Malaysian Journal of Analytical Sciences Vol 19 No 3 (2015): 603 – 610

 

 

 

COMPARISON OF THREE SAMPLE PREPARATION METHODS FOR ANALYIS OF CHEMICAL WARFARE AGENT

SIMULANTS IN WATER

 

(Perbandingan Tiga Kaedah Penyediaan Sampel bagi Analisis Agen Simulan Senjata Kimia

di dalam Air)

 

Alessandro Sassolini^1,4*, Andrea Malizia^1,2, Fabrizio D’Amico^1,2, Orlando Cenciarelli^1,2, Mariachiara Carestia^1,2, Daniele Di Giovanni^1,2, Leonardo Palombi^2,3, Maurizio Guidotti⁴, Carlo Bellecci^1,2, Pasquale Gaudio^1,2

 

¹Department of Industrial Engineering,

²Department of Industrial Engineering and School of Medicine and Surgery,

³Department of Bio-Medical & Prevention, School of Medicine and Surgery,

University of Rome Tor Vergata, Rome, Italy

⁴Regional Agency of Environmental Protection, Rieti, Italy

 

*Corresponding author: alessandro.sassolini@arpalazio.it

 

 

Received: 9 March 2015; Accepted: 5 April 2015

 

 

Abstract

Analytical chemistry in CBRNe (Chemical Biological Radiological Nuclear explosive) context requires not only high quality data; quickness, ruggedness and robustness are also mandatory. In this work, three samples preparation methods were compared using several organophosphorus pesticides as test compounds, used as simulants of nerve CWA (Chemical Warfare Agents) to choose the one with best characteristics. Result was obtained better with the Dispersive Liquid-Liquid Micro Extraction (DLLME), relatively new in CBRNe field, obtaining uncertainty for different simulants between 8 and 15% while a quantification limit between 0.01 and 0.08 µg/l. To optimize this extraction method, different organochlorinated solvents also tested but not relevant difference in these tests was obtained. In this work, all samples were analyzed by using a gas chromatography coupled with mass spectrometer (GC-MS) and also with Gas Chromatograph coupled with Nitrogen Phosphorous Detector (NPD) for DLLME samples to evaluate a low cost and rugged instrument adapt to field analytical methods with good performance in terms of uncertainty and sensibility even if poorer respect to the mass spectrometry.

 

Keywords:    NBC deployable laboratory, CBRNe, chemical warfare agents, dispersive micro liquid - liquid extraction, nerve agent simulants

 

Abstrak

Kontek analisis kimia di CBRNe (letupan radiologikal nuclear kimia biologi) memerlukan bukan hanya data yang berkualiti tinggi; kepantasan, kelasakan dan ketegugan juga adalah mandatori. Di dalam kajian ini, tiga kaedah penyediaan sampel dibandingkan menggunakan beberapa racun perosak organofosforus sebagai sebatian ujian, yang digunakan sebagai simulan CWA (Agen Senjata Kimia) untuk memilih ciri-ciri terbaik. Keputusan yang diperolehi adalah lebih baik dengan kaedah Pengekstrakan Mikro Cecair - Cecair Serakan (DLLME), yang agak baru di dalam bidang CBRNe, yakni ujian ketakpastian bagi simulant berbeza di antara 8 dan 15% manakala had kuantifikasi di antara 0.01 dan 0.08 μg/l. Untuk mengoptimumkan kaedah pengekstrakan ini, pelarut organoklorin berbeza juga diuji tetapi perbezaan tidak relevan telah diperolehi di dalam kajian ini. Di dalam kajian ini, semua sampel telah dianalisis dengan menggunakan kromatografi  gas bergabung dengan pengesan spektrometer jism (GC-MS) dan juga kromatografi gas bergabung dengan pengesan nitrogen fosforus (NPD) untuk sampel DLLME untuk menilai kebolehupayaan instumen yang kos rendah dan lasak dengan prestasi yang baik dari aspek ketakpastian dan sensitif meskipun kurang berbanding spektrometri jisim

 

Kata kunci: Makmal NBC, CBRNe, agen senjata kimia, pengekstrakan mikro cecair – cecair serakan, ejen saraf simulan

 

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