Click to Open Selection Guide of Sorbent Pen Headspace Techniques
LabelVaseR-VaseF-VaseFeveLVSH

LABEL

VASE

Rapid-VASE

Flash-VASE

FEVE

LVSH/X-LVSH

Full Name
Vacuum Assisted Sorbent Extraction
Matrix Accelerated VASE
Flash-VASE
Full Evaporative Vacuum Extraction
(Extremely) Large Volume Static Headspace
Sorbent Pen Type
HSP
HSP
FSP
FSP
ASP
Vial Size
20, 40, 125mL
20mL
2, 6, 20, 40mL
2, 6 mL
250, 500, 1000mL
When to Use
Liquid or Solid Sample Compositional Analysis. SPME Alternative
Faster VASE Technique. Multi-sample automation on SPR40A using 2 Pens
Samples with low volatile contents (solids, powders, Cannabis, packaging, oils)
Volatile Matrix with low solid contents (water, beverages, solvent extracts)
Measurement of equilibrated headspace to determine partition coefficients of aroma compounds.
Extraction Technique
Vacuum, Diffusive, Closed System, Mechanical Agitation
Vacuum, Matrix Accelerated, Diffusive Closed System, Convective Agitation
Diffusive Vacuum Thermal Extraction, Closed System
Matrix Evaporative Transfer followed by Diffusive Extraction in Open System. Matrix eliminated
Dynamic, Fully equilibrated headspace, Static, Open System
Vial Temp Range
30° to 70° C
30° to 100° C
30° to 280° C
30° to 280° C
30° to 70° C
BP Range
-50° to 450° C
-50° to 450° C
-50° to 550° C
80° to 550° C
0° to 450° C
Water Management
Cold tray dehyd., Dry Purge, Split Inj.
Cold tray dehyd., Dry Purge, Split Inj.
Cold tray dehyd., Dry Purge, Split Inj.
Vacuum Removal, Dry Purge
Dry Purge, Split
Typical Pen Cycle Times
200-2000
200-2000
500-2000
500-2000
100-200 (except not for disposible / replaceable inlet filter)
Competitive Technologies Displaced
SPME, SPME Arrow, SPE, SBS
SPME / SPME Arrow, DHS
Micro Chamber, Direct Thermal Extraction, DHS
SBSE when in low dissolved solids / volatile matrix
All other non-static, low sensitivity techniques
Typical Sorbent Combinations
Tenax, Tenax / CPX, PDMS GB / Tenax, Tenax / Carboxen
Tenax, Tenax / CPX, PDMS GB / Tenax, Tenax / Carboxen
Tenax, Tenax / CPX, PDMS GB / Tenax, Tenax / Carboxen
PDMS / Tenax, Tenax / CPX
PDMS / Tenax, Tenax / Carbopack X
Common Applications
Food, Beverage, Flavor, Aroma, Water, Soil, Consumer Products
Non-Equilibrium VASE where online extraction and analysis is required.
Volatiles / Odors in Packaging, Polymers, Powders, Foams, Synthetics, Natural Products, Heavy Oils
SVOCs in Water, Flavors / Aromas in Thermally Labile samples, Pesticides in foods.
Aroma / Flavor Profiling

Definitions:

Open System - Unretained compounds/gases allowed to pass through sorbent for removal by pump/vacuum.

Closed System - Completely isolated during extraction, so breakthrough of even the lightest compounds isn't possible. Allows recovery of wider boiling point range.

The LVSH6 solution from Entech is a next generation Large Volume Static Headspace (LVSH) technique that uses the SPR40 autosampler to carefully and quantitatively transfer the equilibrated  headspace above a liquid or solid sample through an ASP Sorbent Pen in order to measure the composition of the equilibrated headspace. This equilibrated headspace is what a consumer experiences when they open a container of facial cream, or open a food package, or even when they apply a fragrance to their skin. Virtually all other headspace techniques perform extractions,  leaving the fixed gases behind (air, nitrogen, etc), or they add more fixed gases to the headspace to flush compounds to an external sorbent, but in both cases the equilibrium is disturbed which ends up providing a compositional analysis of the liquid or solid sample, not what a consumer would be smelling. Stated another way, if a SPME extraction of a typical 10mL vial were to be  performed over a 10-20 minute period to try to improve the sensitivity of the method, and then this fiber were desorbed into another inert container so that all compounds would be in the gas  phase, the resulting aroma will almost certainly be different than what was present in the original, equilibrated headspace. As long as headspace is pulled from the container without being replaced  by additional gases, the equilibrium that has been set up at a given temperature will not be affected very much, especially if we only collect about half of the volume of the vial. With a 1L  vial where 900cc is headspace, that would be 450-500cc of fully equilibrated headspace, and when using a splitless injection technique, this could provide low to even sub part per trillion detection  limits on some GCMS analyzers. This provides aroma/flavor/fragrance chemists with a whole new approach for “seeing what their customers are smelling”. Knowing the composition in the liquid or  solid is only half the challenge. Unless the partition coefficient for each compounds in each matrix is known ( an near impossible task), the headspace at equilibrium must also be determined  experimentally. That is what LVSH offers. Therefore, VASE to measure the composition of the liquid or solid samples, and LVSH to measure the equilibrated headspace concentrations. The LVSH6  module along with the volume measurement capabilities of the SPR-FM add on module makes the entire process automated for six 1L vials.

