Decontamination solutions are used for an efficient detoxification of chemical warfare agents (CWAs). As these solutions can be composed of strong alkaline chemicals with hydrolyzing and oxidizing properties, the analysis of CWA degradation products in trace levels from these solutions imposes a challenge for any analytical technique. Here, we present results of application of nuclear magnetic resonance spectroscopy for analysis of trace amounts of CWA degradation products in several untreated decontamination solutions. Degradation products of the nerve agents sarin, soman, and VX were selectively monitored with substantially reduced interference of background signals by 1D 1H-31P heteronuclear single quantum coherence (HSQC) spectrometry. The detection limit of the chemicals was at the low part-per-million level (2-10 microg/mL) in all studied solutions. In addition, the concentration of the degradation products was obtained with sufficient confidence with external standards.
Abstract. Nerve agents and two other chemical warfare agents were extracted from spiked soil with supercritical CO,. Supercritical fluid extraction (SFE) was used as an off-line technique. The extracts were analyzed with a two-channel capillary gas chromatograph, equipped with an autosampler and flame ionization and nitrogenphosphorus detectors. Compounds were identified and quantified automatically with the help of retention index monitoring (RIM). Recoveries were equal to or better than those obtained with solvent extraction by sonication.
This article discusses the preparation of environmental samples to be analyzed for chemicals related to the Chemical Weapons Convention (CWC), where analysis takes place off‐site by gas chromatography (GC) or liquid chromatography (LC) as an introduction technique to spectrometers, or by capillary electrophoresis (CE). The specific sample preparation methods required for analysis by spectroscopic techniques such as nuclear magnetic resonance (NMR) spectroscopy are dealt with in separate articles. Preparations of air, aqueous liquid (water), soil, active charcoal, wipe, and concrete samples, and samples of paint, rubber, and other polymeric materials for off‐site analysis are presented in Section 2 and are as described in the corresponding recommended operating procedures (ROPs). In addition, preparations of organic liquid samples are presented, as described in the in‐house operating procedures of the Finnish Institute for CWC analysis. Section 3 examines the question of quality control (QC) in sample preparation and Section 4 discusses the important matter of safety in handling samples that may contain CWC‐related chemicals. Section 5 reports on the use of the methods in international comparison and proficiency tests.
This article discusses the preparation of environmental samples to be analyzed for chemicals related to the chemical weapons convention (CWC), where analysis takes place on‐site or off‐site by gas chromatography (GC) or liquid chromatography (LC) as an introduction technique to spectrometers or by capillary zone electrophoresis (CZE). The specific sample preparation methods required for analysis by spectroscopic techniques such as Fourier transform infrared (FTIR) and nuclear magnetic resonance (NMR) spectroscopy are dealt with in separate articles. Preparations of analytical samples from air, aqueous liquid (water), soil, active charcoal, wipe, concrete, paint, rubber, and other polymeric samples for off‐site analysis are presented in section 2, and preparations of analytical samples from aqueous liquid (water), soil, and wipe samples for on‐site analysis, are covered in section 3. Preparations for on‐site analysis are as described in the standard operating procedures (SOPs) of the international organization responsible for verifying the Convention (Technical Secretariat of the Organization for the Prohibition of Chemical Weapons) and those for off‐site analysis are as described in the corresponding recommended operating procedures (ROPs). Section 4 examines the question of quality control (QC) in sample preparation and section 5 the important matter of safety in handling samples containing CWC‐related chemicals. Section 6 reports on the use of the methods in international comparison and proficiency tests.
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