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本文以钨粉、钨条、碳化钨、三氧化钨、钨酸、蓝钨、紫钨、仲钨酸铵、偏钨酸铵为分析对象,通过实验,提出了钨及其制品经过适当的溶剂处理后,在碱性条件下,以铁(Ⅲ)为共沉淀剂富集铅,用柠檬酸络合残余钨,以原子吸收光谱法测定钨中质量分数为0.000 3%～0.005 0%的铅量。文章分别对铅分离富集条件、主体元素及共存元素干扰情况、工作曲线的线性关系进行了研究,确定了最佳分析条件。采用优化后的测定条件,用原子吸收光谱法进行钨中铅量的测定,主体元素及其共存元素对测定均无干扰;加标回收率在90.33%～110.00%之间;测定编号为YSS001-96-3和YSS001-96-5三氧化钨标准样品,铅标准值分别为0.000 62%和0.004 1%,实际测得值分别为0.000 63%和0.004 2%;上述三氧化钨标样,通过21次独立测定,其相对标准偏差分别为4.17%和5.18%。方法简便,实用性强。
In this paper, the tungsten, tungsten, tungsten carbide, tungsten trioxide, tungstic acid, blue tungsten, purple tungsten, ammonium paratungstate, ammonium metatungstate for the analysis of the object, through experiments, proposed tungsten and its products after appropriate solvent treatment, Under basic conditions, lead (Ⅲ) was used as a coprecipitator to enrich Pb and the residual tungsten was complexed with citric acid. The content of lead in tungsten was 0.0003% ~ 0.005% by atomic absorption spectrometry. The paper separately studied the conditions of Pb enrichment, the interference of main elements and coexisting elements and the linear relationship of work curves, and determined the best analytical conditions. The optimal determination conditions were as follows: the content of lead in tungsten was determined by atomic absorption spectrometry, the main elements and their coexisting elements had no interference on the determination; the recoveries were in the range of 90.33% -110.00%; the determination was YSS001- 96-3 and YSS001-96-5 standard samples of tungsten oxide, lead standard values were 0.000 62% and 0.004 1%, respectively, the actual measured values were 0.000 63% and 0.004 2%; the above tungsten trioxide standard, by 21 independent determination, the relative standard deviations were 4.17% and 5.18% respectively. The method is simple and practical.