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Next Generation of Dual Data Acquisition for High Sample Throughput of Dioxins

Next Generation of Dual Data Acquisition for High Sample Throughput of Dioxins. April 2013 Heinz Mehlmann. Overview. Theoretical background of the Dual Data Option. Improvement on the Hardware. Background. Dual Data Acquisition is based on a double GC HRMS System. first peak (tcdf).

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Next Generation of Dual Data Acquisition for High Sample Throughput of Dioxins

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  1. Next Generation of Dual Data Acquisition for High Sample Throughput of Dioxins April 2013 Heinz Mehlmann

  2. Overview • Theoretical background of the Dual Data Option. • Improvement on the Hardware.

  3. Background • Dual Data Acquisition is based on a double GC HRMS System

  4. first peak (tcdf) last peak (ocdd) Background • The first and last peak of a chromatogram defines the time section of analytical intrest. section of analytical interest wasted time wasted time Chromatogram of a typical Dioxin run on a 60 meter column

  5. Background • Sequence timescale in normal mode (no Dual Data) No benefit in terms of timesaving Dual GC-MS system Single GC-MS system sample 2 sample 3 sample 1 GC 1 GC 2

  6. sample 1 sample 3 waiting Time waiting Time sample 2 waiting Time sample 1 sample 5 sample 3 GC 1 sample 6 sample 4 sample 2 GC 2 Background Sequence timescale in normal mode GC 1 GC 2 Sequence timescale with DUAL DATAAquisition.

  7. Background • Continuous Dataflow

  8. Background • The injection on GC 2 is performed during the aquisition of GC 1 and vice versa. GC1 GC2

  9. Injector swiching valves to MS analytical column T-connector Background • Dynamic Flow Switching System • A staggert injection can only be realised with a hardware based modification in each GC.

  10. The column-flow is directed into the MS. The column-flow is directed into the service vacuum and He compensates the flow into the ionsource. Background • Functioin of the Dynamic Flow Switching System

  11. Background • Functioin of the Dynamic Flow Switching System

  12. Background • Functioin of the Dynamic Flow Switching System

  13. Background Time Timing GC 1 GC 2 GC 1 GC 1 GC 2

  14. Dual Data 2nd Generation Focus regarding the Redesign of the Dual Data Option: • Robustness • Ease of use • Maintenance • Performance

  15. Dual Data 2nd Generation Improvement on the Hardware • Optimization of all restrictions. • Purging the He line between regulator and switching valve. • Using a high quality 3-Way valve in the He makeup gas line. • Implementing a MCD wafer instead of T-pieces in the oven. • Reducing the column connections from four to two. • Using finger tight siltite ferrules® for column connection ® by SGE

  16. He Injector Vacuum Transfereline T-Connector Analytical Column Dual Data 2nd Generation • First version of the Dual Data Hardware

  17. Dual Data 2nd Generation • In case of micro leaks, Air can accumulate in the He Line when the line is closed for a longer time. • Closing the He line (with a leak) over night and reopen it again. He Vacuum N2 Dosing valve Injector O2 Switching valves Column Ar to MS

  18. Dual Data 2nd Generation • Purging the He line during the Off position via a 3-Way switching valve doesn’t allow any air accumulation. • Closing the He line (with a leak) over night and then opened. He Vacuum N2 Dosing valve Injector 3-Way Purge Line O2 Switching valves Column Ar to MS

  19. He Injector Vacuum Transfereline T-Connector Analytical Column Dual Data 2nd Generation • Redesign of the components in the GC oven

  20. Dual Data 2nd Generation • All connections inside the oven are implemented in one single MCD (Multi Chanel Device)® Ø 25mm ® by SGE

  21. Dual Data 2nd Generation • Both T-connections and the restriction in-between are inside the wafer. Vacuum He Column in Ø 25mm Column out

  22. Dual Data 2nd Generation • Dead volume leads to tailing in the chromatography • No dead volume in the T-connection of the wafer • Reproducible conditions (restrictions) MCD Old Hardware

  23. Dual Data 2nd Generation • Separation (CS3WT diluted): Chromatogram direct vs. via Wafer • Column direct into the MS • Column via the Wafer TCDD

  24. Dual Data 2nd Generation • Only two column connection. He Vacuum Column in Column out MCD

  25. Dual Data 2nd Generation • The ferrule is pre-mounted with a fingertite tool® that determines the distances between column and ferrule. • Columns with ID 0.25 mm and ID 0.32 mm are supported. ® by SGE

  26. Dual Data 2nd Generation • The prepared column is then mounted to the MCD® again with a fingertite tool®. ® by SGE

  27. Dual Data 2nd Generation

  28. Dual Data 2nd Generation • Data from Beta Test Site 5Cl-PCB

  29. Dual Data 2nd Generation Customer feedback • 1.200 injections have been made (80 % real samples, 20 % standards and blanks) without any maintenance on the wafer. • There had been no problems neither with the wafers themselves nor with a leakage. • Dual Data with the wafers is now one of the best options of a DFS for a laboratory with a high throughput of similar samples.

  30. Dual Data 2nd Generation • Customer Case Study http://pops.thermo-bremen.com

  31. Dual Data 2nd Generation Dual Data Acquisition

  32. Acknowledgement • KayteParlevliet and R&D team Australia • DetlefGrzelak Hamburg Germany

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