钇铝合金钇、铝联合测定方法

Combined determination of yttrium and aluminum

试料经盐酸溶解,40%氢氧化钠溶液调至沉淀出现并过量20 mL,煮沸,碱分离,保留沉淀和滤液。沉淀用盐酸酸化,定容、干过滤,取适量溶液用抗坏血酸还原Fe^(3+),乙酰丙酮掩蔽少量铝干扰元素,pH=5.5时,以二甲酚橙作指示剂,用EDTA标准溶液测定钇的含量。滤液定容,取适量溶液,加入过量EDTA,在pH=5~6时铝与EDTA定量络合。硫酸铜标准滴定溶液滴定过量的EDTA,氟盐取代与铝络合的EDTA,以吡啶基偶氮萘酚(PAN)为指示剂,用硫酸铜标准滴定溶液滴定,计算铝的质量分数。

The test material was dissolved by hydrochloric acid,40%sodium hydroxide solution was adjusted to precipitate and an excess of 20 mL,boiled,alkali separation,reserving precipitation and filtrate.Precipitation acidized with hydrochloric acid,constant volume.After dry filtration,appropriate amount of solution was taken to reduce Fe3+with ascorbic acid,and a small amount of aluminum interference element was masked by acetyl acetone.When pH=5.5,xylenol orange was used as indicator,and the content of yttrium was determined by EDTA standard solution.The filtrate volume was fixed,appropriate amount of solution was taken,and excessive EDTA was added.When pH=5~6,aluminum and EDTA were quantitatively complexed.The excess EDTA was titrated with copper sulfate standard titration solution,and the EDTA complexed with aluminum was replaced by fluorine salt.The mass fraction of aluminum was calculated by using pyridinyl azonaphthol(PAN)as indicator.