Occupational Hygiene Department, Chemical Agents Laboratory, Italian Workers' Compensation Authority (INAIL)-Research Area, Rome, Italy.
Anal Bioanal Chem. 2013 Jan;405(2-3):961-76. doi: 10.1007/s00216-012-6379-7. Epub 2012 Sep 12.
A desorption study of 57 volatile organic compounds (VOCs) has been conducted by use of accelerated solvent extraction (ASE) and gas chromatography-mass spectrometry. Different solvents were tested to extract activated charcoal tubes with the objective of replacing carbon disulfide, used in official methods, because of its highly toxic health and environmental effects. Extraction conditions, for example temperature and number of cycles, were investigated and optimized. The definitive extraction procedure selected was use of acetone at 150 °C and two consecutive extraction cycles at a pressure of 1,500 psi. Considering a sample volume of 0.005 Nm(3), corresponding to a sampling time of 8 h at a flow rate of 0.01 L min(-1), the method was validated over the concentration range 65-26,300 μg Nm(-3). The lowest limit of quantification was 6 μg Nm(-3), and recovery for the 93 % of analytes ranged from 65 to 102 %. For most of the compounds, relative standard deviations were less than 15 % for inter and intra-day precision. Uncertainty of measurement was also determined: the relative expanded uncertainty was always below 29.6 %, except for dichlorodifluoromethane. This work shows that use of friendlier solvent, for example acetone, coupled with use of ASE, can replace use of CS(2) for chemical removal of VOCs from activated charcoal. ASE has several advantages over traditional solvent-extraction methods, including shorter extraction time, minimum sample manipulation, high reproducibility, and less extraction discrimination. No loss of sensitivity occurs and there is also a salutary effect on bench workers' health and on the smell of laboratory air.
采用加速溶剂萃取(ASE)和气相色谱-质谱联用技术对 57 种挥发性有机化合物(VOCs)进行了解吸研究。测试了不同的溶剂,以提取活性碳管,目的是取代因其具有高度毒性的健康和环境影响而在官方方法中使用的二硫化碳。研究并优化了萃取条件,例如温度和循环次数。选择的最终萃取程序是在 150°C 下使用丙酮,并在 1500psi 的压力下进行两个连续的萃取循环。考虑到样品体积为 0.005Nm(3),相应的采样时间为 8 小时,流速为 0.01Lmin(-1),该方法在 65-26300μgNm(-3)的浓度范围内进行了验证。最低定量下限为 6μgNm(-3),93%的分析物的回收率在 65-102%之间。对于大多数化合物,日内和日间精密度的相对标准偏差小于 15%。还确定了测量不确定度:相对扩展不确定度始终低于 29.6%,除二氯二氟甲烷外。这项工作表明,使用更友好的溶剂(例如丙酮),结合使用 ASE,可以替代 CS(2)用于从活性碳中化学去除 VOCs。ASE 与传统溶剂萃取方法相比具有多个优点,包括萃取时间更短、样品处理最少、重现性高、萃取歧视性低。不会降低灵敏度,对实验员的健康和实验室空气的气味也有有益的影响。