电导检测器离子色谱法测氰根的应用 -学兔兔 www.xuetutu.com.pdf

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第32卷第4期
仪器仪表学报
Vol 32 No. 4
2011年4月
Hese outn
nal of Scientific Instrument
Apr.2011
电导检测器离子色谱法测氰根的应用
刘霞,袁帅,李军,陈雪莉,王辅臣
(华东理工大学煤气化教育部重点实验室上海200237)
摘要:利用电导检测器离子色谱建立了氰根的分析方法,考察了该分析方法的检测下限、线性范围、标准误差(RSD)以及加
标回收率。在高频热解设备中对神府煤和稻草进行了快速热解实验,利用NaOH溶液吸收法将热解气中的HCN转化为氰根离
子,利用所建立的检测方法对氰根进行定量。结果表明,信噪比为3时该分析方法的检测下限为0.01mg/L,在0.1~50mg/L
范围内线性关系良好,标准误差(RSD)小于3%,加标回收率为90%~105%。对HCN吸收液样品进行检测时发现氧根与其他
杂质离子分离效果较好,3次重复实验的重现性良好。所建立的HCN吸收方法和氰根检测方法能够满足煤和生物质热解时
HCN生成率的考察要求。
关键词:离子色谱;电导检测器;氰根;煤;生物质
中图分类号:0657.7文献标识码:A国家标准学科分类代码:150.2540
Determination of cyanide using conductivity detector ion chromatography
Liu Xia, Yuan Shuai, Li Jun, Chen Xueli, Wang Fuchen
( Key Laboratory of Coal Gasification of Ministry of Education, East China University of
Science and Technology, Shanghai 200237, China
Abstract: A CN "ion analysis method was established using conductivity detector ion chromatography, and the d
tection limit, standard error and recovery rate of standard additions were investigated. Rapid pyrolysis of Shenfu coal
and rice straw was carried out in a high frequency furnace, and the HCN in pyrolysis gas was absorbed and converted
o CN ions using NAOH solution, then the CN ions were analyzed by the established method. Research results
show that the detection limit is 0. O1 mg /L when signal-to-noise ratio is 3, there is a good linear relationship in the
range from 0. I to 50 mg/L, the standard errors are lower than 3%, the recovery rate of standard additions is
90%-105%. Experiment also shows that CN ions can be effectively separated from other impurity ions, and fine
repeatability can be obtained. The proposed HCN adsorption method and CN analysis method can meet the investi
gation requirements of HCN formation rate during coal and biomass pyrolysis
Key words: ion chromatography; conductivity detector; cyanide; coal; biomass
另外,随着大规模煤气化技术的发展,由煤中
1引言
的氮在还原性气氛下转化而生成的氧化物污染物也得到
了一些研究者的关注。随着环保标准的提高,含氧废
氰基以其优良的络合能力而广泛应用于炼焦、选矿、水的排放标准也日渐严格,我国在污水排放标准(GB
有色金属冶炼和加工、电镀、制革、电子及仪器仪表等工8978-2000)中对氰化物的最高排放浓度进行了规定
业?,因此以上各行业也是日前含氰废水的主要来源,其
二级排放标准最高为0.5mg/L,三级排放标准最高
中电镀厂废水的氯化物浓度约为几十至几万mg/L,而我为1.0mg/L。因此,含氰废水的监测和控制是目前环境
国仅黄金生产每年所排放的含氰废水就高达1.2×工作者的重要方向之一。
收稿日期:2010-08 Received Date:2010-08
基金项目:国家重点基础研究发展计划(973计划)(2010CB227000)资助项目