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工作场所空气中丁腈和异丁腈的溶剂解吸-气相色谱测定方法

[The method of determination for butyronitrile and isobutyronitrile in the air of workplace by dissolved desorption-gas chromatography].

作者信息

Chen G L, Chen S G, Rong W F, He J H, Liang J Y, Zhou X Q

机构信息

Laboratory Department, Foshan Institute of Occupational Disease Prevention and Control, Foshan 528000, China.

Institute of Toxic Chemical Surveillance, Guangdong Province Hospital for Occupational Disease Prevention and Treatment, Guangzhou 510300, China.

出版信息

Zhonghua Lao Dong Wei Sheng Zhi Ye Bing Za Zhi. 2022 Apr 20;40(4):296-299. doi: 10.3760/cma.j.cn121094-20210119-00034.

DOI:10.3760/cma.j.cn121094-20210119-00034
PMID:35545599
Abstract

To establish a method for the determination of butyronitrile and isobutyronitrile in the air of workplace by gas chromatography. In March 2020, butyronitrile and isobutyronitrile in the air of workplace was collected by silica gel, eluted with methanol, separated and determined by gas chromatogram with flame ionization detector, the characteristics of determination of nitrile and isobutyronitrile by gas chromatography were analyzed. The limit of detection for butyronitrile and isobutyronitrile was 0.33 μg/ml. The linear range of butyronitrile determined by this method was 1.60-1600.00 μg/ml, =2.295-3.480, and the coefficient correlation was 0.99998, and the minimum detection concentration was 0.22 mg/m(3) (collected sample volume was 1.50 L) . The within-run precisions were 2.43%-4.12%, the between-run precisions were 1.72%-3.70%, and the desorption rates were 93.26%-98.41%. The linear range of isobutyronitrile determined by this method was 1.52-1520.00 μg/ml, =2.208-0.102, and the coefficient correlation was 0.99998, and the minimum detection concentration was 0.22 mg/m(3) (collected sample volume was 1.50 L) . The within-run precisions were 2.52%-3.22%, the between-run precisions were 1.20%-3.82%, and the desorption rates were 96.85%-102.50%. The sealed samples could be stored at least 10 days at room temperature without significant loss. The method has the advantages of good precision, high sensitivity and simple operation. It is suitable for the simultaneous determination of butyronitrile and isobutyronitrile in the air of workplace.

摘要

建立气相色谱法测定工作场所空气中丁腈和异丁腈的方法。2020年3月,用硅胶采集工作场所空气中的丁腈和异丁腈,用甲醇洗脱,采用带氢火焰离子化检测器的气相色谱仪进行分离测定,分析气相色谱法测定腈类和异丁腈的特性。丁腈和异丁腈的检出限为0.33μg/ml。该方法测定丁腈的线性范围为1.60~1600.00μg/ml,r=2.295~3.480,系数相关性为0.99998,最低检出浓度为0.22mg/m³(采集样品体积为1.50L)。批内精密度为2.43%~4.12%,批间精密度为1.72%~3.70%,解吸率为93.26%~98.41%。该方法测定异丁腈的线性范围为1.52~1520.00μg/ml,r=2.208~0.102,系数相关性为0.99998,最低检出浓度为0.22mg/m³(采集样品体积为1.50L)。批内精密度为2.52%~3.22%,批间精密度为1.20%~3.82%,解吸率为96.85%~102.50%。密封样品在室温下至少可保存10天,无明显损失。该方法精密度好、灵敏度高、操作简便,适用于工作场所空气中丁腈和异丁腈的同时测定。

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