三辛烷叔胺萃取分光光度法测定水中钍
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摘要
采用氢氧化铁共沉淀载带水中钍,经浓硝酸溶解沉淀后,采用三辛烷基叔胺(N-235)混匀溶液萃取,盐酸反萃取,进一步纯化分离钍,与铀试剂Ⅲ形成络合物后用分光光度法测定。方法在0. 05 mg/L～0. 500 mg/L范围内线性良好,方法检出限为0. 025μg/L,探测下限为0. 10μg/L。将该方法用于实际水样的测定,6次测定结果的RSD为7. 0%～19. 6%,回收率为90. 0%～92. 4%。
Thorium in water was concentrated by Fe( OH)3 coprecipitation. The precipitate was dissolved in concentrated HNO3. With trioctyl tertiary amine( N-235) extraction and hydrochloric acid reextraction for further separation,thorium was then determined by spectrophotometry using uranium reagent Ⅲ. The method had good linearity in the range of 0. 05 mg/L to 0. 500 mg/L. The method detection limit was 0. 025 μg/L and the lower limit of quantitation was 0. 10 μg/L. Applied this method to practical water sample determination,the RSDs of six duplicated measurements were from 7. 0% to 19. 6%,and the recoveries were from 90. 0% to 92. 4%.
Thorium in water was concentrated by Fe( OH)3 coprecipitation. The precipitate was dissolved in concentrated HNO3. With trioctyl tertiary amine( N-235) extraction and hydrochloric acid reextraction for further separation,thorium was then determined by spectrophotometry using uranium reagent Ⅲ. The method had good linearity in the range of 0. 05 mg/L to 0. 500 mg/L. The method detection limit was 0. 025 μg/L and the lower limit of quantitation was 0. 10 μg/L. Applied this method to practical water sample determination,the RSDs of six duplicated measurements were from 7. 0% to 19. 6%,and the recoveries were from 90. 0% to 92. 4%.
引文
[1]国家环境保护局. GB 11224—89水中钍的分析方法[S].北京:中国标准出版社,1989.
[2]余耀仙.水中钍的分析方法[J].辐射防护,1989,9(1):47-51.
[3]郑洁,金家伟,李建辉.铀、钍联合分析技术在水样分析中的应用[J].干旱环境监测,2004,18(4):247-249.
[4]周京霞,游建南. CL-TBP萃淋树脂分离分光光度法连续测定铀和钍[J].湿法冶金,2001,20(4):204-212.
[5]董学畅,戴云,黄俊,等. 2-(H-酸偶氮)-4,5-二硝基苯酚与钍的显色反应研究[J].理化检验:化学分册,2002,38(11):562-563.
[6]罗道成,刘俊锋.三氯偶氮氯膦树脂相光度法测定环境水中微量钍[J].理化检验:化学分册,2006,42(10):871-872.
[7]王雅玲,王霞,张晓华,等.电感耦合等离子体质谱法测定饮用水中15种稀土元素[J].环境监测管理与技术,2013,25(1):37-39.
[8]潘洁,刘建华,董冲,等.电感耦合等离子体质谱法测定水中钍[J].辐射防护,2016,36(6):413-416.
[9]中华人民共和国卫生部. GB 14883. 7—94食品中放射性物质检验天然钍和铀的测定[S].北京:中国标准出版社,1994.
[10]国家环境保护总局. HJ/T 61—2001辐射环境监测技术规范[S].北京:中国标准出版社,2001.
[11]王瑞俊,段媛媛,高泽全,等.放射性平行样品结果处理的探讨[J].环境监测管理与技术,2016,28(5):66-71.
[2]余耀仙.水中钍的分析方法[J].辐射防护,1989,9(1):47-51.
[3]郑洁,金家伟,李建辉.铀、钍联合分析技术在水样分析中的应用[J].干旱环境监测,2004,18(4):247-249.
[4]周京霞,游建南. CL-TBP萃淋树脂分离分光光度法连续测定铀和钍[J].湿法冶金,2001,20(4):204-212.
[5]董学畅,戴云,黄俊,等. 2-(H-酸偶氮)-4,5-二硝基苯酚与钍的显色反应研究[J].理化检验:化学分册,2002,38(11):562-563.
[6]罗道成,刘俊锋.三氯偶氮氯膦树脂相光度法测定环境水中微量钍[J].理化检验:化学分册,2006,42(10):871-872.
[7]王雅玲,王霞,张晓华,等.电感耦合等离子体质谱法测定饮用水中15种稀土元素[J].环境监测管理与技术,2013,25(1):37-39.
[8]潘洁,刘建华,董冲,等.电感耦合等离子体质谱法测定水中钍[J].辐射防护,2016,36(6):413-416.
[9]中华人民共和国卫生部. GB 14883. 7—94食品中放射性物质检验天然钍和铀的测定[S].北京:中国标准出版社,1994.
[10]国家环境保护总局. HJ/T 61—2001辐射环境监测技术规范[S].北京:中国标准出版社,2001.
[11]王瑞俊,段媛媛,高泽全,等.放射性平行样品结果处理的探讨[J].环境监测管理与技术,2016,28(5):66-71.