分光光度法测定酸泥中碲
|
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 for30 min,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/25 m L,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.
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 for30 min,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/25 m L,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.
引文
[1]王冬珍.阳极泥及碲回收物料中高含量碲的测定[J].岩矿测试,2002,21(2):143-146.
[2]沈广鑫.重铬酸钾滴定法测定中和渣中的碲[J].江西冶金,2008,28(5):32-34.
[3]北京矿冶研究总院分析室.矿石及有色金属分析手册,二安替比林丙基甲烷光度法[M].北京:冶金工业出版社,1990.
[4]陈学源.溴化碲分光光度法测定钛铝合金中微量碲[J].稀有金属材料与工程,1997,26(4):56-59.
[5]张渝阳,邓桂春,张新,等.催化动力学分析法测定粗硒粉中微量碲的研究[J].光谱学与光谱分析,2008,28(3):652-655.
[6]凌宗干.催化示波极谱法测定电解铅中痕量硒、碲[J].理化检验-化学分册,2001,37(11):523-524.
[7]黄金,龚竹青.火焰原子吸收光谱法测定铅碲渣中碲[J].冶金分析,2006,26(2):53-54.
[8]展宗波,王冬珍.原子荧光光谱法测定银锭中的硒、碲[J].甘肃冶金,2017,39(5):56-58.
[9]何梅,胡军凯.电感耦合等离子体原子发射光谱法(ICPAES)测定铜阳极泥和分银渣中锡、碲含量[J].中国无机分析化学,2012,2(2):45-48.
[10]董学林,贾正林,汪慧平,等.共沉淀分离-电感耦合等离子体质谱法测定多金属矿石中硒、碲[J].冶金分析,2016,36(3):6-10.
[2]沈广鑫.重铬酸钾滴定法测定中和渣中的碲[J].江西冶金,2008,28(5):32-34.
[3]北京矿冶研究总院分析室.矿石及有色金属分析手册,二安替比林丙基甲烷光度法[M].北京:冶金工业出版社,1990.
[4]陈学源.溴化碲分光光度法测定钛铝合金中微量碲[J].稀有金属材料与工程,1997,26(4):56-59.
[5]张渝阳,邓桂春,张新,等.催化动力学分析法测定粗硒粉中微量碲的研究[J].光谱学与光谱分析,2008,28(3):652-655.
[6]凌宗干.催化示波极谱法测定电解铅中痕量硒、碲[J].理化检验-化学分册,2001,37(11):523-524.
[7]黄金,龚竹青.火焰原子吸收光谱法测定铅碲渣中碲[J].冶金分析,2006,26(2):53-54.
[8]展宗波,王冬珍.原子荧光光谱法测定银锭中的硒、碲[J].甘肃冶金,2017,39(5):56-58.
[9]何梅,胡军凯.电感耦合等离子体原子发射光谱法(ICPAES)测定铜阳极泥和分银渣中锡、碲含量[J].中国无机分析化学,2012,2(2):45-48.
[10]董学林,贾正林,汪慧平,等.共沉淀分离-电感耦合等离子体质谱法测定多金属矿石中硒、碲[J].冶金分析,2016,36(3):6-10.