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    活性炭吸附-二氯甲烷解吸-气相色谱-质谱法测定固定污染源废气中3种丙烯酸酯类化合物的含量

    Determination of 3 Acrylic Esters in Waste Gas from Stationary Pollution Source by Gas Chromatography-Mass Spectrometry with Activated Carbon Adsorption and Dichloromethane Desorption

    • 摘要: 为实现固定污染源废气样品中丙烯酸酯类化合物的低成本、准确测定,通过优化吸附剂、解吸溶剂、解吸时间、色谱柱等试验条件提出了题示方法。以活性炭气体采样管在0.5 L·min-1流量下采集样品40 min,加入二氯甲烷1.00 mL和100 mg·L-1甲基丙烯酸甲酯-d8内标溶液0.020 mL,于室温解吸30 min,解吸液经0.22 μm滤膜过滤,滤液进入气相色谱-质谱仪。丙烯酸甲酯、甲基丙烯酸甲酯和丙烯酸(正)丁酯等3种丙烯酸酯类化合物在DB-624色谱柱上以程序升温条件分离,经电子轰击离子源电离,以选择离子监测模式检测,并用内标法定量。结果显示,3种丙烯酸酯类化合物标准曲线的线性范围为0.200~50.0 mg·L-1,检出限(3.143s)均为0.003 mg·m-3。以氮气为底气进行3个浓度水平的加标回收试验,回收率为85.2%~115%,测定值的相对标准偏差(n=6)为10%~20%。

       

      Abstract: To achieve low-cost and accurate determination of acrylic esters in waste gas samples from stationary pollution source, the method mentioned by the title was proposed by optimizing testing conditions including adsorbent, desorption solvent, desorption time, and chromatographic column. Samples were collected for 40 min at flow rate of 0.5 L·min-1 using activated carbon gas sampling tube. Then, 1.00 mL of dichloromethane and 0.020 mL of 100 mg·L-1 methyl methacrylate-d8 internal standard solution were added, followed by desorption at room temperature for 30 min. The desorption solution was passed through a 0.22 μm filter membrane, and the filtrate was introduced into gas chromatograph-mass spectrometer. Three acrylic esters, including methyl acrylate, methyl methacrylate, and n-butyl acrylate, were separated on DB-624 column using temperature program condition, ionized by electron impact ion source, detected in selected ion monitoring mode, and quantified using the internal standard method. It was shown that the linear range of the standard curves for the 3 acrylic esters was 0.200-50.0 mg·L-1, with the same detection limit (3.143s) of 0.003 mg · m-3. Spike recovery tests at 3 concentration levels using nitrogen as the base gas were conducted, giving recoveries in the range of 85.2%-115%, and RSDs (n=6) of the determined values ranged from 10% to 20%.

       

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