摘要
应用溴化碲分光光度法测定富集物酸泥中的碲时,主要受到样品中共存的硒、钙、铁、铜的干扰,实验采用硝酸溶解试样,通过硫酸冒白烟,用氢溴酸排除硒的干扰;在显色液中加入亚铁氰化钾沉淀铜、铁,静置30 min后过滤,将铜、铁、钙分离除去,用滤液直接进行测定,建立了分光光度法测定酸泥中碲含量的方法。试验表明,显色液中碲的质量浓度在0～200μg/25 m L范围内,符合比尔定律。碲的检出限和测定下限分别为0. 012%和0. 041%(质量分数),将实验方法分别用于0. 05%～10%3个实际酸泥样品、1个加标样品中碲量的测定,结果的相对标准偏差(RSD,n=6)为0. 76%～6. 5%,测定值与原子吸收法的测定结果一致。
Determination on tellurium in enriched acid sludge by application of tellurium bromide spectrophotometric method, the main interference factors are selenium,calcium,iron,copper,which are coexisted with the sample,in the test,nitric acid is adopted for sample dissolving,heating sulfuric acid to make it take white smoke,and then using hydrobromic acid to eliminate the interference of selenium; the potassium ferrocyanide shall be added into color-substrate solution to precipitate copper and iron,it shall be filtrated after leaved for 30min,copper,iron and calcium shall be separated and removed,the filter liquor shall be detected directly,so the determination method for tellurium content in acid sludge by spectrophotometric method is established. The test show,the mass concentration of tellurium in color liquid is in the range of 0~200 μg/25mL,which is conform to Beer’s Law. The detection limit and determination limit of tellurium separately are 0.012% and 0.041%( mass fraction),the experimental method shall be used for tellurium determination in 0.05%~10% three actual acid sludge samples,one spiked sample,the relative standard deviation (RSD,n=6) of results is 0.76%~6.5%,the estimated value and the testing results by atomic absorption method has no different.
作者
段永明
DUAN Yong-ming(Yunnan Gejiu Metallurgical Institute,Gejiu,Yunnan 661000,China)
出处
《云南冶金》
2018年第6期81-85,共5页
Yunnan Metallurgy
关键词
分光光度法
溴化碲
富集物
酸泥
spectrophotometric method
tellurium bromide
enrichment
acid sludge
