用分光光度法测定酸泥中的硒
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摘要
研究了用分光光度法测定酸泥中的硒。采用硝酸、硫酸溶解试样,溶液中加入亚铁氰化钾-铁氰化钾混合溶液消除大部分金属离子的干扰,加入酒石酸溶液消除碲的干扰,在稳定剂丙三醇存在条件下,用抗坏血酸将硒(Ⅳ)还原为橙色单质硒,形成悬浊液,以分光光度法测定酸泥中的硒。结果表明,悬浊液中硒质量浓度在0～400μg/50 mL范围内,测定结果线性关系良好,相关系数为0.999 8,检出限为0.093μg/mL。方法用于4个实际酸泥样品和2个加标样品中硒的测定,测定结果的相对标准偏差(n=6)为0.37%～1.50%,结果较为满意。
Spectrophotometry was adopted to determination the selenium in the acid sludge.Specimen was dissolved using nitric acid and sulfuric acid.The mixed solution of potassium ferrocyanide-potassium ferricyanide was added into the dissolved solution to eliminate the interferences of most metal ions.Tartaric acid solution is added into the solution to eliminate the interferences of tellurium.And using propanetriol as stabilizer,using ascorbic acid to restore selenium(Ⅳ) to orange elemental selenium and to form suspension,then selenium in the acid sludge was determined by spectrophotometry.The result shows that the mass concentration of selenium in the suspension is 0～400 μg/50 mL,and the showing a good linear correlation with absorbance with the correlation coefficient of 0.999 8 and a detection limit of 0.093 μg/mL.The approach can be used to determined selenium in four actual acid sludge samples and two spiked samples.The relative standard deviation(n=6) is 0.37%～1.5% with a satisfactory results.
Spectrophotometry was adopted to determination the selenium in the acid sludge.Specimen was dissolved using nitric acid and sulfuric acid.The mixed solution of potassium ferrocyanide-potassium ferricyanide was added into the dissolved solution to eliminate the interferences of most metal ions.Tartaric acid solution is added into the solution to eliminate the interferences of tellurium.And using propanetriol as stabilizer,using ascorbic acid to restore selenium(Ⅳ) to orange elemental selenium and to form suspension,then selenium in the acid sludge was determined by spectrophotometry.The result shows that the mass concentration of selenium in the suspension is 0～400 μg/50 mL,and the showing a good linear correlation with absorbance with the correlation coefficient of 0.999 8 and a detection limit of 0.093 μg/mL.The approach can be used to determined selenium in four actual acid sludge samples and two spiked samples.The relative standard deviation(n=6) is 0.37%～1.5% with a satisfactory results.
引文
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[2] 罗永锋,谢昆良,余灿辉.硫酸渣中硒的测定方法研究[J]. 中国有色冶金,2016,45(6):70-71.
[3] 张祖琼,冯俊华,商仕杰,等.含硒物料中硒的滴定分析方法研究[J].云南冶金,2018,47(1):73-76.
[4] 北京矿冶研究总院分析室.矿石及有色金属分析手册[M].北京:冶金工业出版社,1990:173-174.
[5] 李咏梅,李人宇,秦纪亮,等.抗坏血酸比浊法测定微量硒[J].冶金分析,2008,28(6):49-52.
[6] 龙萍,邵丹,杨华,等.极谱法快速连续测定硒和碲[J].云南冶金,2012,41(2):91-93.
[7] 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.
[8] 权斌,倪迎瑞,李海涛,等.氯化银沉淀分离—氢化物发生—原子荧光光谱法测定银锭中的硒和碲[J].理化检验(化学分册),2012,48(7):851-853.
[9] 董亚妮,田萍,熊英,等.焙烧分离—氢化物发生—原子荧光光谱法测定铜铅锌矿石中的硒[J].岩矿测试,2011,30(2):164-168.
[10] 张宏丽,倪文山,肖芳,等.砷共沉淀—电感耦合等离子体原子发射氢法测定金精矿中硒和碲[J].冶金分析,2016,36(9):32-36.
[11] 董学林,贾正勋,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和碲[J].冶金分析,2016,36(3):6-10.