Transcript Slide 1
Introducing the DSQII Terry Jeffers Agenda • Update on Thermo’s Environmental Initiatives • Discussion on new approaches to the challenges of 8270 • Introducing Thermo Electrons Productivity Kits • EnviroLab Forms 2.0 – High Throughput Quatification • New application note: Rapid Analysis of 8270 2 Thermo Electron: Environmental Initiative • Focus on Environmental Laboratory needs: – Requirement for Productivity – Need for good work flow in Generating, Reviewing and Reporting data – Benefit from guides for operation, maintenance and troubleshooting specific Methodologies 3 Thermo Electron: Environmental Initiative Product Sales Specialist Environmental Demo Chemist Environmental Seed Chemist New hardware: DSQ II Productivity Kits: 8270 and 525 8260 and 524 4 * Pitt Falls for Method 8270 Those little things that stop everything Activity in the GC/MS system • Activity – These sites can be everywhere • Injector, column, source • SPCC compounds are used to show good system – Nitrophenols are some of the best compounds to find active sites • Minimizing Effects of Activity – Deactivated liners – Good column that shows no active sites – High flow rates to reduce the residence time of any active compound. – Balance temperature zones to reduce activity and thermal break down. 6 Chromatography How important is it really? GC and Autosampler • Separations accomplished with slow chromatography – Common GC methods for 8270 • • • • • Fast injection 250 - 300 0 C injector temperature 1 mL/min flow rate 30 m x 0.25 mm ID column Oven ramps between 5 0 and 10 0 C/min from 35 0 to 300 0 C • Separations accomplished with fast chromatography – Alternate GC method for 8270 • • • • • 8 Hot needle injection 250 0 C injector temperature 3 mL/min flow rate 30 m x 0.25 mm ID x 0.5 µm column Oven stepped ramps to provide the critical pair separations. Hot Needle Injection: Run at Lower Inlet Temperature: Fewer Replacements of Liner 9 Increase the Mobile Phase: 3 mL/min vs 1mL/min • Increase capacity of stationary – No fronting of peak shape for 160 ng/uL PNA • Decrease the irreversible absorption of active species – Pentachlorophenol < 10%RSD • (5-160 ng/uL) • 0.1 ng/uL MDL – replicates at 1 ng/uL 4.7%RSD – Minimal breakdown for endrin or 4,4-DDT • Provide Gaussian shape peaks for the most volatile – No solvent skewing of NDMA and pyridine • Shorter run times: 17 minutes 10 Effects of increased flow rates • Why increase the flow rate to 3.0 mL/min – Learned from applications developed for the analysis of explosives. – Decrease the residence time of the compounds in potential active areas. – Decreases the run time without higher temperatures that could potentially damage thermally labile compounds. – Do not need to expose the column to higher temperatures that will damage it. – Provides better separations and narrower peak widths. – This is balanced with a 20:1 split flow ratio. 11 Injection: Choice of Liner 12 PNAs ( 5 ng and 160 ng) RT: 17.32 - 18.34 RT: 17.45 AA: 1357507 BP: 276.1 100 NL: 4.27E5 m/z= 275.5276.5 F: MS ICIS 031706_b_0 03 RT: 18.05 AA: 1192699 BP: 276.1 80 60 40 20 0 100 RT: 17.47 AA: 38042327 BP: 276.1 NL: 1.14E7 m/z= 275.5276.5 F: MS ICIS 031706_b_0 08 RT: 18.07 AA: 32375912 BP: 276.1 80 60 40 20 0 17.4 13 17.5 17.6 17.7 17.8 17.9 Time (min) 18.0 18.1 18.2 18.3 NDMA and Pyridine RT: 1.71 - 5.17 Split 100 80 4.94 5.05 NL: 3.81 3.19 2.46 1.79E8 TIC F: MS C07 60 4.10 4.45 2.42 40 3.29 20 2.71 3.12 0 100 3.62 3.44 3.97 4.13 4.50 4.84 4.99 Splitless 80 60 4.87 40 20 4.52 0 2.0 14 2.5 3.0 3.5 Time (min) 4.0 4.5 5.0 NL: 8.09E6 TIC F: MS A07 Two Methods: Splitless and Split RT: 0.00 - 30.08 5.85 100 9.50 80 12.89 8.92 8.72 60 40 5.05 NL: 5.80E8 TIC F: MS C07 13.53 14.74 5.40 15.18 17.10 20 17.87 19.87 21.84 0 100 NL: 1.37E8 TIC F: MS A07 9.42 80 8.10 60 8.22 7.49 40 12.12 11.32 7.34 13.34 14.74 15.10 15.82 6.37 6.90 4.87 20 17.41 18.73 22.26 25.26 26.19 0 0 15 5 10 15 Time (min) 20 25 30 TRACE Ultra DSQ II GC/MS 16 Source materials and geometry • New DuraBriteTM Source Open Geometry – Passive Collector • Extends Dynamic Range • Improves Robustness – Optional Closed EI Ion Volume • Constructed of new proprietary material for enhanced inertness • Protects Lens 1 from ion burn 17 New DynaMax XR Ion Detection System SGE ETP AF635 Electron Multiplier • Detector linear range output current >30µA • Simple snap out replacement of multiplier assembly 18 New Linear/Log Hybrid Electrometer • Extends output current to 70µA • Provides dynamic range to >106 • No loss of response or precision at the lower sample/analyte levels Expected Results Results I can get, you can get them too. Calibration Curve • First page of the calibration curve report • All SPCC and CCC requirements met • Average of all RSD calibration curves of 7.46% 20 SPCCs (5ng to 160 ng min >0.05) 21 2,4-dinitrophenol 0.11 4-nitrophenol 0.19 hexachlorocyclopentadiene 0.212 