EDTA络合连续滴定法同时测定铜精矿中高含量铅锌  

Simultaneous Determination of High Content of Lead and Zinc in Copper Concentrate by EDTA Complexation Continuous Titration

作　　者：方彦霞 展之旺 张彦翠[1] 王彬 李金明[1] 孙帅楠 FANG Yan-xia;ZHAN Zhi-wang;ZHANG Yan-cui;WANG Bin;LI Jin-ming;SONG Shuai-nai(Northwest Research Institute of Mining and Metallurgy,Baivin 730900,China)

机构地区：[1]西北矿冶研究院,甘肃白银730900

出　　处：《甘肃冶金》2021年第5期116-118,122,共4页Gansu Metallurgy

摘　　要：建立了EDTA络合连续滴定法同时测定铜精矿中高含量铅锌的分析方法,试样以盐酸、硝酸、硫酸溶解,用氢溴酸挥发除去砷、锑和锡。硫酸铅沉淀分离铅,沉淀用乙酸-乙酸钠缓冲液溶解测定铅,滤液用氨水-氯化铵沉淀分离铁锰,用抗坏血酸、氟化钾、硫脲掩蔽Fe^(3+)、Al^(3+)、Cu^(2+)等杂质,在pH=5.5~6.0的乙酸-乙酸钠缓冲液中,EDTA滴定锌、镉总量,减去原子吸收测定的镉量。采用该方法对样品进行精密度和加标回收试验,锌测定结果的相对标准偏差(RSD,n=6)为0.23%~0.56%。铅测定结果的相对标准偏差(RSD,n=6)为0.12%~0.34%。该方法具有操作简单、成本低、结果准确可靠等优点。An analytical method for the simultaneous determination of high content lead and zinc in copper concentrate by EDTA complexation continuous titration has been established, the samples were dissolved in hydrochloric acid, nitric acid and sulfuric acid and volatilized with hydrobromic acid to remove arsenic, antimony and tin. Lead sulfate was precipitated to separate lead, and the lead and filtrate were determined by dissolution of the precipitate with acetic acid-sodium acetate buffer solution, the filtrate was precipitated by ammonia water and ammonium chloride to separate iron and manganese, and impurities such as Fe^(3+), Al^(3+), and Cu^(2+) were masked by ascorbic acid, potassium fluoride, and thiourea. The total amount of zinc and cadmium was titrated by EDTA in acid-sodium acetate buffer solution with pH=5.5~6.0, and the cadmium content measured by atomic absorption was subtracted. The precision and standard recovery tests of the samples were carried out with this method. The relative standard deviations(RSD,n=6) of the zinc determination results ranged from 0.23%~0.56%. The relative standard deviation(RSD,n=6) of lead determination results ranged from 0.12%~0.34%. This method has the advantages of simple operation, low cost, accurate and reliable results.

关 键 词：铜精矿 EDTA络合连续滴定 高含量铅锌 

分 类 号：O655.22[理学—分析化学]