内标法测定工作场所空气中的三甲基苯  

Determination of trimethyl benzen in workplace air by internal standard method

作　　者：陶雪[1] 刘晓东[1] 宋利群[2] 

机构地区：[1]中国疾病预防控制中心职业卫生与中毒控制所,北京100050 [2]山东省职业卫生与职业病防治研究院,山东济南250062

出　　处：《中国卫生检验杂志》2015年第22期3817-3819,3824,共4页Chinese Journal of Health Laboratory Technology

基　　金：卫生标准制(修)订项目(20140705);卫生部行业公益项目(201402021)

摘　　要：目的建立灵敏、准确的气相色谱内标法测定工作场所空气中三甲基苯的方法。方法工作场所空气中的三甲基苯用活性炭管进行采集,样品用二硫化碳解吸,己基苯作为内标,用FFAP毛细管柱进行分离,气相色谱-火焰离子化检测器进行检测,以保留时间定性,以样品和内标物的峰面积的比值进行定量。结果 3种异构体的浓度为0μg/ml^900μg/ml时,检出限为0.009μg/ml^0.034μg/ml,定量限为0.013μg/ml^0.046μg/ml,批内精密度分别为2.09%~2.71%、2.03%~2.54%、1.96%~2.41%,批间精密度分别为4.21%~5.05%、4.28%~4.91%、4.39%~4.79%,解吸率分别为97%~102%、95%~98%、90%~94%,采样率为100%,穿透容量>22 mg,冷藏或室温可放置7 d。结论内标法测定空气中三甲基苯的方法准确易行,方法性能指标符合《职业卫生标准制定指南第4部分工作场所空气中化学物质测定方法》中相关指标的要求。Objective To establish a gas chromgraphy method for the determination of trimethyl benzen in workplace air by in- ternal standard method. Methods Trimethyl benzens in the air were collected by drawing a known volume of air through a charcoal tube. Samples are desorbed with carbon disulfide and analyzed by gas chromatography with FFAP capillary column. Gas chromatography flame ionization detector was used to detect in order to preserve the time, and the ratio of the sample and the peak area of the internal standard was quantified. Results The concentration ranged from 0 μg/ml to 900 μg/ml. The limit of detection was among 0. 009 μg/ml - 0.034 μg/ml. The limit of quantification was among 0.013 μg/ml - 0.046 μg/ml. The precision within batch was respectively 2.09% - 2.71%, 2.03% - 2.54%, 1.96% - 2.41%, while, that among batches were respectively 4.21% -5.05%, 4.28% -4.91% , 4.39% -4.79%, and the desorption efficiency was 97% - 102%, 95% -98%, 90% -94%. The average sampling efficiency was 100%. Samples could store 7 days at ambient temperature or refrigeration, breakthrough capacity was above 22 mg. Conclusion The method of internal standard method for determination of three methyl benzene in air is accurate and feasible, and the performance index is in line with the requirements of relevant in- dicators in the workplace air, according to Occupational Hygienic Standard Setting Guidelines for the Fourth Part of Workplace Air Determination of Chemical Substances.

关 键 词：三甲基苯 气相色谱法 内标法 

分 类 号：O657.71[理学—分析化学]