N-nitroso-di-n-propylamine 0.688 CCCs < 30% RSD for Initial Calibration Curve 22 BNAs %RSD Acids %RSD 1,4-dichlorobenzene 2.2 2,4-dichlorophenol 8.6 acenaphthene 1.6 3.9 benzo(a)pyrene 7.1 4-chloro-3methylphenol 2-chlorophenol Di-n-octylphthalate 14 pentachlorophenol 9.1 diphenylamine 1.9 phenol 4.7 fluoranthene 3.8 2,4,6-trichlorophenol 11 hexachlorobutadiene 2.6 2-nitrophenol 8.5 5.1 Quantitated Data File • First page of the Quantitation Report • This shows the quantitation of the 20 ng/uL sample for the calibration curve • Meets the requirements of the internal standards and surrogates • Meets all ion ratio requirements • No manual integrations were required 23 Robustness: Split (2gr sediment/2mL methylene chloride + 25 uL diesel fuel) RT: 0.00 - 17.11 8.33 100 7.77 90 Relative Abundance 9.36 9.83 7.18 80 70 10.28 10.71 6.53 5.01 5.82 60 NL: 1.08E9 TIC F: MS rep96 8.87 11.12 4.04 50 11.51 40 30 11.90 2.34 3.97 12.26 20 12.61 12.96 1.40 1.70 10 14.00 14.87 0 0 2 4 6 8 Time (min) 10 12 2.5000 2.0000 1.5000 1.0000 0.5000 0.0000 1 3 5 7 9 11 13 15 17 19 21 23 25 24 14 16 Phenol(CCC) 2% 1,4-Dichlorobenzene(CCC) 1% 2-Nitrophenol(CCC) 2% 2,4-Dichlorophenol(CCC) 1% Hexachlorobutadiene(CCC) 2% 4-Chloro-3-methylphenol(CCC) 2% 2,4,6-Trichlorophenol(CCC) 1 % Acenaphthene(CCC) 1% Pentachlorobenzene(CCC) 2% Diphenylamine(CCC) 2% Pentachlorophenol(CCC) 2% Fluoranthene(CCC) 2% Di-n-octylphthalate(CCC) 3% Benzo(a)pyrene(CCC) 1% How can we prove it Productivity Solutions Productivity Solutions Integrating the DSQ II with Software, Methods, and Consumables to Get Productive, Quickly Productivity Solutions • Provide all of the necessary material to run the method – Proven Thermo Column – Deactivated Liners – Standards • Snap and shoot – prediluted for entire method validation – All other consumables for about 2 weeks • Provide all of the software – EnviroLab Forms 2.0 – Interactive Reference CD • All of the methods, sequences, – Validation data used to generate all of what you see here and in the manuals • Two Boxes full of materials, manuals, and CD’s. 27 Productivity Kit • SOP manual for method • How to Guide • Quick Start Guide • Provide consumables for running method – Standards, liners, septa, syringes, column,… • Instrument method, processing method, reporting package • CD deliverable – SOP – Data from method validation – Instrument method – Processing method – Reporting software with templates 28 Pieces of the Productivity Kit 29 Quick Start Guide 30 8270C/D Productivity Solution • Customer’s system can be taken from installation sign off to method IDL’s in as little as 2 days! • 8270 is a value added product which will sell for ~ $3000 US • Add on service provided by Thermo FSE’s • US Field Service Engineers are being trained on the 8270 PS • Kits serve as a great tool for training aides for the lab 31 Productivity Solutions are a Win-Win • Good for customers – – Improves overall experience – Increases satisfaction – Eases transition to Thermo GC/MS – Gives optimal performance for the DSQ II • Good for Thermo – Easy to support these solutions Helps the customer and support by establishing a known set of criteria to achieve success. Address the new lab environment less highly skilled users with higher throughput requirements 32 Redefining the Way We Look at GC/MS Hardware Productivity Solutions target routine GC/MS applications to offer value to the customer 33 EnviroLab Forms v 2.0 High Throughput Quantification EnviroLab Forms v 2.0 • An entirely new data processing and reporting system running as a layer over Xcalibur 1.4 • While targeted towards environmental laboratories and applications, it has been shown to be valuable for any laboratory performing high-throughput quantification • Adds a significant complement of capabilities that Xcalibur – Ion ratio calculations • Peak integration • Reporting – Integrated data review and reporting • No more batch reprocessing to re-generate reports of edited results – Fully automated while still allowing sophisticated manual review 35 Data Review 36 Report View 37 EnviroLab Forms v 2.0 • Brand new workflow oriented user interface • Substantially improved ion ratio review and editing support • Comprehensive set of textual and graphical reports • Fully automated, fully manual or any combination in between • Can be used as a high-throughput quantification engine for any application – Simply turn off or don’t use those options which aren’t relevant for a given user 38 Conclusion • The DSQ II system provides updates to hardware and software that make it easy to use • The Productivity Solution for method 8270 provides a method that has been validated across multiple DSQ II systems. • All of this allows a new operator to be productive immediately • The proven changes to the method allow an increased amount of productivity and throughput for the analyst and the laboratory. 39 •Questions? Thank You 40