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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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Presentation Transcript
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

Presentation Overview
gc ms detection limits vs headspace sample volume
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)

large volume headspace requires preconcentration
Large Volume Headspace Requires Preconcentration

HP 5973 GCMS Volume Reduction

Large Volume

Inlet or Autosampler

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”

Large Volume Static Headspace Autosampler
slide6

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.
slide7

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)
slide8

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

slide9

7032-LVSH / 7100 /5973

Large Volume Static Headspace Analyzer

M3

SL I/O

SL I/O

M2

6

M1

GC

MS

7100

7032-LVSH

slide10

7100 Open Architecture

Modular design.

Easy replacement of traps

MFC downstream of traps

PCB Integrated wiring for improved reliability

slide11

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

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.

Silonite Tubing VOC Adsorption/Absorption Study

R

E

S

P

O

N

S

E

Silonite

Brand B

Deact. Brand B

Flush Time (Min.)

slide14

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

3 stage flexibility for gcms analysis of multiple sample types and matrices
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

slide16

Improper Water Management

400cc VOC STD, Full Scan 15-270 amu

slide18

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

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

Advantages of 7100 Multi-Stage Preconcentration
slide22

Apple Juice by LVSH / GCMS

TreeTop Apple Juice

100cc, LVSH

60m, HP1, 0.32mm ID, 1um

7032LVSH/7100/5973

slide23

Beer by LVSH/GCMS

Beer, ETOH Removed

200cc, LVSH

60m, HP1, 0.32mm ID, 1um

7032LVSH/7100/5973

slide24

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

slide25

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

slide26

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

slide27

2% Milk by LVSH/GCMS

2% Milk

100cc, LVSH

60m, HP1, 0.32mm ID, 1um

7032LVSH/7100/5973

slide28

2% Milk by LVSH/GCMS

2% Milk

100cc, LVSH

60m, HP1, 0.32mm ID, 1um

7032LVSH/7100/5973

Dimethyl Sulfide

minican samplers allow direct sampling of gas phase flavors and odor compounds
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
slide30

Four Models of MiniCans

MC400 MC400L MC400S MC400V

slide32

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

slide33

2-Day Stability Study of Sulfur Compounds in

Fused Silica Lined vs Electropolished Canisters

7000 / HP5973 Data

slide35

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
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.

Conclusion