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[目的]改进GBZ/T160.30-2004《工作场所空气有毒物质测定无机含磷化合物》中磷酸的钼酸铵分光光度法。[方法]在GBZ/T160.30-2004的基础上,增加体系反应的酸度,并对一些试剂用量等进行调整。更改钼酸铵溶液的配制方法;更改各种试剂的用量;改变标准系列。[结果]本法标准曲线相关性>0.999,检出限0.4μg/ml,最低检出浓度0.13 mg/m3,(以采集75 L空气样品)。相对标准偏差2.5%~7.5%,加标回收率97%~107%,显色1.5 h,其吸光度小于1%变异。测定磷酸标准参考物质结果为668μg/L,测定值在其不确定范围内。[结论]建议对GBZ/T160.30-2004方法进行修订。
[Objective] The research aimed to improve the ammonium molybdate spectrophotometric method of phosphoric acid in GBZ / T160.30-2004 “Determination of inorganic phosphorus compounds in workplace air with toxic substances”. [Method] On the basis of GBZ / T160.30-2004, the acidity of the system reaction was increased, and the dosage of some reagents was adjusted. Change the preparation of ammonium molybdate solution; change the amount of various reagents; change the standard series. [Results] The standard curve of this method was> 0.999, the detection limit was 0.4μg / ml, the lowest detected concentration was 0.13 mg / m3 (to collect 75 L air sample). The relative standard deviations (RSDs) were 2.5% -7.5%. The recoveries were 97% -107%. The color developed for 1.5 h. The absorbance was less than 1%. Determination of phosphate standard reference material results for the 668μg / L, the measured value in its uncertainty. [Conclusion] It is suggested to amend GBZ / T160.30-2004 method.