IC Determination of Fluorine in Solid Biomass Fuel
摘 要
选取7种不同的植物类样品,按GB/T 28730-2012所述方法制备分析样品。经试验提出其最佳样品前处理及色谱分析条件:取样品0.500 0 g,于镍坩埚中用(1.0±0.1) g氢氧化钾,先后在250℃和550℃熔融30 min和30 min。取出坩埚,冷却至室温。用水10 mL浸取熔块,溶液定容至100 mL。用Metrosep A16-150色谱柱作为分离柱,淋洗液为7.5 mmol·L-1碳酸钠-0.75 mmol·L-1氢氧化钠溶液,用抑制型电导检测器测定。氟的线性范围在0.02~1.0 mg·L-1内,检出限为7.6 μg·L-1。在实样的基础上用标准加入法进行回收试验,测得回收率在96.2%~103%之间,测定值的相对标准偏差(n=6)均小于5.0%。
Abstract
Seven kinds of botanic substances were sampled as described in GB/T 28730-2012 and the optimized conditions for sample-pretreatment and IC analysis were found as follows:the sample (0.500 0 g) was fused with (1.0±0.1) g KOH in a nickel crucible at 250℃ and 550℃ for 30 min and 30 min in succession. The melt in the cooled crucible was taken up with 10 mL of water and then made up to 100 mL. Metrosep A16-150 column was used for IC-separation with mixed solution of 7.5 mmol·L-1 Na2CO3 and 0.75 mmol·L-1 NaOH as mobil phase. Restrain conductance detector was used in the determinations. Linearity range for fluorine was found between 0.02 and 1.0 mg·L-1, with detection limit of 7.6 μg·L-1. On the base of substantial samples, test for recovery was made by standard addition method, giving values of recovery in the range of 96.2% to 103% and values of RSD's (n=6) found were all less than 5.0%.
中图分类号 O657.7 DOI 10.11973/lhjy-hx201705021
所属栏目 专题报道
基金项目 国家能源局标准资助项目(20140707);南方电网有限责任公司科技项目(K-GD2013-057)
收稿日期 2016/5/21
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备注张宏亮(1971-),男,河北保定人,高级工程师,硕士,主要从事电力燃料、生物质新能源监督检验与研究工作,gzmeihualu@163.com
引用该论文: ZHANG Hongliang,ZHANG Jifan,LIANG Hanxian,LI Yuchun,LI Wei. IC Determination of Fluorine in Solid Biomass Fuel[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2017, 53(5): 581~584
张宏亮,张吉范,梁汉贤,李宇春,李薇. 离子色谱法测定固体生物质燃料中氟的含量[J]. 理化检验-化学分册, 2017, 53(5): 581~584
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【3】怀颖,孙德忠,吕庆斌.燃烧水解-离子选择性电极法测定植物样品中氟含量的方法改进[J].岩矿测试, 2010,29(1):39-42.
【4】李清彩,赵庆令,张洪民,等.离子选择性电极电位法测定钼矿石和钨矿石中氟[J].理化检验-化学分册, 2011,47(8):932-934.
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【8】冯铁.顶空气相色谱法测定空气中氟化物方法的研究[J].中国卫生检验杂志, 2011,21(3):578-580.
【9】IRGOLICK J, FRENIUS Z. Determination of fluorine in plant by ion chromatography[J]. Anal Chem, 1984,319:556-559.
【10】徐霞,应兴华,段彬伍.植物样品中痕量氟的离子色谱法分析[J].分析测试学报, 2008,27(1):57-59.
【11】胡德新,马德起,安鹏声,等.超声提取-离子色谱法测定铁矿石中水溶性氟氯溴及硝酸根[J].岩矿测试, 2012,31(2):287-290.
【12】HJ 168-2010环境监测、分析方法标准制修订技术导则[S].
【13】周方求,黄学仲,张攀.碱熔-离子色谱法测定茶叶中氟[J].实用预防医学, 2009,16(2):581-582.
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