Headspace Analysis

Headspace analysis a means of separating the volatile material(s) from a liquid or solid prior to analysis by GC/MS.  As one of the leading materials analysis labs, Innovatech Labs uses two basic means of collecting the volatiles for materials testing:  Dynamic Headspace and Static Headspace. Dynamic headspace uses a "purge and trap" method to collect the sample on a sorbent material, then the sample is flushed onto the column for analysis by GC/MS.  In static headspace analysis, the sample is heated in a sealed environment and the gases are removed from the vial for analysis. For more information on the two types of sampling see the text below. 

Our experienced materials testing analysts can help you decide which technique is best suited for your application and help explain what the data means once it is collected.  To discuss your specific needs call us at (888) 740-LABS (5227) or by email.

Dynamic Headspace - DHS utilizes a "purge and trap" method to collect and concentrate outgassed materials for analysis by GC/MS.  In this method, the sample is purged with ultra pure nitrogen while being heated in a Teflon vessel.  As the nitrogen stream exits the vessel it passes through a thermal desorption tube filled with an adsorbent material.  The outgassed products are collected onto the adsorbent material.  Following the predetermined collection time, the tubes are transferred to a thermal desorption unit which is inline with the gas chromatograph and mass selective detector (GC/MS).

The thermal desorption unit heats the individual tubes while a flow of gas is applied through the tube.  The collected materials are flushed from the sorbent material and collected onto a cold trap within the thermal desorption unit.  After the entire sample has been purged from the sample tube and collected on the cold trap, the cold trap is heated rapidly.  The collected materials are then swept from the cold trap into the GC/MS for analysis as a volatile material. 

The typical sensitivity for compounds analyzed by DHS is nanogram per gram.

Static Headspace - In SHS, a liquid or solid sample is placed into a vial, sealed, and heated to a specific temperature.  All of the components that are volatile at or below the pre-set temperature escape from the sample to form a gaseous "headspace" above the sample.  The term "static headspace" refers to the sealed environment in which the outgassed products are collected.

After a certain period of time, the headspace gas is extracted from the vial and injected into a gas chromatograph which separates the various components of the sample based on size and/or polarity.  The separated components then go into a mass selective detector.  The resulting mass spectrum allows for the identification of the components using standard reference libraries.

Static headspace is an ideal choice for volatile compounds, such as residual solvents or low molecular weight additives. The sensitivity for static headspace is typically in the sub microgram range, however this is dependent on the volatility of the compounds.

Comparison of Good and Failed Epoxy

Analysis for Residual Solvents in a Powdered Drug

• Study compounds evolved during a 

  reaction

• Identify materials outgassed from a

  solid during heating

• Identify odor causing compounds

• Identify low boiling additives and

  contaminants in a product

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