Hutchinson Joseph P, Johns Cameron, Breadmore Michael C, Hilder Emily F, Guijt Rosanne M, Lennard Chris, Dicinoski Greg, Haddad Paul R
Australian Centre for Research on Separation Science, School of Chemistry, Faculty of Science, Engineering and Technology, University of Tasmania, Hobart, Tasmania, Australia.
Electrophoresis. 2008 Nov;29(22):4593-602. doi: 10.1002/elps.200800226.
Novel CE methods have been developed on portable instrumentation adapted to accommodate a capacitively coupled contactless conductivity detector for the separation and sensitive detection of inorganic anions and cations in post-blast explosive residues from homemade inorganic explosive devices. The methods presented combine sensitivity and speed of analysis for the wide range of inorganic ions used in this study. Separate methods were employed for the separation of anions and cations. The anion separation method utilised a low conductivity 70 mM Tris/70 mM CHES aqueous electrolyte (pH 8.6) with a 90 cm capillary coated with hexadimethrine bromide to reverse the EOF. Fifteen anions could be baseline separated in 7 min with detection limits in the range 27-240 microg/L. A selection of ten anions deemed most important in this application could be separated in 45 s on a shorter capillary (30.6 cm) using the same electrolyte. The cation separation method was performed on a 73 cm length of fused-silica capillary using an electrolyte system composed of 10 mM histidine and 50 mM acetic acid, at pH 4.2. The addition of the complexants, 1 mM hydroxyisobutyric acid and 0.7 mM 18-crown-6 ether, enhanced selectivity and allowed the separation of eleven inorganic cations in under 7 min with detection limits in the range 31-240 microg/L. The developed methods were successfully field tested on post-blast residues obtained from the controlled detonation of homemade explosive devices. Results were verified using ion chromatographic analyses of the same samples.
新型毛细管电泳(CE)方法已在便携式仪器上得以开发,该仪器适配了电容耦合非接触式电导检测器,用于分离和灵敏检测自制无机爆炸装置爆炸后残留物中的无机阴离子和阳离子。所呈现的这些方法结合了本研究中所使用的多种无机离子的分析灵敏度和速度。阴离子和阳离子的分离采用了不同的方法。阴离子分离方法使用低电导率的70 mM三羟甲基氨基甲烷/70 mM 2-(环己氨基)乙磺酸水性电解质(pH 8.6),以及一根涂有溴化己二甲铵的90 cm毛细管来反转电渗流。15种阴离子能够在7分钟内实现基线分离,检测限在27 - 240 μg/L范围内。在相同电解质条件下,使用较短的毛细管(30.6 cm),45秒内可分离出在本应用中被认为最重要的10种阴离子。阳离子分离方法是在一根73 cm长的熔融石英毛细管上进行的,使用由10 mM组氨酸和50 mM乙酸组成的电解质体系,pH为4.2。添加络合剂1 mM羟基异丁酸和0.7 mM 18-冠-6醚可提高选择性,并能在7分钟内分离出11种无机阳离子,检测限在31 - 240 μg/L范围内。所开发的方法已成功地在自制爆炸装置控制爆破后获得的残留物上进行了现场测试。使用相同样品的离子色谱分析对结果进行了验证。