电感耦合等离子体原子发射光谱法测定核级316不锈钢中痕量铈

Determination of Trace Cerium in Nuclear Grade 316 Stainless Steel by Inductively Coupled Plasma Atomic Emission Spectrometry

提出了电感耦合等离子体原子发射光谱法(ICP-AES)测定核级316不锈钢中痕量铈的方法。取0.100 0 g样品于烧杯中,加入15 m L现配体积比为1∶3∶4的硝酸-盐酸-水混酸溶液,置于150℃电热板上消解30 min,完全溶解后加入5 m L 30%(质量分数)过氧化氢溶液,恒温3 min后取下冷却至室温,用水定容至100 m L。设置仪器射频功率为1 150 W,雾化气流量为0.45 L·min^(-1),测量铈元素在404.076 nm分析谱线处的响应强度,基质匹配法定量。结果表明:铈的质量浓度在100 mg·L^(-1)以内与对应的响应强度呈线性关系,检出限(3s)为0.000 4%。4个样品精密度试验所得测定值的相对标准偏差(n=10)均小于5.0%。按照标准加入法进行回收试验,回收率为95.5%~103%;采用GH56(屑样)铁镍基标准物质进行准确度验证,测定值与认定值基本一致。

A method for the determination of trace cerium in nuclear grade 316 stainless steel by inductively coupled plasma atomic emission spectrometry(ICP-AES)was proposed.0.1000 g of the sample was taken into the beaker,and 15 mL of mixed acid solution consisted of nitric acid-hydrochloric acid-water at volume ratio of 1∶3∶4 was added.The mixture was digested on the 150℃electric heating plate for 30 min.After the sample was completely dissolved,5 mL of 30%(mass fraction)hydrogen peroxide solution was added,and the mixture was kept constant temperature for 3 min,and then cooled to room temperature.The sample solution was made up to 100 mL by water.The response intensity of cerium at 404.076 nm of analysis spectral lines was measured with the radio frequency power of the instrument of 1150 W and the atomizing gas flow of 0.45 L·min-1,and the matrix matching method was used for quantification.It was shown that linear relationship between mass concentration and response intensity was kept within 100 mg·L-1,with detection limit(3s)of 0.0004%.RSDs(n=10)of the determined values of test of four samples for precision were less than 5.0%.Test for recovery was made according to the standard addition method,giving results in the range of 95.5%-103%.GH56(chip sample)iron-nickel based standard substance was used for accuracy verification,and the determined values were basically consistent with the certified values.