当代化工
噹代化工
당대화공
CONTEMPORARY CHEMICAL INDUSTRY
2013年
5期
705-708
,共4页
付文慧%葛艳梅%董贵斌%王玉兰
付文慧%葛豔梅%董貴斌%王玉蘭
부문혜%갈염매%동귀빈%왕옥란
氯化稀土%氧化铈%硫酸亚铁铵滴定法
氯化稀土%氧化鈰%硫痠亞鐵銨滴定法
록화희토%양화시%류산아철안적정법
Rare earth chloride%Cerium oxide%Ammonium ferrous sulfate titrimetric method
硫酸亚铁铵滴定法是测定稀土矿石和矿物中氧化铈含量的常用方法，其测定范围较宽为0.1%～50%氧化铈。试样在酸性溶液中，用过硫酸铵、高氯酸、铋酸钠等氧化剂将低价态的铈氧化成高价态，然后用适当浓度的硫酸亚铁铵标准溶液进行滴定。其实验分析操作过程主要包括试样的溶解、氧化、滴定三个部分。以GB/T16484-2009为主要指导方法，同时结合以浓H2SO4作为溶剂的硫酸亚铁铵滴定法，分别选用过硫酸铵和高氯酸作为氧化剂，邻菲罗啉和苯代邻氨基苯甲酸作为滴定指示剂，对取样量、溶矿方法、氧化条件、氧化时间、指示剂选择等多方面因素进行方法研究试验，确定方法最佳试验条件，从而有效解决了硫酸亚铁铵滴定法测定氯化稀土中氧化铈含量测试结果不稳定性和重现性不强等诸多问题，提高了方法的准确度和精密度。
硫痠亞鐵銨滴定法是測定稀土礦石和礦物中氧化鈰含量的常用方法，其測定範圍較寬為0.1%～50%氧化鈰。試樣在痠性溶液中，用過硫痠銨、高氯痠、鉍痠鈉等氧化劑將低價態的鈰氧化成高價態，然後用適噹濃度的硫痠亞鐵銨標準溶液進行滴定。其實驗分析操作過程主要包括試樣的溶解、氧化、滴定三箇部分。以GB/T16484-2009為主要指導方法，同時結閤以濃H2SO4作為溶劑的硫痠亞鐵銨滴定法，分彆選用過硫痠銨和高氯痠作為氧化劑，鄰菲囉啉和苯代鄰氨基苯甲痠作為滴定指示劑，對取樣量、溶礦方法、氧化條件、氧化時間、指示劑選擇等多方麵因素進行方法研究試驗，確定方法最佳試驗條件，從而有效解決瞭硫痠亞鐵銨滴定法測定氯化稀土中氧化鈰含量測試結果不穩定性和重現性不彊等諸多問題，提高瞭方法的準確度和精密度。
류산아철안적정법시측정희토광석화광물중양화시함량적상용방법，기측정범위교관위0.1%～50%양화시。시양재산성용액중，용과류산안、고록산、필산납등양화제장저개태적시양화성고개태，연후용괄당농도적류산아철안표준용액진행적정。기실험분석조작과정주요포괄시양적용해、양화、적정삼개부분。이GB/T16484-2009위주요지도방법，동시결합이농H2SO4작위용제적류산아철안적정법，분별선용과류산안화고록산작위양화제，린비라람화분대린안기분갑산작위적정지시제，대취양량、용광방법、양화조건、양화시간、지시제선택등다방면인소진행방법연구시험，학정방법최가시험조건，종이유효해결료류산아철안적정법측정록화희토중양화시함량측시결과불은정성화중현성불강등제다문제，제고료방법적준학도화정밀도。
The ammonium ferrous sulfate titrimetric method is a common method for determination of cerium oxide content in rare earth ores and minerals, its measuring range is wide ( 0.1%~50%cerium oxide). Low valence cerium in samples is first oxidized into high valence state in acidic solution by using oxidants, such as ammonium persulfate, perchloric acid, sodium bismuthate and so on. And then ammonium ferrous sulfate standard solution with appropriate concentration is used to titrate. The experimental operation process includes three parts of sample dissolution, oxidation and titration. In this paper, taking GB/T16484-2009 as the main guidance method, combining with the ammonium ferrous sulfate titrimetric method with concentrated sulfuric acid as solvent, sample was determined by respectively using ammonium persulfate and perchloric acid as oxidant, phenanthroline and phenyl anthranilic acid as titration indicator. Effect of sampling amount, mineral dissolution method, oxidation condition, oxidation time, indicator selection and other factors on determination result was investigated, optimal experimental conditions were obtained, which can effectively solve the problems of instability test results and poor reproducibility in the determination of cerium oxide content in rare earth chloride by the ammonium ferrous sulfate titrimetric method, improve accuracy and precision of the method.
