Clarus SQ 8 GC/MS. The NEW

Transcription

1 The NEW Clarus SQ 8 GC/MS Optimizing EPA Method 8270: PerkinElmer Clarus SQ8 Gas Chromatograph/Mass Spectrometer (GC/MS) Meeting the Challenges and Optimizing Results and Profitability Lee Marotta, Sr Field Application Scientist 2013 Perkin Elmer

2 2013 Perkin Elmer Hydrogen vs Helium

3 DFTPP in Hydrogen Passes Passes tuning criteria! 3

4 Passing Criteria All targets quant and qualifying ions were compared in hydrogen versus helium All other criteria were met 4

5 Reducing Sample Amount Why should we reduce sample amount for analysis? 2013 Perkin Elmer

6 Using 1mL instead of 1L sample delivers you more profits By enhancing productivity Elimination of concentration step increases throughput Able to use faster methods, such as SPE By reducing costs Save on expensive extraction solvent required for liquid/liquid extractions Save on precious refrigerator space and glassware Save on disposal costs of recovered solvents Save on shipping costs By increasing instrument uptime Injecting less sample matrix = cleaner system = more time running samples By delivering better performance Meeting required detection limits Enhancing recoveries Optimizing dynamic range use less solvent evaporate less solvent into environment a greener analysis

7 1 ml sample size (or 40mL) Perkin Elmer

8 1 liter liquid/liquid extraction: Disadvantages 1.0 liter of sample Extract with 300 ml dichloromethane Concentrate to 1mL Separate Phases Inject Disadvantages High costs (solvent, glassware, shipping) Requires more space Large containers Laborious sample prep Expensive Environmentally unfriendly

9 Enhance sample prep time and save on laboratory costs! 1mL sample volume (or 40mL) Easily meet DL requirement Extract with 1mL of DCM Separate phases Inject organic phase or use SPE Inject! Advantages: Reduced operating costs Requires less space (smaller containers) Significantly less solvent used Enhanced instrument uptime! Faster sample prep improves lab efficiency GREENER analysis!!!

10 Data and Injector Functions Perkin Elmer

11 PAH detection limits using 1mL extraction volume Injection Calibration Lowest Conc Volume Range Analyzed (DL) 1uL Full Scan 0.4 to 200 ppb 0.4 ppb 1uL SIM 0.2 to 200 ppb 0.2 ppb 5uL Full Scan 0.2 to 50 ppb 0.2 ppb 5uL Sim 0.06 to 50 ppb 0.06 ppb 10 ul Full Scan 0.08 to 50 ppb 0.08 ppb 50 ul Full Scan 0.02 to 50 ppb 0.02 ppb 11

12 2013 Perkin Elmer Why use controlled volatilization (solvent purge) injections instead of hot splitless injections?

13 Disadvantages to hot (flash-vaporizing) injections Potential thermal and catalytic breakdown Potential for backflash and condensation of High boiling components Hot zone Syringe fractionation Flash evaporation (expansion) Column Split Vent

14 Keeping your analytes in the liner: Potential backflash Backflash of analytes due to vapor expansion volume of solvent in hot injector exceeding the available volume of liner full injection will not make its way to column. Vapor (with sample) can enter pneumatics causing contamination requiring maintenance Affect Poor precision and recovery Condensation of high boiling components causing discrimination Carryover into later injections causing ghost peaks and poor performance

15 Why does this happen avoid Backflash Liner Volume Equation of a cylinder (Liner length)(π) r 2 Example for a 4cm x 2mm liner: (4cm)(0.2cm/2) 2 π Parameters to consider (V = nrt/p) Injector temperature Injection volume Injector pressure Solvents (have different expansion volumes) In this example, a 1µL injection of DCM at 10 psig and 250 o C expands to a 400µL vapor volume which exceeds the volume of the liner being used

16 Vapor Expansion: ex. Dichloromethane 1 ul injection volumes Effect of Pressure Advantages to Pressure Pulse reduce vapor expansion Pressure Pulse during injection V=nRT/P. Increase pressure reduces vapor expansion

