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    电感耦合等离子体原子发射光谱法测定高砷铅烟灰中铟的含量

    Determination of Indium in High Arsenic Lead Soot by Inductively Coupled Plasma Atomic Emission Spectrometry

    • 摘要: 提出了电感耦合等离子体原子发射光谱法(ICP-AES)测定高砷铅烟灰中铟含量的方法。取0.10~0.15 g样品置于250 mL烧杯中,加少量水润湿,加入5 mL盐酸在200 ℃电热板上溶解2 min,加入15 mL硝酸,在200 ℃电热板上浓缩至10 mL,冷却后,加入10 mL 1.5 g·L−1铬内标溶液,用水定容至200 mL,在325.606 nm处测量铟的发射强度,在267.716 nm处测量铬内标的发射强度。结果表明,铟的质量浓度在5~40 mg·L−1内与对应的发射强度与内标发射强度比呈线性关系,检出限(3s)为0.002 0%;4个样品的精密度试验所得测定值的相对标准偏差(n=11)均小于1.5%;对实际样品进行加标回收试验,回收率为99.2%~101%;采用标准加入法进行验证,测定值和本方法的基本一致。

       

      Abstract: A method for determination of indium in high arsenic lead soot by inductively coupled plasma atomic emission spectrometry (ICP-AES) was proposed. 0.10-0.15 g of the sample was taken into a 250 mL-beaker, and a little water was added to moisten. 5 mL of hydrochloric acid was added and the mixture was digested at 200 ℃ on a electric heating plate for 2 min. 15 mL of nitric acid was added, and the mixture was concentrated to 10 mL on a 200 ℃ electric heating plate. 10 mL of 1.5 g·L−1 chromium internal standard solution was added after the solution was cooled down. The sample solution was made its volume up to 200 mL with water. The emission intensity of indium was measured at 325.606 nm, and the emission intensity of chromium internal was measured at 267.716 nm. As shown by the results, linear relationship between the ratio of the corresponding emission intensity to the internal standard emission intensity and mass concentration of indium was found in the range of 5-40 mg·L−1, with detection limit (3s) of 0.002 0%. RSDs (n=11) of the determined values of test for precision on four samples were less than 1.5%. Test for the spiked recovery was made on actual samples, giving results in the range of 99.2%-101%. The standard addition method was used for verification, and the detemined values were basically consistent with those from this method.

       

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