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目的研制作业场所空气中氯化氰的检测方法。方法采用磷酸盐缓冲液和吡啶-巴比妥酸作吸收液进行采样,用分光光度法测定。同时对pH值、显色时间、温度、氯胺T加入量、缓冲液不同配比、显色剂配比、最大吸收波长等条件进行优化。对方法的线性范围、检出限、精密度、回收率、采样效率等特性指标进行试验。结果方法的测定范围为0～0.4μg/ml,相关系数为0.9993,回归方程为(?)= 1.547x-0.005,检出限为0.016μg/ml,测定下限为0.07μg/ml,变异度为1.1%～2.8%,样品回收率为98.9%～109.8%。采样效率为92.9%～98.9%。结论吡啶-巴比妥酸光度法测定氯化氰,是一种简单、快速、准确、灵敏、经济、特异度好、易于推广的检测方法,性能指标满足职业接触限值的检测要求。
Objective To develop a method for the detection of cyanogen chloride in the workplace air. Methods Phosphate buffer and pyridine-barbituric acid were used as samples for absorption and determined by spectrophotometry. At the same time, the optimal conditions were pH value, color development time, temperature, addition amount of chloramine T, different ratio of buffer, ratio of developer, maximum absorption wavelength and so on. The linear range of the method, the detection limit, precision, recovery, sampling efficiency and other characteristics of indicators for testing. Results The detection range was 0 ~ 0.4μg / ml, the correlation coefficient was 0.9993, the regression equation was (?) = 1.547x-0.005, the detection limit was 0.016μg / ml, the determination limit was 0.07μg / ml, 1.1% ~ 2.8%, the recovery rate of samples was 98.9% ~ 109.8%. The sampling efficiency is 92.9% ~ 98.9%. Conclusion The pyridine-barbituric acid spectrophotometric method for the determination of cyanogen chloride is a simple, rapid, accurate, sensitive, economical, specific and easy to popularize detection method. The performance index meets the testing requirements of occupational exposure limits.