高温水解–离子色谱法测定八氧化三铀中的氟和氯
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摘要
建立了高温水解–离子色谱法测定八氧化三铀中氟和氯含量的方法。对影响高温水解的因素进行了试验研究,水解温度为1 050℃,水浴温度为(85±1)℃,氩气流量为600 mL/min,水解时间为1 h。选用Ion Pac AG11–HC(50 mm×4 mm)阴离子保护柱和Ion Pac AS11–HC(250 mm×4 mm)阴离子分析柱对样品进行分离,以氢氧化钾溶液等度淋洗。在0~5.00μg/mL范围内,氟和氯均有良好的线性,相关系数(r~2)分别为0.999 9,0.999 4;检出限分别为3,4μg/g。氟和氯测定结果的相对标准偏差分别为4.72%,3.23%(n=6),加标回收率分别为97%~101%,95%~99%。该法操作简便、快速,适用于八氧化三铀中氟和氯的检测。
A method for the determination of fluorine and chlorine in triurannium octoxide(U_3O_8) by pyrohydrolyticion chromatography was established. The factors influencing hydrolysis at high temperature were examined and studied. Pyrohydrolytic temperature was 1 050 ℃, water bath temperature was(85±1) ℃, flow rate of argon was 600 mL/min, and hydrolysis time was 1 h. The chromatographic separation was performed on Ion Pac AG11–HC(50 mm×4 mm) guard column and Ion Pac AS11–HC(250 mm×4 mm) analytical column by using potassium hydroxide solution as eluent. In the range of 0–5.00 μg/mL, the linearity was obtained for fluorine and chlorine, the linear correlation cofficients(r~2) were 0.999 9, 0.999 4, and the detection limits were 3, 4 μg/g, respectively. The relative standard deviations of fluorine and chlorine detection results were 4.72%,3.23%(n=6),and the recoveries were 97%–101%, 95%–99%, respectively. The method is rapid and simple, and it is suitable for the determination of fluorine and chlorine in triurannium octoxide.
A method for the determination of fluorine and chlorine in triurannium octoxide(U_3O_8) by pyrohydrolyticion chromatography was established. The factors influencing hydrolysis at high temperature were examined and studied. Pyrohydrolytic temperature was 1 050 ℃, water bath temperature was(85±1) ℃, flow rate of argon was 600 mL/min, and hydrolysis time was 1 h. The chromatographic separation was performed on Ion Pac AG11–HC(50 mm×4 mm) guard column and Ion Pac AS11–HC(250 mm×4 mm) analytical column by using potassium hydroxide solution as eluent. In the range of 0–5.00 μg/mL, the linearity was obtained for fluorine and chlorine, the linear correlation cofficients(r~2) were 0.999 9, 0.999 4, and the detection limits were 3, 4 μg/g, respectively. The relative standard deviations of fluorine and chlorine detection results were 4.72%,3.23%(n=6),and the recoveries were 97%–101%, 95%–99%, respectively. The method is rapid and simple, and it is suitable for the determination of fluorine and chlorine in triurannium octoxide.
引文
[1]辛仁轩,王建强.色谱分离ICP-AES法测定高纯度八氧化三铀中的13种微量杂质[J].化学分析计量,2002(6):33-34.
[2]杜桂荣,牛洁,刘扬,等.ICP-OES法测定八氧化三铀中杂质元素钨[J].化学分析计量,2014(1):42-44.
[3]刘朝,张鑫,鄢飞燕,等.TBP萃淋树脂分离-ICP-OES法测定U3O8的杂质元素[J].铀矿冶,2016,35(2):138-141.
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[7]吴王锁,陈励权,许君政,等.萃取分离-化学光谱法测定UF4中18种微量杂质元素[J].原子能科学技术,1997,31(3):199-203.
[8]胡红美,郭远明,孙秀梅,等.离子选择电极法测定生活饮用水中氟化物[J].中国无机分析化学,2013,3(3):13-16.
[9]李中贤,赵灿方,刘小培,等.水中氟化物的氟试剂分光光度法测定[J].河南科学,2012,30(1):55-57.
