期刊
JOURNAL OF CHROMATOGRAPHY A
卷 1137, 期 1, 页码 15-21出版社
ELSEVIER SCIENCE BV
DOI: 10.1016/j.chroma.2006.10.016
关键词
bituminous emulsion sealants; aromatic hydrocarbons; BTEX; headspace; solid-phase microextraction
The possibility of quantitative determination of aromatic hydrocarbons in bituminous emulsion sealants was investigated using headspace solid-phase microextraction (HS-SPME) followed by gas chromatography-mass spectrometry (GC-MS). The target analytes studied were benzene, toluene, ethylbenzene, p-, m-, and o-xylene (BTEX) as well as 1,3,5- and 1,2,4-trimethylbenzene. Experimental factors influencing HS-SPME efficiency were studied (sample-headspace equilibration time, extraction time and sample matrix effects). A HS-SPME method using surrogate matrix was developed. The detection limit was estimated as approximately 0.1 ppmw for the target analytes investigated. Good linearity was observed (R-2 > 0.997) for all calibration curves obtained. The repeatability of the method (RSD, relative standard deviation) was found less than 10%. The accuracy of the method given by recovery of spiked samples was between 99 and 116%. The HS-SPME method developed was applied to two commercially available bituminous emulsion sealants. External calibration and standard addition approaches were investigated, and statistical paired t-test was performed. The contents of target aromatic hydrocarbons in the sealants studied varied from approximately 0.4 to 150 ppmw. The method developed shows potential as a tool for the determination of aromatic hydrocarbons in emulsified bituminous materials. (c) 2006 Elsevier B.V. All rights reserved.
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