对氯苯基荧光酮分光光度法测定锌渣中痕量镓
Spectrophotometric Determination of Trace Amounts of Gallium in Zinc Slag with p-Chloro-phenylfluorone in the Presence of CTMAB
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摘要: 在表面活性剂十六烷基三甲基溴化铵存在下,镓(Ⅲ)与对氯苯基荧光酮形成红色的三元络合物.显色体系稳定,最大吸收波长为571 nm,表观摩尔吸光率为1.17×105L·mol-1·cm-1.镓(Ⅲ)质量浓度在8 μg/25 mL以内遵循比耳定律.利用磷酸三丁酯-煤油萃取镓后,用氯化铵溶液反萃取,能有效地消除干扰元素的影响,提高方法的选择性和灵敏度.方法用于锌渣等样品中痕量镓的测定,得到回收率与相对标准偏差值依次为97.6%~102.5%和1.6%~2.6%之间.Abstract: In an acetate buffer medium of pH 5.5,a stable red colored complex was formed between gallium(Ⅲ) and p-chlorophenylfluorone (p-ClPF) in the presence of CTMAB which remarkably sensitized the color reaction,giving a bathochromic shift from (λmax) 530 nm of the complex in the absence of CTMAB to (λmax) 571 nm in the presence of CTMAB and making an increase of molar absorptivity (ε571=1.17×105L·mol-1·cm-1) about 10 times greater. Beer′s law was kept in the range with in 8 μg of Ga(Ⅲ) per 25 mL of solution. In its application to the analysis of zinc slag,a preliminary separation of Ga(Ⅲ) from the interfering ions,by TBP-kerosene extraction and NH4Cl solution-back extraction of Ga(Ⅲ) was necessary to improve the selectivity of the method. Recovery and RSD′s obtained in the analysis of substantial samples of zinc slag and crude zinc oxide were in the ranges of 97.6%-102.5% and 1.6%-2.6% respectively.