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Analysis of Beverages using Large Volume Static Headspace / GCMS

Analysis of Beverages using Large Volume Static Headspace / GCMS Introduction to Large Volume Static Headspace (LVSH) Technique Advantages of LVSH/GC(MS) Analytical Procedure Examples of Beverages Analyzed Remote Headspace Analysis Summary Presentation Overview

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Analysis of Beverages using Large Volume Static Headspace / GCMS

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  1. Analysis of Beverages using Large Volume Static Headspace / GCMS

  2. Introduction to Large Volume Static Headspace (LVSH) Technique Advantages of LVSH/GC(MS) Analytical Procedure Examples of Beverages Analyzed Remote Headspace Analysis Summary Presentation Overview

  3. GC/MS Detection Limits vs Headspace Sample Volume 1000 100 10 1 0.1 0.01 10-3 10-4 10-5 Loop Preconcentration PPM LOD Vol vs Conc. 0.001 0.01 0.1 1.0 10 100 1000 MINIMUM VOLUME REQUIRED (CC)

  4. Large Volume Headspace Requires Preconcentration HP 5973 GCMS Volume Reduction Large Volume Inlet or Autosampler

  5. Introduces 10-200cc of headspace to the 7100 Preconcentrator Accommodates solids and liquids Detection limits 100x lower than conventional loop injection headspace “See what you can smell” Large Volume Static Headspace Autosampler

  6. LVSH Sample Platforms and Enclosures • Samples are placed in disposable vials, reducing potential for contamination of sample platforms. • Sample Platforms use quick connects, simplifying removal for oven bakeout.

  7. Advantages of Large Volume Static Headspace (LVSH) • Cleaner. No aerosols or foaming to contaminate sample transfer lines • Larger Sample Loading • Low detection limits without sample heating. • Less chance of producing artifacts. • Sample remains in natural state. • Ideal for kinetic / aging studies • Outgassing rates • Effects of Atmosphere and Storage Temperature • Better recovery of reactive compounds • Strong carbon based adsorbents are avoided • Inert, Silonite tubing used throughout • No sample fractionation (SPME)

  8. Food and Beverage Analysis by Large Volume Static Headspace (LVSH) / GCMS Analysis HP 5973 GCMS 7100 7032L 4600 7100 3-Stage Preconcentrator 7032L 21-Position LVSH/MiniCan Autosampler 4600 Multi-Channel Standards Diluter

  9. 7032-LVSH / 7100 /5973 Large Volume Static Headspace Analyzer M3 SL I/O SL I/O M2 6 M1 GC MS 7100 7032-LVSH

  10. 7100 Open Architecture Modular design. Easy replacement of traps MFC downstream of traps PCB Integrated wiring for improved reliability

  11. 7100 Heated Flow Path • Silonite tubing used throughout. • Complete heating of sample flow path. Easily accessed for trap and tubing replacement. • External Heaters outside each cryotrap 7100 Preconcentrator

  12. SiloniteTM Fused Silica Lined Tubing

  13. Less adsorption of Diethylbenzene on Silonite tubing. No deactivation needed. Faster sample equilibration with tubing surface. Less potential for carryover. Silonite Tubing VOC Adsorption/Absorption Study R E S P O N S E Silonite Brand B Deact. Brand B Flush Time (Min.)

  14. 7100 Water and CO2 Management Techniques MFC PUMP Removing Water and CO2 CO2 Helium Carrier Helium To GC H2O VOCs Focuser Glass Beads Tenax Sample Internal Standard Calibration Standard Cryogen in

  15. 3-Stage Flexibility for GCMS Analysis of Multiple Sample Types and Matrices Sample Type Mode Trap1 Trap2 Trap 3 - On-column focuser for capillary GC/MS

  16. Improper Water Management 400cc VOC STD, Full Scan 15-270 amu

  17. Vinyl Chloride 100x Calibration Curve usingVariable Volume / Single Standard Calibration

  18. Fast Injection and Proper Water Management Minimizes Tailing of Polar VOCs Column: HP1, 60m, 0.32mm ID, 1um film. Flow rate: 1.5 ccm Carrier: He

