7

8 But Wait Even More Innovation Outcome JetClean self-cleaning ion source technology Reduces cleaning up to 80%. Run more samples! 8

9 But Wait The Proof is in the Pudding! Dramatic visual JetClean demonstration JetClean Easily removed Sharpie marks Prevents deposits that would require manual cleaning 9

10 But Wait Even More Innovation with Intuvo 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 10

11 Reimagine What Can Be Done with Single Quad GC/MS Extremely Low Limits of Detection Rock Solid Precision Exceptional Science -- Analyze and Identify Trace Compounds Previously Unseen with Single Quad GC/MS 10 fg OFN injections LOD = 0.57 fg calculated from 8 consecutive injections Overlay of 8 injections of 2pg of pyrene: Do more with Less Sample Achieve today s analytical sensitivity using a fraction of the sample Minimized Environmental Impact 11

12 Benefits That Touch Your Entire Operation Decreased Shipping Costs Less Frequent Liner Maintenance Decreased Storage Costs Longer Column Life 1 Liter 100 ml Decreased Disposal Costs Faster Sample Prep 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 12

13 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 13

14 Agilent s Programmable Inlet MultiMode Inlet (MMI) 7890 standard pneumatics 7890 turn-top Uses 7890 S/SL liners, septa and o-rings 7890 standard capillary fitting 14

15 Multimode Inlet Features Hardware Temperature range of -160C to 450C 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 15

16 Backflush to remove non-volatile residues 16

17 MassHunter GC/MS Acquisition for GC/MSD Unified GC/MS Acquisition and MassHunter Data Analysis; with MSD ChemStation workflow for GC/MSD 17

18 GC/MSD Software MassHunter Qual MH MassHunter Quant CS MassHunter GC/MS Acquisition MSD ChemStation DA And Use Either MassHunter Data Analysis OR MSD ChemStation Data Analysis G1701FA 18

19 The Value of G1701FA Software All 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 MassHunter Qual MSD ChemStation DA Collated User Information Workflow guides, Video Tutorials, all in one location MassHunter Quant Support 1yr Upgrade, Updates, and Phone Support Training and Familiarization options 19

20 Other Powerful Software Tools Target Deconvolution - Lower limits of detection of target compounds in complex matrix Unknown Analysis - Quick screening, deconvolution and identification tool Versatile Reporting Options - Excel based reports - Powerful - User customizable templates - Fast PDF Reports - Very fast report generation - Templates are not user customizable Enviroquant - Dedicated package for EPA regulated environmental analysis 20

21 Migrate MSD ChemStation Data to MassHunter Data MassHunter Quant MSD ChemStation (.D) Data MassHunter Qual WorkStation (.SMS) Data Generic (.CDF) 21

22 Migrate MSD ChemStation Quantitative Methods to MassHunter MassHunter Quant Method MSD ChemStation (QDB.MTH) Method WorkStation (.mth) 22

23 Data file review - Mass Hunter Quant Compounds-at-a-Glance Review / compare multiple samples / compounds in a fully customizable UI 23

24 Targeted Deconvolution Compound Information Mass Hunter Quant Batch at a Glance Library Match Score from TD Quant ion EIC Expected RT Recognition Window EIC Window Overlayed Quant EIC and Qualifier EICs Head to Tail Deconvoluted component spectrum (top) and reference library spectrum (bottom) 24

25 Example Mass Hunter TD Report 25

26 The Agilent 7010B Triple Quadrupole GC/MS System More Ions Than Ever Before Features a completely new EI source design produces 20-30X more ions Instrument Detection Limit: 0.5 fg OFN 8X better than 7000D Joins the 7000D, the best selling GC/MS/MS system ever 26

27 New Features added to the 7000 Series Instruments Dynamic MRM (dmrm) Retention time Compound 1 Compound 2 Or Compound 1 Compound Retention window Compound 3 2 Compound 3 5 min. Time Segment (TS) 6 min. 5 min. dmrm 6 min. 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 27

28 New Features added to the 7000 Series Instruments Dynamic MRM (dmrm) Easily find and fix highly congested spots by decreasing retention windows Agilent RT locking makes it possible Select desired data rate here dwell times automatically adjust here 28

29 New Features added to the 7000 Series Instruments SIM/Scan: It s Like Having Another Single Quad Whenever You Need One! It s this easy 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 Simultaneous SIM/scan capability, of course! 29

30 The 7010B doesn t just look different 30

31 The 7010B doesn t just look different 31

32 Low ppb quantitation of Captan and Folpet! 1 ng/g 5 ng/g 10 ng/g 50 ng/g 160 %RSD captan = 12 folpet = 10 %RSD captan = 11 folpet = 5 %RSD captan = 7 folpet = 2 %RSD captan = 5 folpet = Captan Folpet 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. 32

33 The 7010B doesn t just look different Cost Breakdown and Cost Savings for Sample Preparation with QuEChERS and Mini-QuEChERS Technique Sample Preparation Cost/Sample Centrifuge Tube ACN Salts Internal Standards: Captan-d6, Folpet-d4 dspe General F&V or Universal Total Cost/ Sample Cost Savings QuEChERS $0.43 $1.50 $2.96 $0.30 $1.32/$1.96 $6.51/$ Mini-QuEChERS $0.42 $0.20 $0.80 $0.04 $1.32/$1.96 $2.78/$ % 48% LOQs for the majority of challenging pesticides in foods are 1 ng/g despite injecting less sample from a smaller aliquot in order to improve method robustness. Cost savings are realized through both scaled down sample prep and decreased instrument maintenance. This was made possible by using a miniaturized QuEChERS method and a High Efficiency Source for GC/MS/MS analysis. 33

34 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 34

35 Benefits of new design ability to aliquot less! Easier sample prep Start with less sample Avoid Concentration step Ship smaller samples from field to lab 35

36 Benefits of new design shorter dwell times! Ultra-short Dwell Times More transitions per compound Weaker transitions can be used for better selectivity 36

37 Benefits of new design more transitions to choose from! Use of Alternate Transitions Better Selectivity Against Interferences Quant transition shows interference 2 nd most abundant transition measured on: C + MRM ( > 107.0) 0pt5ppb_PU_ _04.D Smooth x10 5 Counts min Acquisition Time (min) + MRM ( > 137.0) 0pt5ppb_PU_ _04.D Smooth x min. Counts Acquisition Time (min) 0.5 ppb in Plum 1.1% Area MRM ( > 137.0) FLAG_Inst1_PU_0pt5ppb_70 x min Acquisition Time (min) 0.6% Area

38 Conclusions 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 38