工作场所空气中丙烯酸测定的在线甲基化-气相色谱法

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目的:建立在线甲基化-气相色谱法测定工作场所空气中丙烯酸浓度的方法。方法:2018年1至7月用溶剂解吸型硅胶管采集空气中的丙烯酸,甲醇解吸后,解吸液与衍生化试剂四甲基氢氧化铵(TMAH,25%甲醇溶液)同时进样,在350 ℃的进样口生成丙烯酸甲基衍生物,经气相色谱测定。结果:在0~258.4 mg/L浓度范围线性关系良好,相关系数为0.999 4,方法的检出限为0.9 mg/L,最低检出浓度为0.06 mg/mn 3(以采集15 L空气计),5次平行测定相对标准偏差(n RSD)在2.2%~2.7%,加标回收率在96.9~101.6%。n 结论:结果表明该法有效、简便、准确,可以用于工作场所空气中丙烯酸浓度的测定。“,”Methods:the samples were absorbed by solvent desorption silica gel tube and desorbed by methanol. Desorption fluid in the injector at 350 ℃ in the presence of an organic alkali tetramethylamine hydroxide (TMAH, 25% methanol) , allowed quantitative analysis of acrylic acid as its corresponding methyl derivative by gas chromatography.Results:calibration curve of the method was linear within the range 0-258.4 mg/L and showed good linearity with n r=0.999 4. The determination limit of the method was 0.9 mg/L, and the minimum detection concentration was 0.06 mg/mn 3 (collect 15 L air) . The relative standard deviation (n RSD) was 2.2%-2.7% (n n=5) . Recoveries were between 96.9-101.6%.n Conclusion:the results prove on-line methylation gas chromatography is an accurate, simple and high sensitive method for determining acrylic acid in workplace air.
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