基于溴代比色法的高矿化度浸出液中铀分析方法的优化
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摘要
溴代比色法已广泛应用于CO_2+O_2地浸采铀工艺样品中铀的分析;但存在测定值低于试剂空白测定值和平行分析时测定值呈负增长趋势的问题。为此,对该方法的测定下限和干扰元素做了分析测定。试验结果表明:当铀的质量浓度低于1.000μg/mL时,其标准偏差和离散程度差,最大偏差达31%;当ρ(HCO_3~-)>120μg/mL时,标准曲线呈负增长趋势,干扰铀的测定;缩小取样体积,分析结果的相对误差由-65%降到2.4%。
The bromine colorimetry is widely used in the analysis of samples from in-situ leaching uranium process by CO_2+O_2,but there are problems such as that the measured value is lower than the measured value of the reagent blank and the measured value shows a negative growth trend when compared with parallel analysis.The lower limit and disturbance elements of the method are analyzed and determined.The experimental results show that when the mass concentration of uranium is lower than 1.000 g/mL,the standard deviation and dispersion degree of uranium is different,and the maximum deviation is up to 31%.When HCO_3~- mass concentration is higher than 120 g/mL,the standard curve shows a negative growth trend and interferes with the determination of uranium.When the sample size is reduced in the analysis process,the relative error of the analysis is decreased to 2.4% from -65%.
The bromine colorimetry is widely used in the analysis of samples from in-situ leaching uranium process by CO_2+O_2,but there are problems such as that the measured value is lower than the measured value of the reagent blank and the measured value shows a negative growth trend when compared with parallel analysis.The lower limit and disturbance elements of the method are analyzed and determined.The experimental results show that when the mass concentration of uranium is lower than 1.000 g/mL,the standard deviation and dispersion degree of uranium is different,and the maximum deviation is up to 31%.When HCO_3~- mass concentration is higher than 120 g/mL,the standard curve shows a negative growth trend and interferes with the determination of uranium.When the sample size is reduced in the analysis process,the relative error of the analysis is decreased to 2.4% from -65%.
引文
[1]苏学斌,王海峰,刘乃忠.CO2+O2原地浸出采铀工艺[M].北京:中国原子能出版社,2016.
[2]中国核工业总公司.重铀酸盐技术条件:EJ/T803-1993[S].北京:核工业标准化研究所,1993:1-4.
[3]顾洪云.分光光度计法制作标准曲线应注意的问题[J].中国氯碱,2011,22(7):36-37.
[4]田强兵.分析化学中检出限和测定下限的探讨[J].吉林地质,2012,31(3):92-94.
[5]杨金辉,汪清良.铀矿冶分析原理与方法[M].北京:化学工业出版社,2012.
[6]刘天煦.化验员基础知识问答[M].北京:化学工业出版社,2003.
[2]中国核工业总公司.重铀酸盐技术条件:EJ/T803-1993[S].北京:核工业标准化研究所,1993:1-4.
[3]顾洪云.分光光度计法制作标准曲线应注意的问题[J].中国氯碱,2011,22(7):36-37.
[4]田强兵.分析化学中检出限和测定下限的探讨[J].吉林地质,2012,31(3):92-94.
[5]杨金辉,汪清良.铀矿冶分析原理与方法[M].北京:化学工业出版社,2012.
[6]刘天煦.化验员基础知识问答[M].北京:化学工业出版社,2003.