IC Determination of Inorganic Ions in Explosive Residues
摘 要
提出了离子色谱法测定爆炸残留物中无机离子的方法。DIONEX IonPac AS11-HC型阴离子交换柱及淋洗液20 mmol·L-1氢氧化钾溶液用于5种阴离子(Cl-、NO3-、NO2-、SO42-、ClO3-)的分离;DIONEX IonPac CS12A及淋洗液20 mmol·L-1甲磺酸溶液用于5种阳离子(Na+、K+、NH4+、Ca2+、Mg2+)的分离。测定中均采用抑制电导检测器。10种离子的线性范围均为0.1~100 mg·L-1,Cl-、NO3-、NO2-、SO42-和ClO3- 5种阴离子的检出限(3S/N)分别为2.36,3.87,5.49,6.11,6.02 μg·L-1,Na+、K+、NH4+、Ca2+和Mg2+ 5种阳离子的检出限(3S/N)分别为3.05,6.23,5.42,4.33,5.66 μg·L-1。方法用于爆炸残留物中无机离子的测定,阴、阳离子的回收率分别在91.2%~106.2%%和90.3%~102.3%范围内,相对标准偏差(n=6)分别在2.1%~3.8%和1.1%~4.2%范围之间。
Abstract
The contents of 5 anions and 5 cations in explosive residues were determined by ion chromatography (IC). DIONEX IonPac AS11-HC Anion-exchange column with 20 mmol KOH solution as eluant was used for separation of the 5 anions, i.e., Cl-, NO3-, NO2-, SO42- and ClO3-, and DIONEX IonPac CS12A cation-exchange column with 20 mmol·L-1 methyl sulfonic acid as eluant was used for separation of the 5 cations, i.e., Na+, K+, NH4+, Ca2+ and Mg2+. Inhibitory conductivity detections were adopted in the determinations. Linearity was found in the same range of 0.1-100 mg·L-1 for all the 10 inorganic ions, with values of detection limit (3S/N) of 2.36 μg·L-1 for Cl-, 3.87 μg·L-1 for NO3-, 5.49 μg·L-1 for NO2-, 6.11 μg·L-1 for SO42- and 6.02 μg·L-1 for ClO3-, 3.05 μg·L-1 for Na+, 6.23 μg·L-1 for K+, 5.42 μg·L-1 for NH4+, 4.33 μg·L-1 for Ca2+ and 5.66 μg·L-1 for Mg2+. The proposed method was applied to the determination of 10 inorganic ions in explosive residues, giving values of recovery in the ranges of 91.2%-106.2% and 90.3%-102.3%, and RSD (n=6) in the ranges of 2.1%-3.8% and 1.1%-4.2% for the anions and cations respectively.
中图分类号 O657.7
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收稿日期 2010/8/11
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备注陈祥国(1976-),男,河南台前人,硕士研究生,工程师,主要从事理化检验工作。
引用该论文: CHEN Xiang-guo,Lv Ji-zhong,ZHANG Yin-hua. IC Determination of Inorganic Ions in Explosive Residues[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2011, 47(10): 1200~1202
陈祥国,吕纪忠,张银华. 离子色谱法测定爆炸残留物中无机离子[J]. 理化检验-化学分册, 2011, 47(10): 1200~1202
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参考文献
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【6】裴茂清,郭海荣.离子色谱在无机炸药分析中的应用[J].刑事技术, 2005,6:13-14.
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【2】HAMISH S. Modern inorganic chromatography[J]. Anal Chem, 1983,55:235A.
【3】SOGA T, ROSS G A. Simultaneous determination of inorganic anions, organic acids, amino acids and carbohydrates by capillary electrophoresis[J]. J Chromatogr A, 1999,837:9-231.
【4】SWARTZ M E. Capillary electrophoretic determination of inorganic ions in a prenatal vitamin formulation[J]. J Chromatography, 1993,640:441-444.
【5】DOUGLAS J K B S, DELONN N M F S. The use of capillary electrophoresis in the detection of monomethylamine and benzoate ions in the forensic examination of explosives residues[J]. J Forensic Sci,2001,46(5):1168-1173.
【6】裴茂清,郭海荣.离子色谱在无机炸药分析中的应用[J].刑事技术, 2005,6:13-14.
【7】朱岩.离子色谱仪器[M].北京:化学工业出版社, 2007.
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