滴定法测定矿物中铀
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摘要
对测定矿物中铀含量的滴定法进行改进。在采用规程EJ 267.3–1984 《铀矿石中铀的测定三氯化钛还原/钒酸铵氧化滴定法》的方法测定选冶流程样品中的铀含量时,首先在550℃焙烧样品90 min,继而采用盐酸–双氧水–氢氟酸混酸体系和盐酸–氯化亚锡–磷酸混酸体系两步法溶样,将13 mL磷酸预先加入到锥形瓶中,以降低样品溶液的黏度,从而使过滤时间缩短10 min以上。选用二苯胺作指示剂,二氯化锡作还原剂,改善了终点灵敏度。解决了钼干扰和滴定过量的问题。该方法测定结果的相对标准偏差为0.43%～0.90%(n=5),回收率为99.9%～100.6%。该方法已用于批量样品检测,效果良好。
Improvement of the titration method for determining uranium in minerals was made. When uranium in ore was determined by EJ 267.3–1984 Determination of Uranium in Uranium Ore Titanium Trichloride Reduction/Ammonium Vanadate Oxidation Titration Method, the sample was roasted for 90 min at 550℃ at first, and then dissolved with hydrochloric acid–hydrogen peroxide–hydrofluoric acid mixed acid system and hydrochloric acid–stannous chloride–phosphoric acid mixed acid system in turn. 13 mL phosphoric acid was pre-added into the cone bottle to reduce the viscosity of the sample solution, so that the filtering time was shorten at least 10 min. By using diphenylamine as indicator and stannous chloride as reducing agent, the end-point sensitivity was improved. The problems of molybdenum interference and excessive titration were solved. The relative standard deviation of determination results was 0.43%–0.90%(n=5), the recovery was 99.9%–100.6%. The method has been used for batch sample detection with the good results.
Improvement of the titration method for determining uranium in minerals was made. When uranium in ore was determined by EJ 267.3–1984 Determination of Uranium in Uranium Ore Titanium Trichloride Reduction/Ammonium Vanadate Oxidation Titration Method, the sample was roasted for 90 min at 550℃ at first, and then dissolved with hydrochloric acid–hydrogen peroxide–hydrofluoric acid mixed acid system and hydrochloric acid–stannous chloride–phosphoric acid mixed acid system in turn. 13 mL phosphoric acid was pre-added into the cone bottle to reduce the viscosity of the sample solution, so that the filtering time was shorten at least 10 min. By using diphenylamine as indicator and stannous chloride as reducing agent, the end-point sensitivity was improved. The problems of molybdenum interference and excessive titration were solved. The relative standard deviation of determination results was 0.43%–0.90%(n=5), the recovery was 99.9%–100.6%. The method has been used for batch sample detection with the good results.
引文
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[11]王海塔,师留印,杨剑飞,等.某低品位难选铀钼矿钙化焙烧浸出工艺试验研究[J].铀矿冶,2016,35(3):191–194.
[12]陆诗洁、游建南.铀钼分离工艺中铀和钼的测定(Ⅰ)铀的测定[J].湿法冶金,2002(1):49–55.
[13]杨金辉,王道贤.硫酸–亚钛–钒酸铵滴定法测定矿石中铀[J].铀矿开采,2001(1):74–78,73.
[14]李耀国,冯张生.钼精矿中铀的测定[J].世界核地质科学,2010,27(1):55–57.
[15]刘立坤,郭冬发,黄秋红.岩石矿物中铀钍的分析方法进展:湿法化学法[J].中国无机分析化学,2012(2):6–9.
[2]徐卫东,孙荣,朱霞萍,等.亚钛还原钒酸铵微量滴定法测定矿石中微量铀方法的改进[J].岩矿测试,2010,29(3):325–327.
[3]江玲,邓秀文,颜世栋,等.岩石矿物中的铀的分析方法研究进展[J].广东化工,2017,18:130,140.
[4]倪湖权.原子荧光光谱法测定汞、银、稀土元素及铀的研究[D].广西:广西大学,2014.
[5]宋虎跃,吴勇民,郝佳瑞.钒酸铵滴定铀的原理及实验条件讨论[J].化工之友,2007(13):33–34.
[6]蔡金芳,张富平,张洁,等.砂岩型铀矿勘查样品中铀的野外快速测定方法研究[J].铀矿地质,2005,21(3):177–182.
[7]康瑾瑜,纪玉玲.微量滴定法测定微痕量铀的研究及应用[J].干旱环境监测,1998(4):210–212,239.
[8]李玉成.钒金试剂Ⅱ为指示剂钒酸铵滴定法测定岩矿、天然水、海水、雨水中的铀[J].铀矿地质,1993(4):58–62.
[9]杨金辉,谭海明,胡凯光,等.硫酸–亚钛–钒酸铵滴定法测定矿石中铀[J].铀矿冶,2004(8):147–150.
[10]丁红芳,曹淑琴.铀矿石中铀测定结果的不确定度评定[J].化学分析计量,2004,13(5):9–11,21.
[11]王海塔,师留印,杨剑飞,等.某低品位难选铀钼矿钙化焙烧浸出工艺试验研究[J].铀矿冶,2016,35(3):191–194.
[12]陆诗洁、游建南.铀钼分离工艺中铀和钼的测定(Ⅰ)铀的测定[J].湿法冶金,2002(1):49–55.
[13]杨金辉,王道贤.硫酸–亚钛–钒酸铵滴定法测定矿石中铀[J].铀矿开采,2001(1):74–78,73.
[14]李耀国,冯张生.钼精矿中铀的测定[J].世界核地质科学,2010,27(1):55–57.
[15]刘立坤,郭冬发,黄秋红.岩石矿物中铀钍的分析方法进展:湿法化学法[J].中国无机分析化学,2012(2):6–9.