超级微波消解-电感耦合等离子体发射光谱(ICP-OES)法测定有机硅消泡剂中的总硅  

Determination of Total Silicon Content in Silicone Defoamers by ICP-OES Coupled with Ultra-microwave Digestion

作　　者：张玲帆 阳芳 郭玉清 初秋亭 邵瑞琪 钟星语 高杰 孙海飞 席永清 ZHANG Lingfan;YANG Fang;GUO Yuqing;CHU Qiuting;SHAO Ruiqi;ZHONG Xingyu;GAO Jie;SUN Haifei;XI Yongqing(Research Centre of Analysis and Test,School of Chemistry and Molecular Engineering,East China University of Science and Technology,Shanghai 200237,China;China Laizhou inspection and Testing Center,Yantai,Shandong 261400,China;Bio-Link Pharmaceutical Equipment Technology(Jiangsu)Co.,Ltd.,Nantong,Jiangsu 226500,China)

机构地区：[1]华东理工大学化学与分子工程学院,分析测试中心,上海200237 [2]莱州市检验检测中心,山东烟台261400 [3]百林科制药装备科技(江苏)有限公司,江苏南通226500

出　　处：《中国无机分析化学》2025年第5期723-730,共8页Chinese Journal of Inorganic Analytical Chemistry

基　　金：国家自然科学青年基金资助项目(21407050)。

摘　　要：有机硅消泡剂产品广泛用于多个领域,其消泡效果取决于产品中硅的含量,因此准确测定消泡剂中硅的含量具有重要的意义。通过优化消解条件,包括酸的种类、消解温度;利用混酸体系(3 mL硝酸+1 mL盐酸+2 mL氢氟酸)成功将有机硅消泡剂中的硅元素消解转化为可溶性硅酸盐,进而采用ICP-OES对样品中的总硅含量进行了测定。结果表明,硅元素在浓度为0~50 mg/L拟合曲线线性良好,相关系数为0.9999,方法检出限和定量限分别为0.002%和0.007%,加标回收率在95.7%~103%,相对标准偏差小于2.0%,多类ICP-OES仪器测定Si的重现性小于5.0%。方法具有良好的精密度和准确度,能够有效地测定有机硅消泡剂中的总硅含量,对有机硅消泡剂的质量控制和相关研究具有重要的参考价值。Silicone defoamers are widely used in various fields,and their defoaming effectiveness depends on the silicon content in the product.Therefore,accurately measuring the silicon content in the defoamer is of great significance.By optimizing the digestion conditions,including the type of acid and digestion temperature,and using a mixed acid system(3 mL nitric acid+1 mL hydrochloric acid+2 mL hydrofluoric acid),the silicon element in the organic silicone defoamer was successfully digested and converted into soluble silicate.Subsequently,the total silicon content in the sample was determined using ICP-OES.The results showed that the silicon element followed a good linear relationship within the concentration range of 0-50 mg/L,with a correlation coefficient of 0.9999.The method's detection limit and quantification limit were 0.002%and 0.007%,respectively.The recoveries for spiked samples ranged from 95.7%to 103%,with a relative standard deviation(RSD)of less than 2.0%.The reproducibility of Si measurements across multiple ICP-OES instruments was less than 5.0%.This method exhibits good precision and accuracy,effectively determining the total silicon content in silicone defoamers.It holds significant reference value for the quality control and related research of silicone defoamers.

关 键 词：ICP-OES 有机硅消泡剂 超级微波消解 硅 

分 类 号：O657.31[理学—分析化学]