LVSH - Technique Selection Guide

Sample Type: Liquids/Solids/Consumer Products

Extraction Temperatures: 30° – 60° C

Operational Mode: Large Volume Static Headspace

BP Range: -50° C to >450° C

Vial Sizes: 1Liter

Typical Mode: Split, Splitless VOC Thru SVOC

Water Management: Hydrophobic Media, Split injection

Mode 1: Non-Heated, Fully Static LVSH

LVSH jars with ASP Pens are placed into the 6 position tray, and a volume from 10 – 500 cc of headspace are slowly drawn through each ASP Pen. Pens are isolated for GCMS analysis

Mode 2: Heated, Fully Static LVS

LVSH jars with ASP Pens are placed into the LVSH6 tray, and a transport tool is used to move the vials to a heated oven for a period of time, followed by drawing 10-500cc of headspace through the ASP Pens. Pens are isolated for GCMS Analysis

Mode 3: Vacuum Equilibration / N2 Pulsed LVSH

LVSH jars with sample and ASP Pens are placed into a freezer to minimize volatiles presence in the headspace, then the headspace is evacuated through a separate port in the lid, followed by  placement of samples under vacuum in the LVSH6 tray. Vial assemblies are moved to the heater for vacuum equilibration where equilibration will be reached far faster under vacuum than at  atmospheric pressure. Afterwards, samples are pressurized with UHP Nitrogen, followed by ASP extraction of 10-500cc of sample. Pens are isolated for GCMS analysis.

Mode 4: Vacuum Equilibration / X-LVSH Extraction

Extremely Large Volume Static Headspace (X-LVSH). Similar to Mode 3, except the UHP N2 Fill Tool remains connected to the sample vial during very slow sampling through the ASP, so N2 enters at the  same rate as the flow through the ASP (2-10cc/min). N2 is introduced near the bottom of the vial, while ASP samples near the top, so introduced N2 has time to fully equilibrate with the headspace  prior to collection through ASP. Sample volumes 100-2000cc.

LVSH6 Modules


Click to open parts list




Image (click to enlarge) Part # Description Unit link to product
4lvsh-slider LVSH6 Large Volume Static Headspace Platform and Heater, 120VAC/60Hz EA
4lvsh-slider LVSH6-HV Large Volume Static Headspace Platform and Heater, 240VAC/50Hz EA

LVSH6 Kits

Click to open parts list




Image (click to enlarge) Part # Description Unit link to product
SP-HS-V1L 1L Vial + Lid/Cap/Seal for Sorbent Pen Extraction EA

LVHS6 Vials


Click to open parts list




Image (click to enlarge) Part # Description Unit link to product
39-75500W_500w 39-75500W 500mL LVSH6 Vial Caps not included 12pk
39-76850HS.2 39-76850HS Vial Caps for 500mL vials (high temp) 12pk Product Page
HS-760500.1 HS-76050 Silonite™ Liners for 500mL vials 12pk Product Page
39-75L1W.2 39-75L1W 1L LVSH6 Vials 12pk Product Page
39-76894HS.2 39-76894HS Vials Caps for 1L vials (high temp) 12pk Product Page
HS-761000.2 HS-761000 Silonite™ Liners for 1L vials 12pk Product Page
SP-L100S.2 SP-L100S Lid Bushing Sorbent Pen Interface 12pk Product Page

Extraction Controller

Click to open parts list




Image (click to enlarge) Part # Description Unit link to product
SPR-EMC-VASE Controls MA-VASE10, 3700, and LVSH6 modules, 120VAC/60Hz EA
SPR-EMC-VASE-HV Controls MA-VASE10, 3700, and LVSH6 modules, 240VAC/50Hz EA
LVHS-chocolate-header
Chocolate by Large Volume Headspace Extraction
LVHS-Garlic-header
Garlic by Large Volume Headspace Extraction
LVHS-honey-header
Honey by Vacuum Assisted Sorbent Extraction
LVHS-Pale-Ale-header
Pale Ale by Large Volume Headspace Extraction
LVHS-pink-rose-header
Pink Rose by Large Volume Headspace Extraction
LVHS-Rum-1-header
Rum 1 by Large Volume Headspace Extraction
LVHS-Rum-2-header
Rum 2 by Large Volume Headspace Extraction
LVHS-Rum-3-header
Rum 3 by Large Volume Headspace Extraction
LVHS-pickle-header
Pickle by Large Volume Headspace Extraction
LVHS-sliced-orange-header
Sliced Orange by Large Volume Headspace Extraction
LVHS-white-rose-header
White Rose by Vacuum Assisted Sorbent Extraction
LVHS-whole-orange-header-1
Whole Orange by Large Volume Headspace Extraction
LVHS-dry-formula-header
Dry Baby Formula by Large Volume Headspace Extraction
LVHS-formula-header-1
Baby Formula by Large Volume Headspace Extraction
A Cleaner, More Sensitive Approach to EPA Method 8260 Using Large Volume Static Headspace and Active SPME Preconcentration Prior to GCMS Analysis

Accurate Monitoring of Sulfur Compounds in Silonite® Fused Silica Lined Canisters Utilizing a New Approach for Water Removal During Field Sampling

Please complete the form to download the LVSH Technical Information Document or to request a system quote.