A multiple headspace extraction capillary gas chromatographic (MHE-CGC) method for the quantitative, accurate, and rapid determination of volatile components in solids such as polymers, resins, and activated carbon has been developed. A five-step MHE determination was performed using the Agilent 7694 headspace sampler and a 5890 Series II GC with EPC. A Microsoft® Excel spreadsheet was used to quickly perform the required calculations. Details of the procedure and implications affecting the analysis of polymeric materials are discussed.
This document presents a Multiple Headspace Extraction (MHE) capillary gas chromatography (CGC) method for the quantitative determination of volatile components in solid matrices such as polymers, resins, and activated carbon. The method addresses challenges associated with direct injection, such as sample decomposition and system contamination, by analyzing the gas phase over the solid sample.
The procedure utilizes an Agilent 7694 headspace sampler interfaced with a 5890 Series II GC with electronic pressure control (EPC) and a flame ionization detector (FID). The note details the experimental conditions, including instrument configuration, and discusses the use of an Excel spreadsheet for calculating analyte concentrations based on semilogarithmic plots of peak areas versus extraction number.
| Gas chromatograph | 5890 Series II |
|---|---|
| Column | HP-5, 25-m x 0.32 mm x 1.0 pm |
| Detector | FID |
| Sample introduction | 7694 headspace sampler |
| Extractions/vial | 5 |
| Puncture | 0=S 1=M |
| Oven Program | 40°C, hold for 5 min; ramp to 250°C at a rate of 20° Cimin; hold for 5 minutes. |
A multiple headspace extraction capillary gas chromatographic (MHE-CGC) method is used.
The experiments used a 7694 headspace sampler interfaced to a 5890 Series II GC with electronic pressure control (EPC) and a flame ionization detector (FID).
Concentration is calculated using a Microsoft Excel spreadsheet that performs statistics for the semilogarithmic plot, correlation coefficients, slopes, total peak areas, and analyte concentration.
The correlation coefficient for the sample should be 0.99 or better to ensure thermal equilibrium was established.