工作场所空气中甲基丙烯酸甲酯的溶剂解吸气相色谱测定方法研究

目的建立工作场所空气中甲基丙烯酸甲酯的溶剂解吸气相色谱测定方法。方法采用活性炭管采样二硫化碳解吸,或者硅胶管采样丙酮解吸,经FFAP毛细管色谱柱分离的气相色谱测定甲基丙烯酸甲酯方法。对方法的线性范围、检出限、精密度、解吸效率、采样效率等性能指标进行了规范性研究。结果该试验甲基丙烯酸甲酯线性范围分别为0.6～561.6 mg/L（活性炭管采样二硫化碳解吸）和0.6～1 497.6 mg/L（硅胶管采样丙酮解吸）;检出限（相当于3倍噪声的含量）均为0.6 mg/L;最低检出浓度分别为0.4和0.2 mg/m3（前者以活性炭采集1.5 L空气样品,后者以硅胶采集4.5 L空气样品计）;活性炭管采样二硫化碳解吸和硅胶管采样丙酮解吸的气相色谱测定方法的重现性好,相对标准偏差分别为1.2%～4.0%和0.5%～2.5%;平均解吸效率分别为94.2%～97.5%和97.0%～98.3%;采样效率分别为99.8%～100.0%和94.1%～100.0%;100 mg活性炭对甲基丙烯酸甲酯的穿透容量〉28.6 mg,300 mg硅胶对甲基丙烯酸甲酯的穿透容量〉2.7 mg;2种固体吸附剂管采集的样品在室温下至少可保存7 d。结论活性炭管采样二硫化碳解吸和硅胶管采样丙酮解吸的气相色谱测定方法都可完全适用于工作场所空气中甲基丙烯酸甲酯的测定。

Simultaneous determination of methyl methacrylate in the air of workplaces by solvent desorption gas chromatography

Objective To establish solvent desorption gas chromatographic method for determination of methyl methacrylate in the air of workplaces. Methods Air samples containing methyl metbacrylate in the workplace were collected with activated carbon tube and desorbed with CS2 or with silica gel tube and desorbed with acetone, and then separated with FFAP capillary columns and detected with flame ionization detector. Results The linear ranges were 0.6 - 561.6 mg/L for samples collected with activated carbon tube and desorbed with CS2 and 0. 6 - 1 497.6 mg/L for samples collected with silica gel tube and desorbed with acetone. The limits of detection were both 0. 6 mg/L. The determination had a good reproducibility. Their relative standard deviations were 1.2% -4. 0% and 0. 5% -2. 5% , respectively. The average desorption efficieneies were 94. 2% -97.5% and 97. 0% -98.3%. Absorption effieieneies were 99. 8% - 100. 0% and 94. 1% - 100. 0%. The breakthrough volume was above 28.6 mg in 100 mg activated carbon and 2. 7 mg in 300 mg silica gel. Samples collected by the two solid adsorbent tubes could at least store 7 days at room temperature. Conclusion The two methods proved to be suitable for the simultaneous determination of methyl methacrylate in the air of workplaees.