微波消解-ICP-AES用于硅溶胶中杂质元素测定
详细信息 查看官网全文
- 英文论文题名：Determination of Impurity Element Contents in Silica Sol by Microwave Digestion-ICP-AES
- 论文作者：王月娜 ; 韩建新 ; 高玲 ; 铉烨
- 英文论文作者：WANG Yue-na ; HAN Jian-xin ; GAO Ling ; XUAN Ye ; SINOPEC CATALYST Fushun Division ; China Huanqiu Constructing&Engineering Corp.Liaoning Subcompany
- 年：2016
- 作者机构：中国石化催化剂有限公司抚顺分公司;中国寰球工程公司辽宁分公司;
- 论文关键词：ICP-AES ; 硅溶胶 ; 微波消解 ; 正交设计
- 英文论文关键词：ICP-AES ; Silica sol ; Microwave digestion ; Orthogonal design
- 会议召开时间：2016-11-14
- 会议录名称：2016年全国无机硅化物行业年会暨创新发展研讨会论文集
- 语种：中文
- 分类号：O648.16;O657.31
- 学会代码：WJYG
- 会议名称：2016年全国无机硅化物行业年会暨创新发展研讨会
- 会议地点：中国河南郑州
- 主办单位：中国无机盐工业协会无机硅化物分会
- 学会名称：中国无机盐工业协会无机硅化物分会
- 页数：3
- 文件大小：243k
- 原文格式：O
- 会议级别：全国
摘要
采用微波消解方法处理硅溶胶样品,通过设计正交实验研究消解温度、保留时间和消解溶剂对消解效果的影响,优化了微波消解硅溶胶样品的消解参数。并采用电感耦合等离子体原子发射光谱(ICP—AES)法测定硅溶胶中Fe、Na、K杂质元素的含量。结果表明,优化的硅溶胶消解参数为:消解温度为160℃,保留时间为4 min,盐酸及氢氟酸用量分别为2.0和1.0 mL。该方法Fe、Na、K元素的检出限依次为:0.002、0.002和0.003μg/mL,Fe、Na、K的加标回收率均在97%~103%之间,相对标准偏差(RSD)均小于2%,具有较好的准确度和精密度。方法快速简便、准确可靠,完全能够满足分析要求。
Silica sol samples were treated by microwave digestion method.Influences of digestion temperature,retention time and solvent on the digestion effect were investigated by designing orthogonal test,and the digestion parameters of the microwave digestion were optimized.And then the contents of three impurity elements,including Fe,Na and K in silica sol were determined by atomic emission inductively coupled plasma spectrometry(ICP-AES).The results show that the optimum digestion parameters are as follows:the digestion temperature160℃,the retention time 4 min and the dosages of the digestion solvent 2 mL HCl and 1 mL HF.The element detection limits of Fe,Na and K are 0.002,0.002 and 0.003μg/mL respectively,and the recovery rates of ICPAES method are between 97%~103%,the relative standard deviations(RSD) are lower than 2%.These figures show that the microwave digestion-ICP-AES method has good accuracy and precision.This method is accurate,simple and reliable,which can meet the analysis requirement completely.
Silica sol samples were treated by microwave digestion method.Influences of digestion temperature,retention time and solvent on the digestion effect were investigated by designing orthogonal test,and the digestion parameters of the microwave digestion were optimized.And then the contents of three impurity elements,including Fe,Na and K in silica sol were determined by atomic emission inductively coupled plasma spectrometry(ICP-AES).The results show that the optimum digestion parameters are as follows:the digestion temperature160℃,the retention time 4 min and the dosages of the digestion solvent 2 mL HCl and 1 mL HF.The element detection limits of Fe,Na and K are 0.002,0.002 and 0.003μg/mL respectively,and the recovery rates of ICPAES method are between 97%~103%,the relative standard deviations(RSD) are lower than 2%.These figures show that the microwave digestion-ICP-AES method has good accuracy and precision.This method is accurate,simple and reliable,which can meet the analysis requirement completely.
引文