17 Benefits of Controlled Volatilization Temperature programmed injections is superior than splitless pressure-pulsed (PP) better results! 2013 Perkin Elmer

18 Advantages of a Cold Injection Syringe Cold zone Sample introduced as a liquid onto glass wool (not flashed) Column Split Vent

19 Programmed Evaporation Takes Place after the Syringe is Removed Enhance recoveries by significantly minimizing high boiler condensation which is caused by backflash Enhance recoveries by reducing or preventing thermal and catalytic breakdown of thermally labile and active targets Eliminate problems associated with backflash Enhance accuracy by preventing discrimination caused By syringe fractionation Controlled Volatilization Column Split Vent

20 Do you want even better detection limits? The Technique of Solvent Purge with Enhanced Large Volume Injection for semi-volatile analysis Amount of matrix injected 1 liter sample extract concentrated to 1mL with a 1uL injection 1000x matrix injected 1mL sample with a 50uL injection 50x matrix injected (enhance instrument uptime) Reduce matrix into analytical system using 1 ml sample volume 2013 Perkin Elmer

21 Purge Pneumatics with Swafer Solvent Purge Step Temperature programmable (PSS) inlet Purge solvent while maintaining semi-volatiles in inlet Enables enhanced detection limits Prevents thermal breakdown and flashback (controlled volatilization) Split vent opened Swafer TM (micro channel switcher) Allows for the easy, automated control of effluent stream for many applications Inert For this application, it is used to isolate injector from column and detector 45 C deactivated fused silica (fs) S-Swafer Inlet pressure lower than Mid-point pressure during purge Mid-point pressure is greater than inlet pressure during purge Mass Spectrometer Elite-5 30m x 0.25mm x 0.25um

22 Injection Step Temperature programmable (PSS) inlet Purge solvent while maintaining semi-volatiles in inlet Enables enhanced detection limits Prevents thermal breakdown and flashback (controlled volatilization) Split vent closed 320 C Deactivated fused silica (fs) S-Swafer Inlet pressure higher than Mid-point pressure for injection Mid-point pressure is lower than inlet pressure during injection Mass Spectrometer Elite-5 30m x 0.25mm x 0.25um

23 Bake Step Temperature programmable (PSS) inlet Purge solvent while maintaining semi-volatiles in inlet Enables enhanced detection limits Prevents thermal breakdown and flashback (controlled volatilization) 450 C Split vent opened with faster flows deactivated fused silica (fs) S-Swafer Inlet pressure lower than Mid-point pressure during purge Mid-point pressure is greater than inlet pressure during purge Mass Spectrometer Elite-5 30m x 0.25mm x 0.25um

24 Full Scan/Single Ion Monitoring: Both Acquisitions in One Injection! Apr :45:45 PAH_040412_42 NR 100 % S/N:RMS= Pyrene (0.06 ppb) SIM mass 202 S/N: 1903 to 1 6: SIR of 1 Channel EI e3 0 PAH_040412_42 NR 100 S/N:RMS=67.02 Pyrene (0.06 ppb) 1: Scan EI e4 Full Scan mass 202 % S/N: 67 to Time

25 PAH detection limit results varying injection volume 0.4 ppb 0.2 ppb 0.2 ppb 0.06 ppb 0.08 ppb 0.02 ppb 1uL FS 1uL SIM 5uL FS 5uL SIM 10uL FS 50 ul FS Name r 2 S/N r 2 S/N r 2 S/N r 2 S/N r 2 S/N r 2 S/N 2-fluorobiphenyl (Sur) : : : : : : 1 p-terphenyl-d14 (Sur) : : : : : : 1 Napthalene : : : : : : 1 Acenapthalene : : : : 1** : : 1 Acenapthene : : : : : : 1 Fluorene : 1 n/a n/a : : : : 1 Phenanthrene : : : : : : 1 Anthracene : : : : : : 1 Fluoranthene : : : : : : 1 Pyrene : : : : : : 1 Benzo (a) anthracene : : : : : : 1 Chrysene : : : : : : 1 Benzo (b) fluoranthene : : : : : : 1 Benzo (k) fluoranthene : : : * 27 : : : 1 Benzo (a) pyrene n/a : : : : : 1 Indeno (1,2,3-cd) pyrene : : : * 67 : : : 1 Dibenzo (a,h) anthracene : : : * 62 : : : 1 Benzo (g,h.i) perylene : : : : : : 1 * removed lower level point from curve **0.2 point not 0.06 point 25

