Novel Optimization of HMTD Traces Detection by HS-SPME-GC/MS and HS-SPME-GC/μECD

H. Stambouli, A. E. Bouri, A. Dahrouch, Abdelfattah Boukhaled, T. Bouayoun
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引用次数: 1

Abstract

HMTD is known for its decomposition at low temperatures. The use of common techniques such as GC/MS and GC/μECD for its detection in liquid solutions or solid traces requires the control of analytical conditions. The present work proposes two sensitive methods using GC/MS and GC/μECD where the injector temperature is set at 150°C to analyse successfully the concentrations of 0.1 ng (10-4 mg/mL) and 0.05 ng (0.5-10.4 mg/mL) of HMTD in acetone solutions. The analysis of solid traces of HMTD was performed with the same methods by adopting the headspace mode using the SPME fibre. The exposure the fibre in the headspace during 10 min at ambient temperature (22°C) and the desorption in the injector at 150°C, allow the detection of HMTD without degradation. In addition, to simulate crater sample, 3 mg of HMTD are mixed to 150 g of soil (0.002%). In this case, HMTD was also successfully detected by HS-SPME-GC/MS and HS-SPMEGC/μECD after 1 h exposure of the fibre at 22°C. These results demonstrate the performance of these optimized methods for trace analysis of HMTD.
HS-SPME-GC/MS和HS-SPME-GC/μECD检测HMTD痕量的新优化
HMTD以其在低温下的分解而闻名。使用GC/MS和GC/μECD等常用技术检测其在液体溶液或固体痕量中需要控制分析条件。在150℃的进样温度下,采用GC/MS和GC/μECD两种灵敏的方法,成功地分析了丙酮溶液中浓度为0.1 ng (10-4 mg/mL)和0.05 ng (0.5-10.4 mg/mL)的HMTD。采用同样的方法,采用SPME纤维顶空模式对HMTD固体痕量进行了分析。在环境温度(22°C)下将纤维暴露于顶空10分钟,并在150°C下在注射器中解吸,可以在不降解的情况下检测HMTD。此外,为了模拟陨石坑样本,将3 mg HMTD混合到150 g土壤中(0.002%)。在这种情况下,在22°C下暴露1 h后,通过HS-SPME-GC/MS和HS-SPMEGC/μECD也成功检测到HMTD。结果表明,优化后的方法可用于HMTD的痕量分析。
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