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中国无机分析化学:2025,15(2):231-240
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基于RSM模型对王水-氯酸钾消解-ICP-OES法测定锑矿石中锑的条件优化
康 栋, 何 涛, 甘黎明, 冯博鑫, 门倩妮, 王 鹏
(中国地质调查局西安矿产资源调查中心)
Optimization of conditions for determining antimony in antimony ore by Wangshui-potassium chlorate digestion-ICP-OES method based on the RSM model
Kang Dong, He Tao, Gan Liming, Feng Boxin, Men Qianni, Wang Peng
(Xi’an Center of Mineral Resources Survey, China Geological Survey)
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投稿时间:2024-04-23    修订日期:2024-06-08
中文摘要: 锑是一种全球重要的战略矿产资源,快速准确测定锑矿中锑含量对锑矿的勘查和开采具有重要指导意义。本法采用响应曲面法(RSM)对电感耦合等离子体发射光谱法(ICP-OES)测定锑的试验条件进行优化。试验以氯酸钾加入量、溶解温度、提取液浓度为单因素,确定单因素变量为0.4~1.6 g,70~130 ℃,5~35%;根据RSM中的Box-Behnken(BBD)设计,选择锑矿石测定值为响应值,建立三因素三水平面试验,得到二次多项式回归模型,对该模型进行方差分析并判断其显著性,其中模型F值=421.94,P<0.0001,模型的R2=0.9982,R2adj=0.9958,C.V(变异值)=1.49%,S/N(信噪比)=59.54,可以解释超过98%的响应值变化。通过研究结果显示,在氯酸钾加入量为0.9 g、溶解温度为100℃、提取液盐酸浓度为15%的条件下,可以获得最佳的测定效果。4个锑矿石标准物质测定结果相对误差是0.34%~0.89%,相对标准偏差(RSD)是0.54%~1.12%,满足岩石矿物分析准确度和精密度控制要求,表明基于RSM模型优化锑矿石中锑量测定的试验方法准确可靠。该研究展示了RSM在复杂样品分析中的应用潜力,为分析化学方法优化提供了有效的试验工具。
Abstract:Antimony is a globally significant strategic mineral resource.Rapid and accurate determination of antimony content in antimony ores is crucial for their exploration and extraction. This study employs Response Surface Methodology (RSM) to optimize the experimental conditions for the determination of antimony using Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES).The study considers the amount of potassium chlorate,dissolution temperature,and extractant concentration as single factors,with ranges set at 0.4-1.6 g,70-130℃, and 5-35%,respectively.Based on the Box-Behnken Design (BBD) in RSM,a three-factor, three-level experimental design was established using the measured values of antimony ore as the response value.A quadratic polynomial regression model was obtained,and variance analysis was conducted to evaluate its significance.The model yielded an F-value of 421.94,P-value < 0.0001, R2 = 0.9982, R2adj = 0.9958,C.V. (coefficient of variation) = 1.49%,and S/N (signal-to-noise ratio) = 59.54,indicating that the model explains over 98% of the response value variation.The optimal determination conditions identified were 0.9 g of potassium chlorate,a dissolution temperature of 100℃,and a hydrochloric acid concentration of 15% in the extractant.The relative errors in the determination of four antimony ore standard materials ranged from 0.34% to 0.89%,with relative standard deviations (RSD) from 0.54% to 1.12%,meeting the accuracy and precision requirements for rock and mineral analysis.This indicates that the RSM-optimized method for determining antimony content in antimony ores is accurate and reliable.This study demonstrates the potential application of RSM in complex sample analysis and provides an effective experimental tool for optimizing analytical chemistry methods.
文章编号:     中图分类号:O657.31    文献标志码:
基金项目:战略性矿产勘查岩矿测试技术支撑(西安矿产中心)项目(DD20243334) 中国地质调查局自然资源综合调查指挥中心科技创新基金项目(KC20230012)金矿等战略性矿产实验测试技术支撑与服务(DD20242769)
康 栋  何 涛  甘黎明  冯博鑫  门倩妮  王 鹏
中国地质调查局西安矿产资源调查中心,中国地质调查局西安矿产资源调查中心,中国地质调查局西安矿产资源调查中心,中国地质调查局西安矿产资源调查中心,中国地质调查局西安矿产资源调查中心,中国地质调查局西安矿产资源调查中心
Kang Dong  He Tao  Gan Liming  Feng Boxin  Men Qianni  Wang Peng
Xi’an Center of Mineral Resources Survey, China Geological Survey,Xi’an Center of Mineral Resources Survey, China Geological Survey,Xi’an Center of Mineral Resources Survey, China Geological Survey,Xi’an Center of Mineral Resources Survey, China Geological Survey,Xi’an Center of Mineral Resources Survey, China Geological Survey,Xi’an Center of Mineral Resources Survey, China Geological Survey
引用文本:
康 栋,何 涛,甘黎明,冯博鑫,门倩妮,王 鹏.基于RSM模型对王水-氯酸钾消解-ICP-OES法测定锑矿石中锑的条件优化[J].中国无机分析化学,2025,15(2):231-240.
Kang Dong,He Tao,Gan Liming,Feng Boxin,Men Qianni,Wang Peng.Optimization of conditions for determining antimony in antimony ore by Wangshui-potassium chlorate digestion-ICP-OES method based on the RSM model[J].Chinese Journal of Inorganic Analytical Chemistry,2025,15(2):231-240.

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