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试样经酸分解后,加氢氟酸沉淀稀土,分离除去Ni,Mn,Fe,Co等元素;用硝酸和高氯酸破坏滤纸并溶解沉淀,经氨水分离再次沉淀稀土,过滤去除Ni,Co,M g等元素;用盐酸溶解沉淀,在p H 1.8~2.0的条件下用草酸沉淀稀土,以分残余离Ni,Co,Al等杂质,灼烧至恒重完成稀土总量测定。本方法适合稀土总量的测定范围为25.00%~45.00%,测定结果相对标准偏差在0.39%~0.44%之间,标准加入回收率为98.7%~102.3%。同时选择8家试验室进行数据比对,并将精密度数据进行正态分布检验、等精度检验和可疑值检验,检验结果均符合要求。采用本方法测定贮氢合金中的稀土总量准确、稳定,可用于仲裁判定。
After the sample is acid decomposed, hydrofluoric acid is used to precipitate the rare earth and the elements such as Ni, Mn, Fe and Co are separated and removed; the filter paper is dissolved by nitric acid and perchloric acid to dissolve the precipitate; the rare earth is precipitated again by ammonia water; , M g and other elements; dissolving the precipitate with hydrochloric acid, precipitating the rare earth with oxalic acid under the condition of p H 1.8-2.0, separating the residual impurities such as Ni, Co, Al and the like, and burning to constant weight to complete the determination of the total rare earth. The method is suitable for the determination of the total rare earth content of 25.00% ~ 45.00%, the relative standard deviation of determination results between 0.39% ~ 0.44%, the standard addition recovery was 98.7% ~ 102.3%. At the same time, eight laboratories were selected for data comparison, and the precision data were tested for normal distribution, such as accuracy test and suspicious value test, the test results were in line with the requirements. The method for determining the total amount of rare earth in hydrogen storage alloy is accurate and stable and can be used for arbitration judgment.