顶空气相色谱法测定土壤中总氰化物  

Determination of Total Cyanide in Soil by Headspace Gas Chromatography

作　　者：韦桂欢[1] 张洪彬[1] 龙庆云[1] 王晓利[1] 李占强[1] 

机构地区：[1]中国船舶重工集团公司第七一八研究所河北邯郸056027

出　　处：《舰船防化》2015年第2期12-17,共6页

摘　　要：建立了测定环境土壤中总氰化物的顶空气相色谱检测方法。环境土壤中总氰化物经过50％氢氧化钠溶液提取50min，于pH〈2的酸性体系中进行蒸馏，总氰化物以简单氢化氰的形式释放出来，被碱液吸收。得到的吸收液样品在顶空瓶中进行衍生化，用气相色谱．电子捕获检测器对顶空瓶液上气中的氯化氰进行检测。试验以气相色谱／盾谱确认了衍生化生成的氯化氰，讨论了不同极性色谱柱对样品分离的效果，优化了样品分析顶空气液比、平衡衍生温度以及平衡时间等分析条件，对简单氰化物、强络合氰化物进行了回收加标试验。实验表明，方法标准曲线线性相关系数为0．9977，相对标准偏差在7．1％～15％，回收率在78％～97％，最低检测浓度为0．15mg·kg^-1。A method for determinating total cyanide in soil by headspace Gas Chromatography was researched. Total cyanide in soil was extracted by 50% sodium hydroxide for 50 minutes, then distillated in the condition of pH〈2, and absorption of the liberated HCN gas was carried out by using a glass coil and 1% sodium hydroxide solution. The sample absorption obtained was derivatized with chloramines-T in the headspace bottle, and analyzed by headspace gas chromatography with electron capture detector after derivatization. The CNC1 generated was qualitated by gas chromatography-mass spectrometry. The conditions of different polar capillary column, the influences of different vapor liquid radio, derivative equilibration temperature and equilibration time were optimized. The experiments of the recovery for the amenable cyanide and the strongly-bound complex cyanides were discussed respectively. The coefficient of correlation for the calibration curve was 0.9977, the relative standard deviations were between 7.1% and 15%, the recoveries varied from 78% to 97%, and the lowest detection concentration of the method was 0.15 mg·kg^-1.

关 键 词：土壤 总氰化物 测定 气相色谱法 

分 类 号：O659.21[理学—分析化学]