Elke K, Jermann E, Begerow J, Dunemann L
Medizinisches Institut für Umwelthygiene, Department of Analytical Chemistry, Düsseldorf, Germany.
J Chromatogr A. 1998 Nov 27;826(2):191-200. doi: 10.1016/s0021-9673(98)00736-5.
An improved analytical method for passive air sampling is presented based on a combination of commercially available diffusive samplers with headspace solid-phase microextraction and high-resolution gas chromatography with flame ionization detection (HRGC-FID). This procedure is targeted for short-term BTEX (benzene, toluene, ethylbenzene and o-, m- and p-xylenes) determinations at environmental concentrations and can be applied for sampling intervals between 30 min and 24 h. The analytes are adsorbed onto the charcoal pad of a passive sampler and then extracted with carbon disulphide-methanol. After removal of the carbon disulphide by xanthation, the BTEXs are enriched on a Carboxen SPME fiber, thermally desorbed and analysed by HRGC-FID. Detection limits for a sampling interval of 2 h are between 0.4 and 2 micrograms/m3, within-series precision ranges between 6.6 and 12.8%, day-to-day precision is between 11.1 and 15.2%. The results obtained with this procedure are validated by comparison with active sampling. Detection limits and a further reduction of the sampling time are limited by blanks of the chemicals and the diffusive samplers. Procedures to eliminate these blanks are described in detail. Applications such as the determination of BTEXs in indoor air inside buildings, inside a train and a car are presented, indicating the usefulness of the described procedure for short-term measurements of environmental BTEX concentrations. An advantage of passive samplers is the storage stability for at least six months, which is essential for its use in large epidemiological studies.
基于市售扩散采样器与顶空固相微萃取以及带火焰离子化检测的高分辨率气相色谱法(HRGC-FID)的结合,提出了一种改进的被动空气采样分析方法。该方法旨在测定环境浓度下的短期BTEX(苯、甲苯、乙苯以及邻二甲苯、间二甲苯和对二甲苯),适用于30分钟至24小时的采样间隔。分析物吸附在被动采样器的活性炭垫上,然后用二硫化碳 - 甲醇进行萃取。通过黄原酸化去除二硫化碳后,BTEX在Carboxen SPME纤维上富集,热解吸并通过HRGC-FID进行分析。2小时采样间隔的检测限在0.4至2微克/立方米之间,系列内精密度范围在6.6%至12.8%之间,日间精密度在11.1%至15.2%之间。通过与主动采样进行比较,验证了该方法获得的结果。检测限以及采样时间的进一步缩短受到化学物质和扩散采样器空白的限制。详细描述了消除这些空白的程序。介绍了该方法在建筑物内室内空气、火车和汽车内BTEX测定等方面的应用,表明该方法对于环境BTEX浓度的短期测量是有用的。被动采样器的一个优点是至少六个月的储存稳定性,这对于其在大型流行病学研究中的应用至关重要。