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    高分辨电感耦合等离子体质谱法测定含钌单晶高温合金中的铟及钌干扰的消除

    HR-ICP-MS Determination of Indium in Single Crystal Superalloy Containing Ru and Elimination of Interference from Ruthenium

    • 摘要: 建立了高分辨电感耦合等离子体质谱法(HR-ICP-MS)测定含钌单晶高温合金中铟含量的方法,并研究了铟测定时可能存在的质谱干扰。钼的氧化物离子对113In的质谱干扰很严重;钌的氧化物离子对115In有一定程度的干扰,但其产生的干扰量与钌在样品中的含量呈线性关系,可通过建立的校正方程扣除,故选择115In作为铟检测同位素。0.1 g样品中加入体积比为3∶1的盐酸-硝酸混合溶液9 mL和氢氟酸1 mL,在80℃下常压消解60 min,用水稀释至250 mL,用HR-ICP-MS在低(分辨率为300)、中(分辨率为4 000)、高(分辨率为10 000)等3种分辨率模式下测定115In含量,用高纯镍的消解液配制的标准溶液系列制作标准曲线。铟的质量分数在2 μg·g-1以内与其对应的响应值呈线性关系,检出限(3s)分别为0.002 μg·g-1(低分辨率),0.004 μg·g-1(中分辨率)和0.009 μg·g-1(高分辨率)。对标准物质(GBW 01636)进行分析,测定值与认定值基本一致。对样品进行加标回收试验,所得回收率为76.0%~90.0%,测定值的相对标准偏差(n=5)均小于3.0%。

       

      Abstract: A method for the determination of In in single crystal superalloy containing Ru was established by HR-ICP-MS, and the possible MS interference in the determination of In was studied. MS interference from the ion of Mo oxide to 113In was very serions; MS interference from the ion of Ru oxide to 115In was found in a certain extent, the amount of interference produced was linearly related to the content of Ru in the sample, which could be eliminated by correction equation. Based on these facts, 115In was selected for detection. 0.1 g of sample was digested with 9 mL of hydrochloric acid and nitric acid with a volume ratio of 3:1 and 1 mL hydrofluoric acid at 80℃ under normal pressure for 60 min, and the digestion solution obtained was diluted to 250 mL with water. HR-ICP-MS was used to determine the content of 115In at three resolution modes, including low resolution of 300, medium resolution of 4 000 and high resolution of 10 000. Standard solution series were prepared by high-purity nickel digestion solution. The mass fractions of In had a linearity relationship with its corresponding response values within 2 μg·g-1, with detection limits (3s) of 0.002 μg·g-1 (for low resolution), 0.004 μg·g-1 (for medium resolution) and 0.009 μg·g-1 (for high resolution). The standard material (GBW 01636) was analyzed, and the determined values were consisted with the certified values. The sample was used in the spiked recovery test, giving values of recovery in the range of 76.0%-90.0%, and RSDs (n=5) of the determined values were less than 3.0%.

       

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