  19. Multiple Preconcentration Options Depending on Target Compounds and Matrix (CO2, ETOH) Reduced Temperature Trapping Minimizes Sample Stress, Maximizing Recovery of Thermally Labile Flavor and Odor Compounds Silonite Tubing Creates an Extremely Inert Sample Flow Path to Further Improve Recovery Demonstrated Recovery of Sulfur and Nitrogen Compounds Advantages of 7100 Multi-Stage Preconcentration

  20. LVSH Analysis of Yuban Coffee - 100cc

  21. 100cc LVSH - Coke/Pepsi Challenge Coke Pepsi

  22. Apple Juice by LVSH / GCMS TreeTop Apple Juice 100cc, LVSH 60m, HP1, 0.32mm ID, 1um 7032LVSH/7100/5973

  23. Beer by LVSH/GCMS Beer, ETOH Removed 200cc, LVSH 60m, HP1, 0.32mm ID, 1um 7032LVSH/7100/5973

  24. Beer by LVSH/GCMS Beer, ETOH Removed Front End, Post ETOH 200cc, LVSH 60m, HP1, 0.32mm ID, 1um 7032LVSH/7100/5973 1 1 Acetone 2. Ethyl Formate 3. Dimethyl Sulfide 4. Propanol 3 2 4

  25. Beer Light Ends by LVSH/GCMS Beer, ETOH M1 Retained Cold Trap Dehydration Light Ends 200cc, LVSH 60m, HP1, 0.32mm ID, 1um 7032LVSH/7100/5973

  26. Beer Light Ends by LVSH/GCMS Beer, ETOH M1 Retained Cold Trap Dehydration Light Ends 200cc, LVSH 60m, HP1, 0.32mm ID, 1um 7032LVSH/7100/5973 Acetaldehyde COS

  27. 2% Milk by LVSH/GCMS 2% Milk 100cc, LVSH 60m, HP1, 0.32mm ID, 1um 7032LVSH/7100/5973

  28. 2% Milk by LVSH/GCMS 2% Milk 100cc, LVSH 60m, HP1, 0.32mm ID, 1um 7032LVSH/7100/5973 Dimethyl Sulfide

  29. Collection of Remote Headspace Samples Improves Monitoring Effeciency. MiniCan Samplers are SiloniteTM Coated to reduce surface losses. Monitor Process Streams, Holding Tanks, Reactors, etc. MiniCan Samplers Allow Direct Sampling of Gas Phase Flavors and Odor Compounds

  30. Four Models of MiniCans MC400 MC400L MC400S MC400V

  31. Gas Phase Analysis Using MiniCan Silonite Coated Samplers 7032 Autosampler Surrogate Spiking

  32. 5973/7100/7032 200cc Injection10 PPB Sulfur Std., ECTD 5 1. CO2 2. H2S 3. COS 4. MeSH 5. DMS 6. CS2 6 4 3 1 2

  33. 2-Day Stability Study of Sulfur Compounds in Fused Silica Lined vs Electropolished Canisters 7000 / HP5973 Data

  34. 5-PointSulfur Gas Calibrations H2S DMS CS2 MeSH

  35. Support for R&D and QA • Fully Characterize Products down to Olfactory Detection Limits • Identify Good and Bad “Markers” in product or packaging • Monitoring on-line (Sequence Looping) • Monitoring at-line (Sampling Ports) • Solids, Liquids by LVSH • Gases by MiniCan Samplers

  36. Large Volume Static Headspace (LVSH) is a new analytical tool available to food and beverage Chemists which enhances the detection of headspace components using GC and GCMS analysis. Maintaining the sample in a more natural state allows the analysis of “normally occurring” odor and flavor compounds. Inert flow paths and reduced temperature trapping increases the range of analytes that can be recovered, including oxygen, nitrogen, and sulfur containing compounds. Conclusion

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