塑料生产物流场所空气中邻苯二甲酸酯的气相色谱-质谱测定法

Determination and status quo survey of phathalic acid esters in air of plastic production logistics by GC-MS

目的建立塑料生产物流场所空气中邻苯二甲酸酯类增塑剂(PAEs)的气相色谱-质谱(GC-MS)测定方法,并应用该方法进行职业环境中PAEs污染现状调查。方法按照《工作场所空气中毒物检测方法的研制规范》建立测定方法,采用该方法测定现场采集的样品以进行现状调查。结果6种PAEs在2～1000ng/ml范围内均呈线性关系(以采集3L空气样品计,相当于空气中浓度为0.67～333μg/m3);检出限均低于1ng/ml,相当于空气中最低检出浓度均低于0.33μg/m3;分别以相对标准偏差和回收率计,日内精密度和准确度分别为3.0%～7.8%和93.1%～105.1%,日间精密度和准确度分别为3.4%～9.9%和93.4%～106.4%;解吸效率为92.9%～97.9%;采样效率为约100%;穿透容量大于1.4mg;样品在室温下可稳定保存7天;选择性良好。现场调查结果显示,塑料生产物流场所空气中PAEs的污染情况尚不严重,职业接触工人中也未见明显临床症状与体征。结论GC-MS法灵敏度高、线性范围宽、精密度和准确度好,可用于塑料生产物流场所空气中PAEs的测定。

Objective To establish GC-MS method for the determination of phathalic acid esters （PAEs） in the air of plastic production logistics,and conduct a status quo survey of PAEs pollution in occupational environments basing on it.Methods The determination method was established according to the Monitor Investigating Guidelines on Poisons in Workplace Air,and then used to determine samples collected to carry out an on-the-spot investigation.Results Calibration curves of the six PAEs were proved to be all linear in the range of 2-1000ng/ml,equivalent to 0.67-333μg/m^3 in the air considering 3 L air sample was collected.The sensitivities were high with all limits of detection lower than 1ng/ml,i.e.,the minimum detectable concentrations of the six PAEs were all lower than 0.33μg/m^3.Intra-day precision and accuracies were all good,with relative standard deviation in the range of 3.0%-7.8% and recoveries in the range of 93.1%-105.1% respectively.And inter-day precision and accuracies were 3.4%-9.9% and 93.4%-106.4% correspondingly.The eluting efficiency was 92.9%-97.9%,and the sampling efficiencies were nearly 100%.The breakthrough capacities were all larger than 1.4 mg.And samples could be stored stably at room temperature for 7 days.The selectivity of this method was good.Results of status quo survey indicated that the PAEs pollution in the air of plastic production logistics was not serious,and no obvious clinical symptoms and signs were found in those occupationally-exposed workers.Conclusion This method meets the demand of the Monitor Investigating Guidelines on Poisons in Workplace Air,and thus then could be applied to determine PAEs in the air of plastic production logistics.