分光光度法测定三氧化铀中的硫酸根
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摘要
采用TBP-萃淋树脂吸附三氧化铀样品中的铀,硫酸根与铬酸钡进行交换反应后,直接比色法测定硫酸根的含量。实验中研究了三氧化铀样品中硫酸根含量测定的样品制备、分离、反应酸度,煮沸时间,铬酸钡用量等影响因素。优化条件下,采用硝酸(5mol/L)淋洗、1mL HCl溶液(2.5mol/L)调节溶液中酸浓度、使用2mL BaCrO_4进行交换反应、煮沸3min,得到方法相对标准偏差小于10%,加标回收率为92.9%～110%。实验结果表明,直接显色的测定方法灵敏、快速、准确度高。方法测定条件易于获得,适于推广应用。
The uranium in uranium trioxide sample was adsorbed by TBP resin,after the sulfate was exchanged with barium chromate,the content of sulfate was determined directly by colorimetry.The influence factors on the determination of sulfate in uranium trioxide were studied,including the preparation,separation,reaction acidity,boiling time and the amount of barium chromate.Under the optimal conditions,rinsed by 5 mol/L nitric acid,adjust solution acidity by 1 mL 2.5 mol/L HCl solution,exchanged reaction by 2 mL BaCrO_4 and boiled 3 minutes.The relative standard deviation of the method was less than 10%,and the standard recovery was 92.9%—110%.Experimental results show that the method is sensitive,rapid and accurate.The determination conditions are easy to obtain,and the method is suitable for promotion application.
The uranium in uranium trioxide sample was adsorbed by TBP resin,after the sulfate was exchanged with barium chromate,the content of sulfate was determined directly by colorimetry.The influence factors on the determination of sulfate in uranium trioxide were studied,including the preparation,separation,reaction acidity,boiling time and the amount of barium chromate.Under the optimal conditions,rinsed by 5 mol/L nitric acid,adjust solution acidity by 1 mL 2.5 mol/L HCl solution,exchanged reaction by 2 mL BaCrO_4 and boiled 3 minutes.The relative standard deviation of the method was less than 10%,and the standard recovery was 92.9%—110%.Experimental results show that the method is sensitive,rapid and accurate.The determination conditions are easy to obtain,and the method is suitable for promotion application.
引文
[1]中华人民共和国环境保护部.水质硫酸盐的测定铬酸钡分光光度法(试行):HJ/T 342-2007[S].北京:中国环境科学出版社,2007.
[2]马秀卿,宣春生,贾晓红.用分光光度法间接测定微量硫酸根的研究[J].太原工业大学学报(Journal of Taiyuan University of Technology),1989,20(3):68-72.
[3]刘峻岭,赵立飞.硫酸钡沉淀-等离子体发射光谱法(ICP-AES)测定高放废液样品中的硫酸根[J].中国原子能科学研究院年报(Annual report of China academy of atomic energy),2004,31:132-133.
[4]王力君,石华.电感耦合等离子体原子发射光谱法(ICP-AES)直接测定天然矿泉水中的硫酸根[J].中国无机分析化学(Chinese Journal of Inorganic Analytical Chemistry),2014,4(4):16-17.
[5]董灵英.铀的分析化学[M]北京:原子能出版社,1982.
[6]戚月花,张淑玲,李先和,等.离子色谱法测定胺液中硫酸根含量[J].中国无机分析化学(Chinese Journal of Inorganic Analytical Chemistry),2016,6(2):25-27.
[7]宋金如,于荣,李发亮.铀矿石菌浸液中硫酸根测定方法的研究[J].东华理工学院学报(Journal of east china institute of technology),200421(1):69-72.
[2]马秀卿,宣春生,贾晓红.用分光光度法间接测定微量硫酸根的研究[J].太原工业大学学报(Journal of Taiyuan University of Technology),1989,20(3):68-72.
[3]刘峻岭,赵立飞.硫酸钡沉淀-等离子体发射光谱法(ICP-AES)测定高放废液样品中的硫酸根[J].中国原子能科学研究院年报(Annual report of China academy of atomic energy),2004,31:132-133.
[4]王力君,石华.电感耦合等离子体原子发射光谱法(ICP-AES)直接测定天然矿泉水中的硫酸根[J].中国无机分析化学(Chinese Journal of Inorganic Analytical Chemistry),2014,4(4):16-17.
[5]董灵英.铀的分析化学[M]北京:原子能出版社,1982.
[6]戚月花,张淑玲,李先和,等.离子色谱法测定胺液中硫酸根含量[J].中国无机分析化学(Chinese Journal of Inorganic Analytical Chemistry),2016,6(2):25-27.
[7]宋金如,于荣,李发亮.铀矿石菌浸液中硫酸根测定方法的研究[J].东华理工学院学报(Journal of east china institute of technology),200421(1):69-72.