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    微波消解-电感耦合等离子体原子发射光谱法测定钛及钛合金中19种元素的含量

    Determination of 19 Elements in Titanium and Titanium Alloy by Inductively Coupled Plasma Atomic Emission Spectrometry with Microwave Digestion

    • 摘要: 考察了消解方式、消解酸体系、升温时间和目标温度对样品消解效果的影响,提出了微波消解-电感耦合等离子体原子发射光谱法(ICP-AES)同时测定钛及钛合金中Fe、Si、Mn、Mo、B、Al、Sn、Cr、V、Zr、Mg、Nb、Pd、Ni、Ta、W、Nd、Ru、Cu等19种元素含量的方法。取0.100 0 g钛及钛合金样品置于聚四氟乙烯消解罐中,再加入8.0 mL 33%(体积分数)盐酸溶液、3.0 mL 25%(体积分数)氢氟酸溶液、1.0 mL 50%(体积分数)硝酸溶液和0.5 mL高氯酸,将其置于微波消解仪于最高消解温度120 ℃下保持10 min,冷却至室温,用水将消解液定容至50 mL,采用ICP-AES测定质量分数不大于1.0%的元素,将样品溶液稀释10倍,同法测定质量分数大于1.0%的元素。结果表明,19种元素的质量浓度在一定范围内与对应的响应强度呈线性关系,检出限(3s)为0.006~0.033 mg·L−1。对4种钛合金标准样品和3种钛合金实际样品进行分析,并与标准方法GB/T 4698系列的测定结果进行对比,结果显示本方法的测定值与认定值基本一致。以两种钛合金标准样品和两种钛合金实际样品为研究对象进行精密度试验,每个样品平行测定5次,测定值的相对标准偏差均小于4.0%。

       

      Abstract: The effects of digestion method, digestion acid system, heating up time, and target temperature on sample digestion efficiency were investigated in this experiment. A method was proposed for simultaneous determination of 19 elements, including Fe,Si, Mn, Mo, B, Al, Sn, Cr, V, Zr, Mg, Nb, Pd, Ni, Ta, W, Nd, Ru, and Cu in titanium and titanium alloy by inductively coupled plasma atomic emission spectrometry(ICP-AES) with microwave digestion. 0.100 0 g of the titanium or titanium alloy sample was placed into a polytetrafluoroethylene digestion tank, and then 8.0 mL of 33%(volume fraction) hydrochloric acid solution, 3.0 mL of 25%(volume fraction) hydrofluoric acid solution, 1.0 mL of 50%(volume fraction) nitric acid solution, and 0.5 mL of perchloric acid were added. The mixture was placed into a microwave digestion instrument, keeping for 10 min at the highest digestion temperature of 120 ℃. After cooling to room temperature, the digestion solution was made its volume up to 50 mL with water, and the elements with mass fraction not exceeding 1.0% were detemined by ICP-AES. The sample solution was diluted 10 times and the elements with mass fraction greater than 1.0% were detemined by the same method. As shown by the results, linear relationships between the corresponding response intensity and mass concentration of 19 elements were found in definite ranges, with detection limits(3s) of 0.006-0.033 mg·L−1. Four titanium alloy standard samples and three actual titanium alloy samples were analyzed, and the obtained results were compared with those of the standard method GB/T 4698 series. It was shown that the determined values of this method were basically consistent with the certified values.Test for precision was made on two standard samples and two actual samples of titanium alloys. Each sample was determined five times in parallel, with RSDs of the determined values less than 4.0%.

       

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