顶空气相色谱法测定固体废物中氰化物
魏鑫，王遥雪，凌约涛，潘瑞花，郭少飞
武汉海关技术中心，武汉 430050
Determination of cyanide in solid wastes by headspace gas chromatography
WEI Xin, WANG Yaoxue, LING Yuetao, PAN Ruihua, GUO Shaofei
Technology Center of Wuhan Customs, Wuhan 430050, China
摘要：建立顶空进样气相色谱法测定固体废物中氰化物的方法。固体废物中的氰化物经零顶空提取后，含氰化物滤液经氯胺T衍生，生成具有挥发性的氯化氰，顶空进样后，经气相色谱柱分离，采用电子捕获检测器(ECD)检测，以外标法定量。在最优条件下，氰化物的质量浓度在0.50～50.0 μg/L范围内与色谱峰面积具有良好的线性关系，相关系数为0.999 4，方法检出限为0.1 μg/L。在1.0，5.0，10 μg/L 3个添加水平时，加标回收率为55.2%～92.3%，测定结果的相对标准偏差为1.8%～3.2%(n=7)。与传统的离子色谱法相比，该方法操作安全，抗干扰能力强，在固废检测领域具有有很好的应用前景。
Abstract：A method for the determination of cyanide in solid wastes by headspace gas chromatography was established. Cyanide in solid waste was extracted by zero headspace, and the cyanide containing filtrate was derivatized by chloramine T to form volatile cyanogen chloride. After headspace injection, the extract were separated by the gas chromatographic column, detected by electron capture detector(ECD) and quantified by external standard method. Under the optimal conditions, the mass concentration of cyanide had a good linear relationship with the chromatographic peak area in the range of 0.50-50.0 μg/L, the correlation coefficient was 0.999 4, and the detection limit was 0.1 μg/L. At the addition levels of 1.0, 5.0 and 10 μg/L, the recoveries were 55.2%-92.3%, and the relative standard deviations of determination results were 1.8%-3.2%(n=7). Compared with the traditional ion chromatography, the method is safe to operate, and good anti-interference ability, and it has a good application prospect in the field of solid waste detection.
关键词：固体废物；顶空气相色谱法，氰化物，衍生
Keywords：solid wastes; headspace gas chromatography; cyanide; derivative
基金：武汉海关关级项目(2019WK007)
本文引用格式：
魏鑫，王遥雪，凌约涛，等.顶空气相色谱法测定固体废物中氰化物[J].化学分析计量，2020，29(6)：15-18.
WEI X，WANG Y X，LING Y T，et al. Determination of cyanide in solid wastes by headspace gas chromatography[J]. Chemical analysis and meterage，2020，29(6)：15-18.
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