电感耦合等离子体原子发射光谱法测定高钡光学玻璃中锶的含量

Determination of Strontium in High Barium Optical Glass by Inductively Coupled Plasma Atomic Emission Spectrometry

将0.100 0 g样品和0.500 0 g氟化氢铵粉末置于密闭消解罐中,加入几滴水润湿,再用10 mL盐酸、5 mL硝酸和2 mL高氯酸于200℃消解2.0 h,冷却后于200℃蒸发至近干。残渣用5 mL硝酸提取6~8 min,用水定容至100 mL,在分析谱线460.733 nm下采用电感耦合等离子体原子发射光谱法测定其中锶的含量,以两点校正法进行背景修正,用基体匹配的标准溶液系列绘制工作曲线。结果表明,锶的质量浓度在0.50~20.00 mg·L^(-1)内与对应的响应强度呈线性关系,检出限(3s)为5μg·g^(-1)。对某一样品测定12次,测定值的相对标准偏差为2.5%。对实际样品进行加标回收试验,回收率分别为98.0%和101%。

0.100 0 g of the sample and 0.500 0 g of ammonium hydrogen fluoride powder were placed into a closed digestion tank, and few drops of water were added to wet. The mixture was digested at 200 ℃ for 2.0 h in 10 mL of hydrochloric acid, 5 mL of nitric acid and 2 mL of perchloric acid, and then evaporated to near dryness at 200 ℃ after cooling. The residue was extracted in 5 mL of nitric acid for 6-8 min, and the volume was made up to 100 mL with water. Strontium in the solution was determined by inductively coupled plasma atomic emission spectrometry under the analytical spectral line of 460.733 nm. The background was corrected by two-point correction method, and the working curve was drawn with the standard solution series matched with the matrix. As shown by the results, linear relationship between the mass concentration of strontium and the corresponding response intensity was found in the range of 0.50-20.00 mg·L^(-1), with detection limit(3s) of 5 μg·g^(-1). Strontium in a sample was determined 12 times, with RSD of the determined values of 2.5%. Test for recovery by the standard addition method was made on the actual sample, giving results of 98.0% and 101%, respectively.