酸溶-电感耦合等离子体发射光谱法测定土壤中的全硅  

Determination of total silicon in soil by acid dissolution and ICP-OES method

作　　者：杨晓燕 YANG Xiaoyan(Yunnan Zhinong Hi Tech Co.,Ltd.,Kunming 650600,China)

机构地区：[1]云南智农高新技术有限公司,云南昆明650600

出　　处：《生态产业科学与磷氟工程》2025年第1期120-123,共4页Eco-industry Science & Phosphorus Fluorine Engineering

基　　金：云南现代农业绿色关键技术创新与平台建设(202102AE090053);滇池流域农业绿色生产关键技术研究与体系构建(202102AE090030)。

摘　　要：建立电感耦合等离子体发射光谱法测定土壤中全硅的分析方法,采用盐酸-硝酸-氢氟酸在100~110℃电热板上消解试样,形成氟硅酸、氢氟酸和水的三元恒沸体系,选择有梯度的土壤标准物质配制标准溶液系列,加入内标元素,利用分析线与内标线强度比进行标准化,抵消了由于分析条件波动引起的谱线强度波动,直接用电感耦合等离子体原子发射光谱法(ICP-OES)测定土壤中的全硅。在仪器最佳工作条件下,硅元素校准曲线的线性相关系数为0.9999;方法检出限为3.3 mg/kg,测定结果的相对标准偏差(RSD,n=11)小于3.8%,加标回收率为98%~101%,测定结果与国家土壤标准物质认定值基本一致。该方法操作简单,耗时少,结果准确度高、精密性好,适合大批量土壤中全硅的检测。The analytical method of ICP-OES to determine the total silicon in soil is established,the sample is digested by hydrochloric acid-nitric acid-hydrofluoric acid in the range of 100-110℃to form a ternary azeotropic system of fluorosilicic acid,hydrofluoric acid and water.The gradient soil standard materials are selected to prepare the standard solution series,and the internal standard element is added,the intensity ratio of the analytical line and the internal standard line is used for standardization,to counteract the fluctuation of spectral line intensity caused by the fluctuation of analytical conditions,and ICP-OES method is used to determine the total silicon in soil.Under the best working conditions of the instrument,the linear correlation coefficient of the calibration curve of silicon element is 0.9999;The detection limit of the method is 3.3 mg/kg;The relative standard deviation(n=11)of the results is less than 3.8%,and the recovery rate is 98%-101%;The measured values of national soil standard materials are basically consistent with the certified value.This method is easy to operate,time-consuming,and has high accuracy and precision,making it suitable for the detection of total silicon in large quantities of soil.

关 键 词：盐酸-硝酸-氢氟酸 电感耦合等离子体原子发射光谱法(ICP-OES) 土壤 全硅 

分 类 号：O657.31[理学—分析化学] X833[理学—化学]