在 pH 为6条件下，以过氧化氢为氧化剂，三氯化铁为沉淀剂，使红土镍矿浸出液中的Fe2＋和 Mn2＋氧化水解生成沉淀物；该沉淀物及其他干扰元素（如铜、铅、锌、钴、镍、铬、镉、铋等）用六次甲基四胺和铜试剂共沉淀而与钙分离。以盐酸羟胺掩蔽微量的锰而消除其干扰，用三乙醇胺和 L －半胱氨酸掩蔽残留的其他金属离子，在氢氧化钠溶液中，用钙试剂为指示剂，以 EDTA 络合滴定法测定钙。该方法对浸出液样品进行多次测定，相对标准偏差为7．10％～8．80％（n ＝6），加入标准物质的回收率在99％以上。
Under the condition of pH 6,Fe2 + and Mn2 + in the leaching solution of nickel laterites were oxidized to precipitate with hydrogen peroxide as oxidant and ferric chloride as precipitator.The precipitate and other impurities such as copper,lead,zinc,cobalt,nickel,chromium,cadmium,bismuth formed co-precipitation by hexamethylene tetra-mine and cupral,realizing the separation of calcium.Then trace manganese was masked by hydroxylamine hydrochlo-ride to eliminate its interference,while other residual metal ions were masked by triethanolamine and L-cysteine.The sodium hydroxide solution was added in the same solution to determine the content of calcium using calcon as indicator by EDTA complexometric titration.The proposed method was applied to the parallel determination of calcium in the leaching solution.The relative standard deviations(RSD,n =6)of determination results were 7.10 % to 8.80 %.The recoveries were higher than 99 % with the addition of standard substance.
参考文献
| [1] | 许祥红,王桂群,刘洪清,孙雪松,陈京魏.电感耦合等离子体原子发射光谱法测定铁矿石中Si,Ca,Mg,Mn,Al,P,V,Ti[J].冶金分析,2006(02):89-90. |
| [2] | 北京矿冶研究总院测试研究所.有色冶金分析手册[M].北京:冶金工业出版社,2004:210-214. |
| [3] | 北京矿冶研究总院分析室.矿石及有色金属分析手册[M].北京:冶金工业出版社,1990:123-128. |
| [4] | 武映梅,宋兆华.EDTA容量法测定炉渣中CaO、MgO时干扰元素的消除[J].南方金属,2004(05):29-31,47. |
| [5] | 张建珍,樊晓红,薛丽华.EDTA络合滴定法连续测定铁矿石中钙和镁[J].冶金分析,2011(08):74-78. |
| [6] | 林才顺.从湿法硫酸镍中去除锰、铁的新工艺研究[J].湿法冶金,2002(03):139-142. |
| [7] | 吴展,陈志友,侯琼英,李伟,陈志华,宁瑞.从粗硫酸镍溶液中净化分离铁砷试验研究[J].湿法冶金,2013(02):122-124. |
| [8] | Dean J A;魏俊发.兰氏化学手册[M].北京:科学出版社,2003:121-136. |
- 下载量()
- 访问量()
- 您的评分：
-
10%
-
20%
-
30%
-
40%
-
50%