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化学学报
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化学学报 ›› 1964, Vol. 30 ›› Issue (6): 562-569. 上一篇    下一篇

论文

α-羟基苯甲膦酸用作锆的沉淀剂

严仁荫, 容庆新, 刘秀英   

  1. 北京大学化学系
  • 投稿日期:1963-12-26 发布日期:2013-06-03

α-HYDROXYL α-TOLUENEPHOSPHONIC ACID AS A PRECIPITANT FOR ZIRCONIUM

YEN JEN-YIN, RONG QING-XIN, LIU XIU-YING   

  1. Department of Chemistry, Peking University
  • Received:1963-12-26 Published:2013-06-03

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α-羟基苯甲膦酸是锆的高选择性沉淀剂.在4N盐酸介质中只用两倍过量试剂即可将锆定量沉淀.其组成为Zr(C6H5CHOHPO3)2·xH2O.结晶水含量不固定,最后须灼烧成焦磷酸锆形式称重.可用于20-70毫克二氧化锆的测定.大多数金属离子甚至大量Mn(Ⅱ),Fe(Ⅲ),Ni不干扰.Ti(Ⅳ),Nb(Ⅴ),Ta(Ⅴ)可用过氧化氢及酒石酸掩蔽,只有钍干扰锆的测定.络合阴离子对沉淀的干扰较小,用七倍过量试剂沉淀锆时,在200毫升溶液中可以允许5克硫酸铵、5克柠檬酸、0.6克EDTA、2克酒石酸、0.2克草酸(相当于锆量八倍)存在而不干扰测定.0.7克氟化钠(相当于锆量十倍)用硼酸掩蔽,也不影响锆的测定.有上述阴阳离子与锆同时存在时,重沉淀可得满意结果.

α-Hydroxyl α-toluenephosphonic acid,being similar to mandelic acid in structure,has been found to be a highly specific and sensitive reagent for zirconium.It is easily prepared and is very soluble in water.From 4 N hydrochloric acid medium,the reagent precipitates immediately zirconium(hafnium),titanium,niobium and tantalum only.However,the latter three can be masked by hydrogen peroxide.Thorium is only slowly and partially precipitated at this acidity and is coprecipitated with zirconium.From 3-4 N hydrochloric acid media,zirconium is quantitatively precipitated with only two-fold excess of the precipitant while large excess is required in the case of mandelic acid.