Sample Preparation for Analysis of Chemicals Related to the Chemical Weapons Convention

Kuitunen, Marja‐Leena

doi:10.1002/9780470027318.a0410

Cited by 3 publications

(5 citation statements)

References 19 publications

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“…The standard approach adopted by the OPCW Mobile Laboratory is based on the work of technical experts from the member states, brought together by working groups before entry into force with the CWC. It includes laborious sample processing using solidliquid extraction (SLE) and liquid-liquid extraction (LLE) [5]. Fig.…”

Section: Introductionmentioning

confidence: 99%

Identification of chemicals relevant to the Chemical Weapons Convention using the novel sample-preparation methods and strategies of the Mobile Laboratory of the Organization for the Prohibition of Chemical Weapons

Terzic

Gregg

Voogt

2015

TrAC Trends in Analytical Chemistry

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Section: Introductionmentioning

confidence: 99%

Identification of chemicals relevant to the Chemical Weapons Convention using the novel sample-preparation methods and strategies of the Mobile Laboratory of the Organization for the Prohibition of Chemical Weapons

Terzic

Gregg

Voogt

2015

TrAC Trends in Analytical Chemistry

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“…Sample cleanup through an extraction process is the most reliable tool for chromatographic separations and analysis. However, only a few sample preparation methods are reported in the form of the recommended operating procedures (ROPs) for the analysis of CRCs in organic samples in the presence of high matrix background. ,− These include concentration, dilution, solvent exchange, liquid–liquid extraction (LLE) and solid phase extraction (SPE). Each type of sample clean up procedure has its own limitations.…”

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confidence: 99%

Polymeric Sorbent with Controlled Surface Polarity: An Alternate for Solid-Phase Extraction of Nerve Agents and Their Markers from Organic Matrix

et al. 2018

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Extraction and identification of lethal nerve agents and their markers in complex organic background have a prime importance from the forensic and verification viewpoint of the Chemical Weapons Convention (CWC). Liquid-liquid extraction with acetonitrile and commercially available solid phase silica cartridges are extensively used for this purpose. Silica cartridges exhibit limited applicability for relatively polar analytes, and acetonitrile extraction shows limited efficacy toward relatively nonpolar analytes. The present study describes the synthesis of polymeric sorbents with tunable surface polarity, their application as a solid-phase extraction (SPE) material against nerve agents and their polar as well as nonpolar markers from nonpolar organic matrices. In comparison with the acetonitrile extraction and commercial silica cartridges, the new sorbent showed better extraction efficiency toward analytes of varying polarity. The extraction parameters were optimized for the proposed method, which included ethyl acetate as an extraction solvent and n-hexane as a washing solvent. Under optimized conditions, method linearity ranged from 0.10 to 10 μg mL ( r = 0.9327-0.9988) for organophosphorus esters and 0.05-20 μg mL ( r = 0.9976-0.9991) for nerve agents. Limits of detection (S:N = 3:1) in the SIM mode were found in the range of 0.03-0.075 μg mL for organophosphorus esters and 0.015-0.025 μg mL for nerve agents. Limits of quantification (S:N = 10:1) were found in the range of 0.100-0.25 μg mL for organophosphorus esters and 0.05-0.100 μg mL for nerve agents in the SIM mode. The recoveries of the nerve agents and their markers ranged from 90.0 to 98.0% and 75.0 to 95.0% respectively. The repeatability and reproducibility (with relative standard deviations (RSDs) %) for organophosphorus esters were found in the range of 1.35-8.61% and 2.30-9.25% respectively. For nerve agents, the repeatability range from 1.00 to 7.75% and reproducibility were found in the range of 2.17-6.90%.

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“…Among various chromatographic and spectroscopic techniques that can be employed for the analysis of CRCs, gas chromatography coupled with mass spectrometry (GC-MS) is widely employed, because it provides both characteristic spectra and molecular weight information. − Recommended operating procedures (ROPs) have been developed for the gas chromatographic analysis of polar precursors/degradation products of toxic chemicals. , Prior to GC-MS analysis, these compounds are converted to their respective volatile derivatives. Unlike other schedule 3.B.…”

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confidence: 99%

Method for Derivatization and Detection of Chemical Weapons Convention Related Sulfur Chlorides via Electrophilic Addition with 3-Hexyne

et al. 2015

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Sulfur monochloride (S 2 Cl 2 ) and sulfur dichloride (SCl 2 ) are important precursors of the extremely toxic chemical warfare agent sulfur mustard and classified, respectively, into schedule 3.B.12 and 3.B.13 of the Chemical Weapons Convention (CWC). Hence, their detection and identification is of vital importance for verification of CWC. These chemicals are difficult to detect directly using chromatographic techniques as they decompose and do not elute. Until now, the use of gas chromatographic approaches to follow the derivatized sulfur chlorides is not reported in the literature. The electrophilic addition reaction of sulfur monochloride and sulfur dichloride toward 3-hexyne was explored for the development of a novel derivatization protocol, and the products were subjected to gas chromatography−mass spectrometric (GC-MS) analysis. Among various unsaturated reagents like alkenes and alkynes, symmetrical alkyne 3-hexyne was optimized to be the suitable derivatizing agent for these analytes. Acetonitrile was found to be the suitable solvent for the derivatization reaction. The sample preparation protocol for the identification of these analytes from hexane spiked with petrol matrix was also optimized. Liquid−liquid extraction followed by derivatization was employed for the identification of these analytes from petrol matrix. Under the established conditions, the detection and quantification limits are 2.6 μg/mL, 8.6 μg/mL for S 2 Cl 2 and 2.3 μg/mL, 7.7 μg/mL for SCl 2 , respectively, in selected ion monitoring (SIM) mode. The calibration curve had a linear relationship with y = 0.022x − 0.331 and r 2 = 0.992 for the working range of 10 to 500 μg/mL for S 2 Cl 2 and y = 0.007x − 0.064 and r 2 = 0.991 for the working range of 10 to 100 μg/mL for SCl 2 , respectively. The intraday RSDs were between 4.80 to 6.41%, 2.73 to 6.44% and interday RSDs were between 2.20 to 7.25% and 2.34 to 5.95% for S 2 Cl 2 and SCl 2 , respectively.

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Sample Preparation for Analysis of Chemicals Related to the Chemical Weapons Convention

Cited by 3 publications

References 19 publications

Identification of chemicals relevant to the Chemical Weapons Convention using the novel sample-preparation methods and strategies of the Mobile Laboratory of the Organization for the Prohibition of Chemical Weapons

Identification of chemicals relevant to the Chemical Weapons Convention using the novel sample-preparation methods and strategies of the Mobile Laboratory of the Organization for the Prohibition of Chemical Weapons

Polymeric Sorbent with Controlled Surface Polarity: An Alternate for Solid-Phase Extraction of Nerve Agents and Their Markers from Organic Matrix

Method for Derivatization and Detection of Chemical Weapons Convention Related Sulfur Chlorides via Electrophilic Addition with 3-Hexyne

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