聚环氧乙烷凝聚重量法结合ICP–AES法测定玻璃中的二氧化硅

建立聚环氧乙烷凝聚重量法结合电感耦合等离子体发射光谱法(ICP–AES)法测定玻璃中二氧化硅的分析方法。玻璃试样经1 000℃高温下无水碳酸钠熔融,以盐酸浸出后蒸成湿盐状,再用聚环氧乙烷凝聚,过滤并将沉淀灼烧,然后用氢氟酸处理,其前后的质量差即为沉淀的二氧化硅量,滤液中的二氧化硅用ICP–AES法测定,两者相加得试样中二氧化硅的总含量。在选定的条件下,用ICP–AES法测定二氧化硅的线性范围为0.20~50μg/m L,线性相关系数为0.999 5,检出限为0.20μg/m L。测定结果的相对标准偏差为0.45%(n=6),方法的回收率在98.6%~101.9%之间。该方法具有较高的准确度和良好的精密度,测定速度快,可用于玻璃中二氧化硅含量的测定。

Determination of Silicon Dioxide in Glass by Poly Ethylene Oxide Condensation Weight Method Combined with ICP-AES

The method for determination of silicon dioxide in glass by poly ethylene oxide condensation weight method combined with inductively coupled plasma atomic emission spectrometry(ICP-AES) was established.The sample was fused by Na2CO3 at 1 000 ℃ and lixiviated by HC1,then was evaporated to wet salt which was condensed by poly ethylene oxide.The obtained sample was filtered,and then the precipitate was burned to constant weight and followed by reacting with hydrofluoric acid.The difference of the two mass results were the amount of silicon dioxide in the sample.While the silicon dioxide left in the filtrate was determined by ICP-AES.The total amount of silicon dioxide in the sample was obtained by adding the two results.Under the selected conditions,the linear range was 0.20-50 μ g/mL,the linear correlation coefficient was 0.999 5,and the detection limit was 0.20 μ g/mL.The relative standard deviation of determination results was 0.45％(n=6),and the recovery was 98.6％-101.9％.The method has high accuracy and good precision,it is suitable for the determination of silicon dioxide in glass with rapid measuring speed.