A multicomponent mobile phase for ion chromatography applied to the separation of anions from the residue of low explosives

被引:54
作者
Doyle, JM [1 ]
Miller, ML [1 ]
McCord, BR [1 ]
McCollam, DA [1 ]
Mushrush, GW [1 ]
机构
[1] FBI Lab, Ctr Forens Sci Res & Training, Quantico, VA 22135 USA
关键词
D O I
10.1021/ac991346z
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
A multicomponent mobile phase utilizing ion-exchange, ion-exclusion, and ion-pairing principles for the rapid isocratic separation of anions in low explosives residue by ion chromatography (IC) has been developed. The notable feature of this system is that an ion-pairing reagent and an ion-exclusion reagent are combined in the same mobile phase. Contrary to expectation, these reagents act independently of each other in solution. The stock mobile-phase composition consisted of boric acid, D-gluconic acid, Lithium hydroxide, and glycerol. Tetrapropylammonium hydroxide, an ion-interaction reagent was used to achieve pH 8.5. Acetonitrile (ACN) was added to enhance resolution and octanesulfonic acid, an ion-exclusion reagent, was added to adjust the retention time of perchlorate, Separation of a mixture of anions common to low explosives residue was achieved in less than 16 min using a Waters IC-Pak Anion HR column, Optimization studies were performed by changing the concentration of the ACN and by altering the pH or the type of ion-interaction or -exclusion agents. Simulated case studies were performed using postblast residues from pipe bombs. The results show this method to be a valid and reproducible procedure for forensic casework analysis. The practical significance of this system is that a reduction in the analysis time and an improvement in efficiency of late-eluting peaks can be achieved without resorting to gradient elution techniques. For the analysis of anions detected in explosives residue, the Waters IC-Pak Anion HR column has proven to be a suitable replacement for the Vydac 300IC405 column, which has been discontinued by the manufacturer.
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页码:2302 / 2307
页数:6
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