Heated Purge and Trap Method Development and Testing
Lucas, SV; Burkholder, HM
| HERO ID | 2116798 |
|---|---|
| In Press | No |
| Year | 1988 |
| Title | Heated Purge and Trap Method Development and Testing |
| Authors | Lucas, SV; Burkholder, HM |
| Abstract | A heated purge-trap-desorb (H-PTD) analysis method for polar, water soluble volatile organic analytes was developed and tested. The research goal was to obtain analysis sensitivities for the target analytes comparable to those achieved presently for non-polar analytes using the room temperature PTD approach of EPA SW-846 Method 5030 while at the same time not deviating significantly from the type of apparatus currently in use for Method 5030. Thirty-three polar, water soluble analytes from Appendix VIII and the Michigan list were included in the scope of work. Eight analytes proved to be amenable to the developed method: acrolein, methyl ethyl ketone, methylacrylonitrile, acrylonitrile, acetonitrile, propionitrile, 1,4-dioxane and isobutanol. The gas chromatography-mass spectrometry (GC-MS) method detection limits for the analytes ranged from 2 to 9 micrograms/L and were about 5-fold higher than would be obtainable with more optimized chromatography. Three alcohols, propargyl alcohol, 2-chloroethanol and 1,3-dichloro-2-propanol could not be recovered to any degree by H-PTD even using 80% saturation of the sample with salts and dramatically increased purge gas volumes. One analyte, 3-chloroproprionitrile, could not be recovered from the trap desorption step, even though it was shown to be only slightly hydrolytically unstable. The other 21 analytes had plausible chemical reasons for the absence of any H-PTD recovery for them: nine were nitrogen bases, six were hydrolytically unstable, two were mercaptans and four had very low volatility and/or very high water solubility. The absolute H-PTD recoveries obtained ranged from about 80% for analytes such as acrylonitrile and methylacrylonitrile to about 30% for 1 ,4-dioxane. The developed method employs a standard 5-ml purge vessel with an integral, very small volume water cooled condenser and the same all-Tenax trap as specified in Method 5030 for use in Method 8030. Commercially available PTD apparatus can be used without modification except to accommodate the 90 C water bath used to heat the purged sample. (Author 's abstract) |
| Is Certified Translation | No |
| Dupe Override | No |
| Comments | Journal: ISSN: |
| Is Public | Yes |
| Keyword | Gas chromatography; Chloropropionitrile; Alcohol; Water analysis; Organic compounds; Isobutanol; Dioxane; Acrolein; Propionitrile; Methyl ethyl ketone; Pollutant identification; Mass spectrometry; Methylacrylonitrile; Acetonitrile; Acrylonitrile; Chemical analysis |