高铍铍铝合金中铍含量的测定
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摘要
高铍铍铝合金试样以盐酸溶解,以EDTA为掩蔽剂,在pH=9~10条件下使铍转化为氢氧化铍沉淀,沉淀分离净化后,以酚酞为指示剂,以氟化钾与氢氧化铍反应生成氟铍酸钾络合物并析出相应的等当量的碱,用稀盐酸滴定至无色为终点。经试样分析,相对标准偏差RSD<1%,标准加入回收试验,回收率为98%~103%。方法准确可靠,简便稳定,适用于高铍铍铝样品中铍的测定。
High beryllium aluminum alloy samples dissolved in hydrochloric acid,using EDTA as a masking agent,under the condition of pH = 9 ~ 10 made into beryllium hydroxide precipitation,precipitation separation and purification,using phenolphthalein as indicator,with potassium fluoride and hydrogen induced reaction of fluoride potassium complexes,and generate the corresponding alkali in dilute hydrochloric acid titration to colorless as the end point. After sample analysis,the relative standard deviation is RSD < 1%,the standard is added to the recovery test,and the recovery rate is 98% ~ 103%. The method is accurate,reliable,simple and stable,and is suitable for the determination of beryllium in beryllium aluminum samples with high beryllium.
High beryllium aluminum alloy samples dissolved in hydrochloric acid,using EDTA as a masking agent,under the condition of pH = 9 ~ 10 made into beryllium hydroxide precipitation,precipitation separation and purification,using phenolphthalein as indicator,with potassium fluoride and hydrogen induced reaction of fluoride potassium complexes,and generate the corresponding alkali in dilute hydrochloric acid titration to colorless as the end point. After sample analysis,the relative standard deviation is RSD < 1%,the standard is added to the recovery test,and the recovery rate is 98% ~ 103%. The method is accurate,reliable,simple and stable,and is suitable for the determination of beryllium in beryllium aluminum samples with high beryllium.
引文
[1]李军义,王东新,刘兆刚,等.铍铝合金的制备工艺与应用进展[J].稀有金属,2014,38(6):283-290.
[2]刘孝宁,马世光.铍铝合金的研究与应用[J].稀有金属,2003,27(1):62-65.
[3]YS/T 807.7-2012,铝中间合金化学分析方法[S].
[4]张雨平.用铍试剂Ⅲ光度法测定铝-铍中间合金中铍含量[J].轻合金加工技术,2001,29(4):43-45.
[5]YS/T 426.1-2000,锑铍芯块化学分析方法[S].
[2]刘孝宁,马世光.铍铝合金的研究与应用[J].稀有金属,2003,27(1):62-65.
[3]YS/T 807.7-2012,铝中间合金化学分析方法[S].
[4]张雨平.用铍试剂Ⅲ光度法测定铝-铍中间合金中铍含量[J].轻合金加工技术,2001,29(4):43-45.
[5]YS/T 426.1-2000,锑铍芯块化学分析方法[S].