微波消解/ICP-AES法测定拟薄水铝石中的微量Na和S元素

石油炼制与化工 ›› 2022, Vol. 53 ›› Issue (7): 86-91.

微波消解/ICP-AES法测定拟薄水铝石中的微量Na和S元素

赖婷婷,戴新,刘雅琼,王轲,吴梅,曾双亲

中国石化石油化工科学研究院

收稿日期:2021-12-10 修回日期:2022-03-22 出版日期:2022-07-12 发布日期:2022-06-29
通讯作者: 赖婷婷 E-mail:laitingting.ripp@sinopec.com

DETERMINATION OF TRACE SULFUR AND SODIUM IN PSEUDO-BOEHMITE BY ICP-AES BASED ON MICROWAVE DIGESTION

Received:2021-12-10 Revised:2022-03-22 Online:2022-07-12 Published:2022-06-29

摘要/Abstract

摘要： 建立了同时测定工业拟薄水铝石中Na含量和S含量的微波消解-电感耦合等离子体发射光谱法（ICP-AES）分析方法，考察了微波消解条件、元素间干扰对测定结果的影响，建立了测定Na、S含量的标准曲线。优化的微波消解条件为：样品0.1 g，消解液（盐酸）10 mL，消解温度185 ℃，消解时间50 min。所建ICP-AES方法测定溶液的Na质量分数为0.07~15.00 μg/g，测定结果拟合线性相关系数为1.000 00，相对标准偏差为1.1%，加标回收率为100.0%~101.0%；测定溶液的S质量分数为0.10~35.00 μg/g，测定结果拟合线性相关系数为0.999 99，相对标准偏差为1.1%，加标回收率为95.0%~100.0%。该方法适用于Na质量分数为35~7 500 μg/g、S质量分数为50~17 500 μg/g的工业拟薄水铝石的Na、S含量测定。

关键词: 微波消解, ICP-AES, 拟薄水铝石, 杂质

Abstract: A novel method was developed to determine trace sulfur and sodium in pseudo-boehmite commercial products by ICP-AES based on microwave digestion. Then the conditions of microwave digestion and interelement interference were investigated to optimize the microwave digestion procedure and accuracy of analysis. Finally, the standard curve for analyzing the content of sodium and sulfur was established. In the method, 0.1 g pseudo-boehmite was completely digested with 10 mL hydrochloric at the temperature of 185 ℃ in 50 min. The linear range of the standard curve for analyzing the content of sodium in solution by ICP-AES was 0.07-15.00 μg/g with a linear correlation coefficient of 1.000 00; relative standard deviation was 1.1%, and the recovery of the method was between 100.0% and 101.0%. The linear range of the standard curve for analyzing the content of sulfur in solution by ICP-AES was 0.10-35.00 μg/g with a linear correlation coefficient of 0.999 99; relative standard deviation was 1.1%, and the recovery of the method was between 95.0% and 100.0%. The method is suitable for the analysis of contents of sulfur and sodium in pseudo-boehmite commercial products with sodium of 35-7 500 μg/g and sulfur of 50-17 500 μg/g.

Key words: microwave digestion, ICP-AES, pseudo-boehmite, impurity

赖婷婷戴新刘雅琼王轲吴梅曾双亲. 微波消解/ICP-AES法测定拟薄水铝石中的微量Na和S元素[J]. 石油炼制与化工, 2022, 53(7): 86-91.

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