scholarly journals Solid Phase Microextraction–Gas Chromatography For The Analysis Of Explosives In Post Blast Water Samples

2012 ◽  
Author(s):  
Umi Kalthom Ahmad ◽  
Kee Heng Kiu
Keyword(s):  
Gas Chromatography ◽  
Water Samples ◽  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Fiber Types ◽  
Qualitative And Quantitative Analysis ◽  
Salting Out ◽  
Fiber Coating ◽  
Stirring Effect ◽  
Direct Immersion

Dalam kajian ini, teknik pengekstrakan mikro fasa pepejal (SPME) diikuti dengan kromatografi gas (GC) telah digunakan untuk menentukan sisa letupan. Beberapa parameter termasuk masa penjerapan, masa dan suhu nyahjerapan, jenis gentian SPME, kesan pengadukan dan kesan garam telah dioptimumkan untuk mendapat data yang tepat. Penambahan 10% w/v NaCl dalam medium akues dan penggunaan gentian Carboxen/Polidimetilsiloksana (CAR/PDMS) menghasilkan pengekstrakan yang paling cekap. SPME/GC–ECD yang telah dioptimumkan digunakan untuk menganalisis sisa letupan 2,6–dinitrotoluena (2,6–DNT), trinitrotoluena (TNT) dan pentaeritritol tetranitrat (PETN) berjaya dikesan daripada sampel air. SPME/GC–ECD secara rendaman langsung didapati kaedah yang menarik digunakan untuk menganalisis bahan letupan dalam sampel air pasca letupan secara kualitatif dan kuantitatif. Kata kunci: Bahan letupan, SPME rendaman langsung, GC–ECD, sampel air pasca letupan In this study, a solid–phase microextraction (SPME) technique followed by gas chromatography (GC) was used to determine explosive residues. Several parameters including adsorption time, desorption time and temperature, SPME fiber types, stirring effect and salting out effect were optimized to obtain reproducible data with good accuracy. Addition of 10% w/v of NaCl in the aqueous medium and the use of a Carboxen/Polydimethylsiloxane (CAR/PDMS) fiber coating led to optimal extraction efficiencies. The optimized SPME/GC–ECD method was applied to the trace analysis of explosive residues in water samples. 2,6–dinitrotoluene (2,6–DNT), trinitrotoluene (TNT) and pentaerythritol tetranitrate (PETN) were successfully detected from water samples. Direct Immersion SPME/GC–ECD was found to be an attractive technique for qualitative and quantitative analysis of explosives in post blast water samples. Key words: Explosives, direct immersion SPME, GC–ECD, post blast water samples

scholarly journals Determination of Volatile Compounds in Foxtail Millet Sake Using Headspace Solid-Phase Microextraction and Gas Chromatography-Mass Spectrometry

2015 ◽  
Vol 2015 ◽  
pp. 1-9 ◽  
Author(s):  
Jingke Liu ◽  
Wei Zhao ◽  
Shaohui Li ◽  
Aixia Zhang ◽  
Yuzong Zhang ◽  
...  
Keyword(s):  
Gas Chromatography ◽  
Sample Preparation ◽  
Volatile Compounds ◽  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Foxtail Millet ◽  
Diethyl Ester ◽  
Fiber Types ◽  
Headspace Solid Phase Microextraction ◽  
Spme Fiber

The volatile compounds in foxtail millet sake were extracted by headspace solid-phase microextraction (HS-SPME) and analyzed using gas chromatography-mass spectroscopy (GC-MS). Different methods of sample preparation were used to optimize this method (SPME fiber types, sample amount, extraction time, extraction temperature, content of NaCl, and rotor speed). For final method of sample preparation, 8 mL of sake was placed in a 15 mL headspace vial with addition of 1.5 g of NaCl; a 50/30 μm DVB/CAR/PDMS SPME fiber was used for extraction at 50°C for 30 min with 10 rpm continuous stirring. A total of 41 volatile compounds were identified from the sake sample, including 9 esters, 6 alcohols, 4 acids, 4 aldehydes, 9 hydrocarbons, 7 benzene derivatives, and 2 others. The main volatile compounds were ethyl acetate, phenylethyl alcohol, butanedioic acid diethyl ester, and hexadecane. According to their odors active values (OAVs), 10 volatile compounds were established to be odor active compounds and to contribute to the typical foxtail millet sake aroma. Hexanoic acid ethyl ester was the most prominent odor active compound.

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