电感耦合等离子发射光谱法测定三元乙丙橡胶中钒

Determination of vanadium in ethylene propylene diene monomer by inductively coupled plasma optical emission spectrometry

建立电感耦合等离子发射光谱法测定三元乙丙橡胶中金属钒含量的方法。样品经高温灰化、溶解后,以1.0%的硝酸溶液进行稀释,射频功率为1 200 W,分析谱线为292.401 nm,等离子体气为氩气,流量为15.0 L/min,辅助气流量为1.50 L/min,雾化气为氩气,压力为200 kPa,观测高度为10 mm,采用等离子体原子发射光谱外标法进行定量测定。结果表明,在优化的实验条件下,钒元素的质量浓度在0~100 μg/L范围内与发射光谱强度呈良好的线性关系,线性相关系数为0.999 6,检出限为2.5 μg/L。测定结果的相对标准偏差均小于1.0 %(n=7),加标回收率为97.5%~100.5%。该方法可以替代紫外分光光度法,用于绝热层用ENB型三元乙丙橡胶中金属钒含量的测定。

A method for the determination of vanadium in ethylene propylene diene monomer(EPDM) by inductively coupled plasma optical emission spectrometry(ICP–OES) was established.After high temperature ashing and dissolution,the sample was diluted with 1.0% nitric acid solution.The RF power was 1 200 W,the analytical spectral line was 292.401 nm,the plasma gas was argon with the flow rate of 15.0 L/min,the auxiliary gas flow was 1.50 L/min,the atomization gas was argon with the pressure rate of 200 kPa,the observation height was 10 mm.The external standard method of plasma optical emission spectrometry was used for quantitative determination.The results show that under the optimized experimental conditions,the mass concentration of vanadium had a good linear relationship with the emission intensity in the range of 0–100 μg/L,the linear correlation coefficient was 0.999 6,and the detection limit was 2.5 μg/L.The relative standard deviation of the determination results was less than 1.0%(n=7),and the recovery was 97.5%–100.5%.The method can be used to determine the content of metal vanadium in ENB EPDM rubber for thermal insulation instead of ultraviolet spectrophotometry.