基于响应面中心复合设计法优化ICP-OES测定钴基费托合成催化剂中Co含量的前处理方法  

Optimization of ICP-OES Pretreatment Method for Determination ofCo Content in Co-based Catalysts for Fischer-Tropsch SynthesisBased on Response Surface Center Composite Design

作　　者：蒋智慧 赵帅 刘聪云 马琳鸽 龙银花 李永龙 JIANG Zhihui;ZHAO Shuai;LIU Congyun;MA Lin′ge;LONG Yinhua;LI Yonglong(National Institute of Clean and Low Carbon Energy,Beijing 100029,China)

机构地区：[1]北京低碳清洁能源研究所,北京100029

出　　处：《中国无机分析化学》2023年第5期490-498,共9页Chinese Journal of Inorganic Analytical Chemistry

摘　　要：为提高电感耦合等离子体发射光谱仪(ICP-OES)测定钴基费托合成催化剂中Co含量的准确度,采用单因素结合响应面中心复合设计法(RSM-CCD),优化了ICP-OES测定钴基费托合成催化剂中Co含量的前处理工艺。响应面法以Co含量测定值与真实值之间的相对误差δ和前处理时间作为指标,考察了影响前处理的三个主要参数,即酸比例(VHCl∶V((HCl+HNO3)))、酸用量和消解温度,采用统计分析和方差分析确定了最优的反应条件。结果表明,在消解温度180℃,酸用量10.6 mL,酸比例0.44的条件下,理论值δ可低至0.001%,置信区间为[0,0.297],消解时间缩短为0.57 h,置信区间为[0,1.21]。通过三次验证实验,δ和消解时间均落在置信区间内。利用RSM得到的分析结果合理可行,通过优化实验因素,可实现催化剂中Co含量简单快速准确率高且重复性好的测定,同时也为其他金属元素的检测提供了参考。To improve the accuracy of the determination of Co content in cobalt-based Fischer-Tropsch synthesis catalyst by inductively coupled plasma emission spectrometer(ICP-OES),the response surface method center composite design(RSM-CCD)combined with single factor was used to optimize the pretreatment process for the determination of Co content in Co-based catalysts for Fischer-Tropsch synthesis by the inductively coupled plasma optical emission spectrometer(ICP-OES).Three main parameters,i.e the acid ratio(V HCl∶V(HCl+HNO 3)),acid dosage,and temperature were considered in RSM.The relative errorδbetween the measured value of Co content and the true value and pretreatment time were selected as response of design.The optimum conditions were determined using statistical analysis and analysis of variance(ANOVA).The results showed that the theoreticalδwas 0.001%,with the confidence interval at[0,0.297]and digestion time was 0.57 h,confidence interval was[0,1.21]under the optimum condition.The amount of acid was obtained to be 10.6 mL in optimum condition and the best ratio and temperature were 0.44 and 180℃.Bothδand time fall within the confidence interval of the theoretical value through verification tests.The analysis results obtained by RSM were reasonable and feasible.In general,a simple,fast,high-accuracy and repeatable determination can be achieved by optimizing the experimental factors.

关 键 词：ICP-OES 响应面 中心复合设计 湿法消解 固体催化剂 钴 

分 类 号：O657.31[理学—分析化学] TH744.11[理学—化学]