高温燃烧热导法中木质纤维素主元素分析条件优化  

Optimization of Principal Elements Analysis Conditions of Lignocellulose by Response Surface Methodology in Thermal Conductivity Method of High Temperature Combustion

作　　者：陈康道 汪红梅[1] 石炎军 徐开群 CHEN Kangdao;WANG Hongmei;SHI Yanjun;XU Kaiqun(College of Chemistry and Chemical Engineering,Changsha University of Science and Technology,Changsha,Hu’nan Province,410114;Changsha Kaiyuan Instruments Co.,Ltd.,Changsha,Hu’nan Province,410114)

机构地区：[1]长沙理工大学化学化工学院,湖南长沙410114 [2]长沙开元仪器股份有限公司,湖南长沙410100

出　　处：《中国造纸学报》2025年第1期40-48,共9页Transactions of China Pulp and Paper

基　　金：国家重大科学仪器研发项目(2018YFF01014000);湖南省学位与研究生教学改革研究项目(2021JGYB133);湖南省教育厅科学研究重点项目(23A0269)。

摘　　要：为准确测定木质纤维素的主元素含量,本研究基于高温燃烧热导法测定煤主元素的分析条件,采用二阶因子法筛选得到木质纤维素主元素含量测定的4个显著影响因素,其对木质纤维素主元素含量测定的影响由大到小依次为:供氧时间、供氧流量、样品质量、燃烧管温度;并通过单因素实验和响应面法优化测试参数,所得最佳实验条件为:样品质量30 mg、供氧时间90 s、供氧流量100 mL/min、燃烧管温度950℃。在最佳测试条件下,对6种木质纤维素标准物质进行主元素分析,并与煤测试条件和国家标准规定的方法对比。结果表明,优化后木质纤维素主元素分析条件的准确度与精确度均优于煤测试条件和国家标准规定的方法,主元素含量测定的标准偏差均<0.2,符合碳、氢、氮、硫4种主元素含量测定标准偏差≤0.3的目标要求,相对标准偏差(RSD,n=6)在0.04%~1.35%范围内。In order to accurately determine lignocellulosic main element content,in this study,based on the analytical conditions for the de⁃termination of coal main element by thermal conductivity method of high temperature combustion,four significant influencing factors of deter⁃mination of lignocellulosic main element content were selected by second-order factor method.The effects of significant influencing factors on the determination of lignocellulosic main element content were in descending order as follows:oxygen supply time,oxygen supply flow,sam⁃ple mass and combustion tube temperature.The test parameters were optimized by single factor experiment and response surface method.The optimum experimental conditions were as follows:sample mass was 30 mg,oxygen supply time was 90 s,oxygen supply flow was 100 mL/min,and combustion tube temperature was 950℃.The main element analysis of 6 lignocellulosic standard substances was carried out under the optimum test conditions,and compared with coal test conditions and national standard method.The results showed that the accuracy and precision of the optimized lignocellulose main element analysis conditions were superior to the coal test conditions and the national standard method.The standard deviation of the main element content determination<0.2,meeting target requirement for standard deviation≤0.3 in C,H,N,S content determination,and the relative standard deviation(RSD,n=6)was in the range of 0.04%~1.35%.

关 键 词：木质纤维素 主元素分析 高温燃烧热导法 响应面法 

分 类 号：TS7[轻工技术与工程—制浆造纸工程] TQ533.1[化学工程—煤化学工程]