a023000deb746731e9eb6c4cfe92d574.ppt
- Количество слайдов: 40
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 • Enviro. Lab 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 m. L/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 m. L/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 m. L/min vs 1 m. L/min • Increase capacity of stationary – No fronting of peak shape for 160 ng/u. L PNA • Decrease the irreversible absorption of active species – Pentachlorophenol < 10%RSD • (5 -160 ng/u. L) • 0. 1 ng/u. L MDL – replicates at 1 ng/u. L 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 m. L/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) 13
NDMA and Pyridine Splitless 14
Two Methods: Splitless and Split 15
TRACE Ultra DSQ II GC/MS 16
Source materials and geometry • New Dura. Brite. TM 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 Dyna. Max XR Ion Detection System SGE ETP AF 635 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 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 (5 ng to 160 ng min >0. 05) 2, 4 -dinitrophenol 4 -nitrophenol 0. 19 hexachlorocyclopentadiene 0. 212 N-nitroso-di-n-propylamine 21 0. 11 0. 688
CCCs < 30% RSD for Initial Calibration Curve BNAs Acids %RSD 1, 4 -dichlorobenzene 2. 2 2, 4 -dichlorophenol 8. 6 acenaphthene 1. 6 7. 1 4 -chloro-3 methylphenol 2 -chlorophenol 3. 9 benzo(a)pyrene Di-n-octylphthalate 14 pentachlorophenol 9. 1 diphenylamine 1. 9 phenol 4. 7 fluoranthene 3. 8 2, 4, 6 -trichlorophenol 11 hexachlorobutadiene 22 %RSD 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/u. L 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 (2 gr sediment/2 m. L methylene chloride + 25 u. L diesel fuel) 24
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 – Enviro. Lab 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
8270 C/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
tw So f t Ki ar e Redefining the Way We Look at GC/MS Hardware Productivity Solutions target routine GC/MS applications to offer value to the customer 33
Enviro. Lab Forms v 2. 0 High Throughput Quantification
Enviro. Lab 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
Enviro. Lab 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