[10]赵立晶,赵萍,魏月仙.流动分析-离子选择电极法测定水中痕量氟化物[J].分析化学,2011,390(10):1 526-1 530.
[11]佟琦,高丽华.莫尔法与自动电位滴定法测定水中氯离子含量的比较[J].工业水处理,2008(11):74-76.
[12]田秀君,線香芹.分光光度法测定水中微量的氯离子[J].仪器仪表与分析监测,2004(2):33-34.
[13]李红,王云娟.离子色谱法测定地下水中氯化物[J].全面腐蚀控制,2013(4):67-70.
[14]王芳,王海峰,徐建,等.高温燃烧水解-离子色谱法测定煤中的氟和氯[J].化学分析计量,2016,25(4):27-30.
[15]张黎辉,陈贵福.高温水解-离子色谱法测定核电级二氧化铀中的氟、氯、溴、硫[J].湿法冶金,2000,19(1):51-56.
[16]王春叶,王林根,曹淑琴.高温水解-离子色谱法测定重铀酸盐中的Cl-和SO42-[J].湿法冶金,2008,27(3):188-190.
[17]张芳.热水解离子色谱法测定岩石样品中的氯和硫[J].光谱试验室,1998,15(2):31-35.
[18]GB/T 13369-1992二氧化铀粉末和芯块中氯的测定:高温水解-离子选择性电极法[S].
[2]杜桂荣,牛洁,刘扬,等.ICP-OES法测定八氧化三铀中杂质元素钨[J].化学分析计量,2014(1):42-44.
[3]刘朝,张鑫,鄢飞燕,等.TBP萃淋树脂分离-ICP-OES法测定U3O8的杂质元素[J].铀矿冶,2016,35(2):138-141.
[4]朱留超,徐常昆,王同兴,等.八氧化三铀中杂质元素的电感耦合等离子体质谱分析方法研究[J].中国原子能科学研究院年报,2013(1):201-201.
[5]郭东发,伍朝辉,黄秋红,等.电感耦合等离子体质谱法测定二氧化铀和八氧化三铀粉末中的杂质元素[J].铀矿地质,1999,15(3):177-180.
[6]鄢飞燕,刘朝,张鑫,等.TBP萃淋树脂分离ICP-MS法测定八氧化三铀中的钍和锆[J].化学分析计量,2016,25(3):16-19.
[7]吴王锁,陈励权,许君政,等.萃取分离-化学光谱法测定UF4中18种微量杂质元素[J].原子能科学技术,1997,31(3):199-203.
[8]胡红美,郭远明,孙秀梅,等.离子选择电极法测定生活饮用水中氟化物[J].中国无机分析化学,2013,3(3):13-16.
[9]李中贤,赵灿方,刘小培,等.水中氟化物的氟试剂分光光度法测定[J].河南科学,2012,30(1):55-57.
[10]赵立晶,赵萍,魏月仙.流动分析-离子选择电极法测定水中痕量氟化物[J].分析化学,2011,390(10):1 526-1 530.
[11]佟琦,高丽华.莫尔法与自动电位滴定法测定水中氯离子含量的比较[J].工业水处理,2008(11):74-76.
[12]田秀君,線香芹.分光光度法测定水中微量的氯离子[J].仪器仪表与分析监测,2004(2):33-34.
[13]李红,王云娟.离子色谱法测定地下水中氯化物[J].全面腐蚀控制,2013(4):67-70.
[14]王芳,王海峰,徐建,等.高温燃烧水解-离子色谱法测定煤中的氟和氯[J].化学分析计量,2016,25(4):27-30.
[15]张黎辉,陈贵福.高温水解-离子色谱法测定核电级二氧化铀中的氟、氯、溴、硫[J].湿法冶金,2000,19(1):51-56.
[16]王春叶,王林根,曹淑琴.高温水解-离子色谱法测定重铀酸盐中的Cl-和SO42-[J].湿法冶金,2008,27(3):188-190.
[17]张芳.热水解离子色谱法测定岩石样品中的氯和硫[J].光谱试验室,1998,15(2):31-35.
[18]GB/T 13369-1992二氧化铀粉末和芯块中氯的测定:高温水解-离子选择性电极法[S].