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    电感耦合等离子体质谱法测定纯铝中17种痕量元素

    Determination of 17 Trace Elements in Pure Aluminum by Inductively Coupled Plasma Mass Spectrometry

    • 摘要: 取0.1 g纯铝样品置于聚四氟乙烯烧杯中,加入3 mL盐酸,于80 ℃加热溶解,冷却,用水定容至50 mL。取5 mL上述溶液,用2%(体积分数)硝酸溶液定容至50 mL,在动能歧视碰撞模式、射频功率1 400 W、雾化气流量1.00 mL·min−1、碰撞气(氦气)流量3.5 mL·min−1的条件下采用电感耦合等离子体质谱法(ICP-MS)测定溶液中17种痕量元素(铜、锰、钛、镓、铬、镍、铋、铅、锡、钒、钡、铍、镉、钴、钼、锑、锶),选用铑为内标进行在线校正,基体匹配法定量。结果显示,17种痕量元素的质量分数在100 μg·g−1以内与对应的内标校正后的信号强度呈线性关系,检出限(3s)为0.001~0.75 μg·g−1。实际纯铝样品测定值的相对标准偏差(n=8)为0.50%~3.6%,按照标准加入法进行回收试验,回收率为91.4%~112%。方法用于分析实际纯铝样品,各元素的测定值与GB/T 20975.25—2020的基本一致。

       

      Abstract: The pure aluminum sample (0.1 g) was taken and placed in a polytetrafluoroethylene beaker, and 3 mL of hydrochloric acid was added, then the mixture was heated at 80 °C for dissolution. After cooling, the solution was made its volume up to 50 mL with water. 5 mL of aforementioned solution was taken and made its volume up to 50 mL with 2% (volume fraction) nitric acid solution. 17 trace elements (copper, manganese, titanium, gallium, chromium, nickel, bismuth, lead, tin, vanadium, barium, beryllium, cadmium, cobalt, molybdenum, antimony, and strontium) in the solution was determined by inductively coupled plasma mass spectrometry under the condition of kinetic energy discrimination collision mode, radio frequency power of 1400 W, atomization gas flow rate of 1.00 mL·min−1, and collision gas (helium) flow rate of 3.5 mL·min−1. Rhodium was selected as the internal standard for online correction, and the matrix matching method was used for quantification. As shown by the results, linear relationships between the corresponding signal intensities after internal standard correction and mass fractions of 17 trace elements were found within 100 μg·g−1, with detection limits (3s) in the range of 0.001‒0.75 μg·g−1. RSDs (n=8) of the determined values of the actual pure aluminum sample were in the range of 0.50%‒3.6%. Test for recovery was made according to the standard addition method, giving results in the range of 91.4%‒112%. The method was applied to the analysis of an actual pure aluminum sample, and the determined values of elements were basically consistent with those obtained by GB/T 20975.25—2020.

       

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