应用化学 ›› 1984, Vol. 0 ›› Issue (3): 25-29.

• 研究论文 • 上一篇    下一篇

多元稀土薄膜的微量化学分析法(YSmLuCa)3(FeGe)5O12原子比值

胡承苓, 盛娟娟, 陈荷莲, 汪咪珍   

  1. 中国科学院上海冶金研究所
  • 收稿日期:1984-01-23 修回日期:1984-03-05 出版日期:1984-09-10 发布日期:1984-09-10

MICROCHEMICAL DETERMINATION OF ELEMENTS IN BUBBLE GARNET FILM:THE ATOMIC RATIO IN(YSmLuCa)3(FeGe)5O12

Hu Chengling, Sheng Juanjuan, Chen Helian, Wang Mizhen   

  1. Institute of Metallurgy, Academia Sinica, Shanghai
  • Received:1984-01-23 Revised:1984-03-05 Published:1984-09-10 Online:1984-09-10

摘要: 本法解决了薄膜取样问题,以及稀土与非稀土元素的分离和测定,从而确定了薄膜组份的原子比值。方法的准确度与精密度都达到要求,并可为非破坏性测定提供校对数据。本法也适用于其他类型的多元稀土薄膜的测定。

Abstract: Samples of bubble films upon gadolinium-gallium garnet substract were dissolved in conc. nitric and 18N sulfuric acids mixture (2:1). The resulting solution was used for following determinations.(a)Chelometric micro titration of iron with EDTA using N-benzoyl-N-phenylhydroxylamine as indicator. Iron was also determined spectrophotometrically with o-phena-nthroline. (b) Calcium was determined chelometrically with cyclohexanedia-minetetraacetic acid (CYDTA), after removal of gallium, germanium and iron by extraction with butylacetate from 7N HCl medium and titration of total rare earths with EDTA at pH5, using xylenol orange as indicator.The latter should be destroyed by saturated bromine water before calcium titration. (c) Germanium was determined spectrophotometrically with fluoronecetyltrimethylammonium bromide (CTAB) at 506 nm. (d) The separation and determination of gadolinium, lutetium, samarium and yttrium: the rare earths were extracted with 0.5% 1-phenyl-3-methyl-4-benzoylpyrazol-5-one in benzene and then separated by reversed-phase column chromato-graphy. The column was filled with silanized silicagel (100-00mesh) impregnated with 2-ethyl-hexylphosphoric acid mono-2-ethylhexylester and the 3 RE were eluted subsequently by HCl of different concentration. They were finally determined spectrophotometrically with arsenazo Ⅲ. The results from two film samples were. given in the paper for illustration.