IC Determination of Sulfur and Chlorine in Solid Biomass Fuel with Tube Furnace Combustion
摘 要
取粉碎的固体生物质燃料样品于管式炉的瓷舟中,燃烧后气体被吸收液吸收。吸收液用水定容至5.0 mL,过0.45 μm滤膜,采用离子色谱法测定滤液中硫和氯的含量。采用Dionex IonPac AS18阴离子色谱柱进行色谱分离,以12 mmol·L-1氢氧化钾溶液为流动相,电导检测器测定。硫酸根、氯离子的质量浓度均在0.1~10.0 mg·L-1内与其对应的峰面积呈线性关系,检出限(3S/N)依次为0.005,0.003 mg·L-1。对5.0 mg·L-1硫酸根、氯离子的混合标准溶液平行测定6次,硫酸根和氯离子峰面积的相对标准偏差(n=6)依次为2.1%,2.2%。以空白固体生物质燃料样品为基体进行加标回收试验,所得回收率为96.0%~98.2%。方法应用于固体生物质燃料样品的分析,测定值与艾士卡法和高温水解-电位滴定法测定结果基本一致。
Abstract
The crushed sample of solid biomass fuel was taken in the porcelain boat of tube furnace. After combustion, the gas was absorbed by the absorbing liquid. The absorption solution was diluted to 5.0 mL with water, and then filtered on 0.45 μm filtering membrane. IC was applied to the determination of sulfur and chlorine in the filtrate. Dionex IonPac AS18 anionic chromatographic column was used for chromatographic separation. 12 mmol·L-1 potassium hydroxide solution was used as mobile phase, and conductance detector was used in determination. Linear relationships between values of peak area and mass concentration of sulfate and chloride were kept in the range of 0.1-10.0 mg·L-1, with detection limit (3S/N) of 0.005, 0.003 mg·L-1, respectively. Precision of the method was tested at the mass concentration level of 5.0 mg·L-1 mixed standard solution of sulfate and chloride for 6 parallel determinations, and values of RSDs (n=6) of peak area of sulfate and chloride were 2.1%, 2.2%, respectively. On the base of blank sample of solid biomass fuel, test for recovery was made by standard addition method; values of recovery found were in the range of 96.0%-98.2%. The proposed method was applied to the analysis of samples of solid biomass fuel, giving results in consistency with values given by Eschkal method and potentiometric titration with high temperature hydrolysis.
中图分类号 O657.7 DOI 10.11973/lhjy-hx202007002
所属栏目 工作简报
基金项目 辽宁省自然科学基金指导计划(20170520108)
收稿日期 2020/3/9
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备注王诗语,助理研究员,硕士,主要从事油品分析工作,wangshiyu.fshy@sinopec.com
引用该论文: WANG Shiyu,LING Fengxiang,HAN Bo,GAO Bo. IC Determination of Sulfur and Chlorine in Solid Biomass Fuel with Tube Furnace Combustion[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2020, 56(7): 755~759
王诗语,凌凤香,韩博,高波. 管式炉燃烧-离子色谱法测定固体生物质燃料中硫和氯[J]. 理化检验-化学分册, 2020, 56(7): 755~759
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