孔雀绿-磷钼杂多酸离子缔合物分光光度法测定钨制品中的痕量磷  

Spectrophotometric Determination of Trace Phosphorus in Tungsten Products by Ion Association Complex of Malachite Green-Phosphorus Molybdenum Heteropoly Acid

作　　者：林丽君 陈焕涛 LIN Lijun;CHEN Huantao(Guangdong Xianglu Tungsten Industry Co.,Ltd.,Chaozhou 515633,Guangdong,China)

机构地区：[1]广东翔鹭钨业股份有限公司,广东潮州515633

出　　处：《中国钨业》2023年第4期81-86,共6页China Tungsten Industry

摘　　要：实验研究了在聚乙烯醇存在下,采用孔雀绿-磷钼杂多酸离子缔合物分光光度法测定钨制品中痕量磷。考察了掩蔽剂的选择及用量、硫酸用量、钼酸铵用量、孔雀绿用量、聚乙烯醇用量、显色时间以及显色温度等几个关键因素对测定结果的影响。实验表明,采用柠檬酸络合钨以及钨基体匹配工作曲线消除钨的干扰,在聚乙烯醇存在下,磷钼杂多酸与碱性染料孔雀绿反应生成稳定的离子缔合物。该缔合物的最大吸收波长为620 nm,摩尔吸光系数ε为1.05×10^(5) L/(mol·cm),磷在0~0.08μg/mL含量范围内遵守朗伯比尔定律。该方法的线性相关系数R2=0.9998,加标回收率在99%~102%之间,可测量含量在0.0030%以下的痕量磷,实验结果满足目前钨制品生产中磷的分析要求,可成功地应用于钨制品中磷含量的测定。This experiment studied the spectrophotometric determination of trace phosphorus in tungsten products by ion association complex of malachite green-phosphorus molybdenum heteropoly acid in the presence of polyvinyl alcohol.The effects of several key factors,such as the selection and dosage of masking agent,sulfuric acid dosage,ammonium molybdate dosage,malachite green dosage,polyvinyl alcohol dosage,color development time and color development temperature,on the determination results were investigated.The experiment shows that the interference of tungsten can be eliminated by using citric acid to complex tungsten and matching the working curve of tungsten matrix.In the presence of polyvinyl alcohol,phosphorus molybdenum heteropoly acid reacts with basic dye malachite green to form a stable ion association complex.The maximum absorption wavelength of the complex is 620 nm,the molar absorption coefficientεis 1.05×10^(5) L/(mol·cm),and the phosphorus content obeys the Beer-Lambert Law in the range of 0~0.08μg/mL.The linear correlation coefficient of this method is R2=0.9998,and the recovery rate of standard addition is between 99%and 102%.Trace phosphorus with content below 0.0030%can be measured.The experimental results meet the requirements of phosphorus analysis in tungsten products production at present,and can be successfully applied to the determination of phosphorus content in tungsten products.

关 键 词：钨制品 磷 碱性染料孔雀绿 离子缔合物 聚乙烯醇 

分 类 号：O657.3[理学—分析化学] TF841.2[理学—化学]