高频燃烧红外吸收光谱法测定仲钨酸铵(APT)中微量硫

Determination of Trace Sulfur in Ammonium Paratungstate by High Frequency Combustion Infrared-Absorption Spectroscopy

对高频燃烧红外吸收光谱法测定仲钨酸铵（APT）中的微量硫含量进行了研究。依据仲钨酸铵的材料性质和高频燃烧红外吸收光谱分析方法的分析特点,分别针对样品的前处理、样品称样量、助熔剂的选择及用量、校准物质的选择等做了条件实验。最终得出最佳的实验条件是称取1g仲钨酸铵样品,进行一定的前处理,再加入0.3g纯铁和1.5g钨助熔剂。按照最佳实验方法,对仲钨酸铵中微量硫含量进行测定,结果的相对标准偏差（RSD,n=5）小于8%,加标回收率为98%-109%。

High frequency combustion infrared-absorption spectroscopy was applied to the determination of trace sulfur in ammonium paratungstate （APT）. Based on the material properties of APT and the performance of high frequency combustion infrared-absorption spectroscopy, experiments conditions, including sample pretreatment, sample weight, dosage of the flux and choice of the flux and calibration materials, were performed. The optimized experiment conditions were obtained as follows： a 1 g APT was weighted with pretreatment, and 0.3 g pure iron and 0.3 g tungsten flux were added. Under the optimized experimental conditions, the relative standard deviation （RSD, n=5） was less than 8% with the recovery rate of 98%-109%.