1. hit “esc” to quit hit any key to continue Analysis of Beverages using Large Volume Static Headspace / GCMS

2. hit “esc” to quit hit any key to continue Presentation Overview Introduction to Large Volume Static Headspace (LVSH) Technique Advantages of LVSH/GC(MS) Analytical Procedure Examples of Beverages Analyzed Remote Headspace Analysis Summary

3. hit “esc” to quit hit any key to continue GC/MS Detection Limits vs Headspace Sample Volume 0.001 0.01 0.1 1.0 10 100 1000 1000 100 10 1 0.1 0.01 10-3 10-4 10-5 PPM LODPPM LOD MINIMUM VOLUME REQUIRED (CC) Vol vs Conc. LoopPreconcentration

4. hit “esc” to quit hit any key to continue Large Volume Headspace Requires Preconcentration HP 5973 GCMS Volume ReductionLarge Volume Inlet or Autosampler

5. hit “esc” to quit hit any key to continue Large Volume Static Headspace Autosampler 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”

6. hit “esc” to quit hit any key to continue 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. hit “esc” to quit hit any key to continue 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. hit “esc” to quit hit any key to continue 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. hit “esc” to quit hit any key to continue 7032-LVSH / 7100 /5973 Large Volume Static Headspace Analyzer GC MS 6 71007032-LVSH SL I/O M1 M2 M3

10. hit “esc” to quit hit any key to continue PCB Integrated wiring for improved reliability Modular design. Easy replacement of traps MFC downstream of traps 7100 Open Architecture

11. hit “esc” to quit hit any key to continue Silonite tubing used throughout. Complete heating of sample flow path. Easily accessed for trap and tubing replacement. External Heaters outside each cryotrap 7100 Heated Flow Path 7100 Preconcentrator

12. hit “esc” to quit hit any key to continue Silonite TM Fused Silica Lined Tubing

13. hit “esc” to quit hit any key to continue Silonite Tubing VOC Adsorption/Absorption Study Less adsorption of Diethylbenzene on Silonite tubing. No deactivation needed. Faster sample equilibration with tubing surface. Less potential for carryover. RESPONSERESPONSE Flush Time (Min.) Silonite Brand B Deact. Brand B

14. hit “esc” to quit hit any key to continue Internal Standard Calibration Standard Glass BeadsTenax Cryogen in CO2 Focuser To GC VOCs 7100 Water and CO2 Management Techniques H2O Helium PUMPMFC Helium Carrier Removing Water and CO2 Sample

15. hit “esc” to quit hit any key to continue 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. hit “esc” to quit hit any key to continue Improper Water Management 400cc VOC STD, Full Scan 15-270 amu

17. hit “esc” to quit hit any key to continue Vinyl Chloride 100x Calibration Curve using Variable Volume / Single Standard Calibration

18. hit “esc” to quit hit any key to continue 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. hit “esc” to quit hit any key to continue Advantages of 7100 Multi-Stage Preconcentration 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

20. hit “esc” to quit hit any key to continue LVSH Analysis of Yuban Coffee - 100cc

21. hit “esc” to quit hit any key to continue 100cc LVSH - Coke/Pepsi Challenge Coke Pepsi

22. hit “esc” to quit hit any key to continue TreeTop Apple Juice 100cc, LVSH 60m, HP1, 0.32mm ID, 1um 7032LVSH/7100/5973 Apple Juice by LVSH / GCMS

23. hit “esc” to quit hit any key to continue Beer by LVSH/GCMS Beer, ETOH Removed 200cc, LVSH 60m, HP1, 0.32mm ID, 1um 7032LVSH/7100/5973

24. hit “esc” to quit hit any key to continue Beer by LVSH/GCMS Beer, ETOH Removed Front End, Post ETOH 200cc, LVSH 60m, HP1, 0.32mm ID, 1um 7032LVSH/7100/5973 1 2 3 4 1 Acetone 2. Ethyl Formate 3. Dimethyl Sulfide 4. Propanol

25. hit “esc” to quit hit any key to continue 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. hit “esc” to quit hit any key to continue 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. hit “esc” to quit hit any key to continue 2% Milk by LVSH/GCMS 2% Milk 100cc, LVSH 60m, HP1, 0.32mm ID, 1um 7032LVSH/7100/5973

28. hit “esc” to quit hit any key to continue 2% Milk 100cc, LVSH 60m, HP1, 0.32mm ID, 1um 7032LVSH/7100/5973 Dimethyl Sulfide 2% Milk by LVSH/GCMS

29. hit “esc” to quit hit any key to continue MiniCan Samplers Allow Direct Sampling of Gas Phase Flavors and Odor Compounds Collection of Remote Headspace Samples Improves Monitoring Effeciency. MiniCan Samplers are Silonite TM Coated to reduce surface losses. Monitor Process Streams, Holding Tanks, Reactors, etc.

30. hit “esc” to quit hit any key to continue Four Models of MiniCans MC400 MC400L MC400S MC400V

31. hit “esc” to quit hit any key to continue 7032 Autosampler Gas Phase Analysis Using MiniCan Silonite Coated Samplers Surrogate Spiking

32. hit “esc” to quit hit any key to continue 5973/7100/7032 200cc Injection 10 PPB Sulfur Std., ECTD 1 2 3 4 6 5 1. CO2 2. H2S 3. COS 4. MeSH 5. DMS 6. CS2

33. hit “esc” to quit hit any key to continue 2-Day Stability Study of Sulfur Compounds in Fused Silica Lined vs Electropolished Canisters 7000 / HP5973 Data

34. hit “esc” to quit hit any key to continue 5-Point Sulfur Gas Calibrations H2S MeSH CS2 DMS

35. hit “esc” to quit hit any key to continue 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. hit “esc” to quit hit any key to continue Conclusion 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.