氯苯类化合物空气采样管制备及其配套测定方法

Preparation of air sampling tube for chlorobenzene compounds and establishment of its matching detecting method

目的研制用于同时采集工作场所空气中12种氯苯类化合物(CBs)的GDH-2空气采样管,并建立配套的测定方法。方法自主研制GDH-2空气采样管,填充物为离子交换树脂和活性炭,质量配比为10∶1,以该采样管采集工作场所空气中蒸气态和气溶胶态共存的12种CBs,样品经甲苯洗脱,以DB-23毛细管色谱柱分离,微池电子捕获检测器测定。方法本方法定量测定范围为0.51×10^(-3)~6000.00 mg/L,相关系数均大于0.9994,最低检出浓度为0.02~61.99μg/m^(3),最低定量浓度为0.05~206.62μg/m^(3),平均洗脱效率为90.8%~104.0%,批内相对标准偏差(RSD)为1.0%~5.7%,批间RSD为3.0%~7.3%,样品在室温下可保存26 d以上。结论自主研制的GDH-2空气采样管及配套测定方法可用于工作场所空气中12种CBs的采集及测定。

Objective To prepare and develop a GDH-2 air sampling tube for detecting 12 kinds of chlorobenzenes(CBs) in workplace air and to establish a matching detecting method. Methods The self-developed GDH-2 air sampling tube was filled with ion exchange resin and activated carbon, and the mass ratio was 10 ∶1. The GDH-2 air sampling tube was used to collect 12 kinds of CBs with coexistence of gaseous and aerosol in the air. After elution with toluene, they were separated on a chromatographic column and determined by microcell electron capture detector. Results The quantitative detecting range of the method was 0.51×10^(-3)-6 000.00 mg/L, with the correlation coefficients greater than 0.999 4. The minimum detection concentration was 0.02-61.99 μg/m^(3), and the minimum quantitative concentration was 0.05-206.62 μg/m^(3). The average desorption efficiency was 90.8%-104.0%. The within-run relative standard deviation(RSD) was 1.0%-5.7%, and the between-run RSD was 3.0%-7.3%. The samples can be stored at room temperature for at least 26 days. Conclusion The self-developed GDH-2 air sampling tube and its matching measuring method can be used for the collection and determination of the 12 kinds of CBs in the air of workplace.