26 Pyrene Calibration from 0.06 to 50 ppb (10uL injection) SIM Extraction Volume: 1mL Concentration: 0.06 ppb Fluoranthene and Pyrene r 2 : Compound 14 name: Pyrene Coefficient of Determination: Calibration curve: * x Response type: Internal Std ( Ref 3 ), Area * ( IS Conc. / IS Area ) Curve type: Linear, Origin: Exclude, Weighting: 1/x, Axis trans: None 12.5, 05-Apr :45:45 Response Conc 26

27 7 level Calibration Full Scan processing from FS/SIM Acquisition Chlordane 0.2 ppb to 200 ppb Extraction Volume: 1mL Compound 8 name: Chlordane Coefficient of Determination: Calibration curve: * x Response type: External Std, Area Curve type: Linear, Origin: Exclude, Weighting: 1/x, Axis trans: None 7.00e6 File Name Std Conc Calc. % dev Result Pest_01603_ ppb std Pest_01603_07 2 ppb std Pest_01603_08 10 ppb std Pest_01603_09 20 ppb std Pest_01603_ ppb std Pest_01603_ ppb std Response -297 Conc

28 7 level Calibration SIM processing from FS/SIM Acquistion Aldrin 0.1 ppb to 200 ppb Extraction Volume: 1mL Compound 6 name: Aldrin Coefficient of Determination: Calibration curve: * x Response type: External Std, Area Curve type: Linear, Origin: Exclude, Weighting: 1/x, Axis trans: None 2.24e5 File Standard Area Result % dev Conc (PPB) Pest_01603_ ppb std Pest_01603_ ppb std Pest_01603_07 2 ppb std Pest_01603_08 10 ppb std Pest_01603_09 20 ppb std Pest_01603_ ppb std Pest_01603_ ppb std Response 0 Conc

29 Increasing Productivity, Efficiency and Performance Meet required reporting limits while using less sample New detector technology SIFI Larger injection volumes Inject less matrix cleaner system means enhanced instrument uptime increasing productivity Extract less sample reduce operating costs (less solvent, less glassware and less storage space required) Adds up to faster return on investment and a more productive laboratory with improved recoveries

30 Enhancing Instrument uptime Injecting less matrix Extending maintenance interval! Experiments performed at environmental testing lab 100mL injection volume Collected at an Environmental Testing lab in Shelton, CT 2013 Perkin Elmer

31 Results Comparing 1L to 100mL Detection limit achieved 10x improved over regulated detection limits for all targets More Clocks achieved than 1L extract because less matrix being injecting 1.0uL splitless injection _02 8: SIR of 6 Channels EI S/N:RMS= e4 % _02 1: Scan EI+ S/N:RMS= e5 % From Matrix spike Pyrene ppb 100mL extract conc to 5mL SIM FS Time

32 Getting more from your GC/MS! Enable lower detection limits! 2013 Perkin Elmer

33 Easy to Use and Maintain SMARTSource Now it is Plug and Play with a twist no wires to remove Change source components in under 5 minutes with no tools

34 Enhance Performance Enhance Uptime! Clarifi Detector Enhance Sensitivity Increase Operating Range More Flexibility Longer Life Less Downtime Enhance Library Matches most sensitive (improve detection limits) and robust (increase throughput)!

35 The Clarus SQ8 GC/MS Contact Information