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    电感耦合等离子体光谱法测定纳米二氧化钛及钛基物料中痕量钒

    ICP-AES Determination of Trace Amounts of Vanadium in Nano-Titanium Dioxide and Other Titanium-Base Materials

    • 摘要: 对用电感耦合等离子体光谱法(ICP-AES)测定以钛为基体元素的物料(如二氧化钛、金红石等)中痕量钛的最佳分析条件作了研究.结果表明选择波长为310.023 nm的谱线作为分析线可避免大量钛的严重干扰.在应用适宜的同步背景校正条件下,钛及其他常见元素的干扰均能有效消除,而且在制备钒的标准工作曲线时也毋需作基体匹配.试样用HCl-HF-H2SO4混合酸消解,经硫酸冒烟逐除氢氟酸后用HCl(5+95)定容至一定体积.此方法可测定质量分数为2×10-4%~5%钒的试样,不需要任何富集或分离步骤.用不同含钒量(0.01%~0.20%)的试样作精密度试验,所得结果的RSD(n=8)值均小于3%,方法的检出限为0.01 mg·L-1,回收率在99%~106%之间.

       

      Abstract: Optimum condition for the ICP-AES determination of trace amounts of vanadium in samples with titanium as matrix element,e.g.,titanium dioxide,rutile and etc.,was studied.It was found that by choosing wavelength 310.023 nm as the analytical spectral line,the serious interference of titanium(Ⅳ) was avoided.By applying the synchronous backgroud correction,interferences of Ti(Ⅳ) and other commonly encountered ions were effectively eliminated.And also no matrix matching was necessary in the preparation of working curve of vanadium.The sample was digested with HCl-HF-H2SO4 acid mixture and fumed with H2SO4 to expel HF,and finally made up to a definite volume with HCl (5+95).Vanadium content in the range from (w) 2×10-4% to 5% was determined by the proposed method without any procedure of enrichment or separation.Test for precision with samples of different vanadium contents (0.01%-0.20%) gave RSD′s (n=8) less than 3%.Detection limit of this method was found to be 0.01 mg·L-1.Recoveries found were in the range of 99%-106%.

       

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