滴定法测定矿物中铀
穆佩娟1,程文康2
1.中陕核工业集团综合分析测试有限公司,西安 710024; 2.西安西北有色地质研究院有限公司,西安 710054
Determination of uranium in minerals by titration
穆佩娟1,程文康2
1. China Shaanxi Nuclear Industry Group Comprehensive Analysis and Testing Co., Ltd., Xi'an 710024, China; 2. Xi'an Northwest Nonferrous Geological Research Institute Co., Ltd., Xi'an 710054, China
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。
Abstract: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.
关键词:滴定法;铀;选冶联合流程;氯化亚锡;二苯胺
Keywords:titration; uranium; beneficiation-metallurgy combination process; stannous chloride; diphenylamine
本文引用格式:
穆佩娟,程文康.滴定法测定矿物中铀[J].化学分析计量,2018,27(5):59-63.
MU P J,CHENG W K. Determination of uranium in minerals by titration[J]. Chemical analysis and meterage,2018,27(5):59-63.
相似文章: