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目的建立作业场所空气中三氯氧磷的化学测定法。方法用水作吸收液,大型气泡吸收管采样,以钼酸铵,氯化亚锡做显色剂,生成磷钼蓝比色测定。选择了最佳的采样和测定条件,确定适宜的硫酸和氯化亚锡的用量、反应温度和时间。结果方法的检出限为0.1μg/ml,最低检测浓度为0.17mg/m3(采样体积以7.5L计)。当标准溶液浓度在0.2~20mg/L时,相对标准偏差为3.3%~5.7%,线性范围为0.2~20mg/L,采样效率达到95.6%~100%。样品在吸收管中可稳定3d。结论通过实验室和现场试验证明,该法简便、快速、灵敏,不需要特殊仪器,适宜基层使用。
Objective To establish a chemical assay of phosphorus oxychloride in the air at workplaces. Methods Water was used as absorption liquid, large bubble absorption tube was sampled, and ammonium molybdate and stannous chloride were used as chromogenic reagent to generate phosphomolybdate blue colorimetric assay. Selected the best sampling and determination conditions, to determine the appropriate amount of sulfuric acid and stannous chloride, reaction temperature and time. Results The detection limit of the method was 0.1μg / ml, the lowest detection concentration was 0.17mg / m3 (sampling volume was 7.5L). The relative standard deviation (RSD) was 3.3% ~ 5.7% when the concentration of standard solution was 0.2 ~ 20mg / L, the linear range was 0.2 ~ 20mg / L and the sampling efficiency was 95.6% ~ 100%. Sample in the absorption tube can be stable 3d. Conclusion The laboratory and field tests show that the method is simple, rapid and sensitive, and does not require special instruments and is suitable for grassroots use.