scholarly journals On-Line Sorbentless Cryogenic Needle Trap and GC–FID Method for the Extraction and Analysis of Trace Volatile Organic Compounds from Soil Samples

2020 ◽  
Vol 58 (10) ◽  
pp. 887-895
Author(s):  
Djavanshir Djozan ◽  
Jamal Norouzi ◽  
Mir Ali Farajzadeh

Abstract In this study, an automated sorbentless cryogenic needle trap device (ASCNTD) coupled with a gas chromatograph (GC) was developed with the aim of sampling, pre-concentration and determination of volatile organic compounds (VOCs) from soil sample. This paper describes optimization of relevant parameters, performance evaluation and an illustrative application of ASCNTD. The ASCNTD system consists of a 5 cm stainless steel needle passed through a hollow ceramic rod which is coiled with resistive nichrome wire. The set is placed in a PVC (Polyvinyl chloride) chamber through which liquid nitrogen can flow. The headspace components are circulated with a pump to pass through the needle, and this results in freeze-trapping of the VOCs on the inner surface of the needle. When extraction is completed, the analytes trapped in the inner wall of the needle were thermally desorbed and swept by the carrier gas into the GC capillary column. The parameters being effective on the extraction processes, namely headspace flow rate, the temperature and time of extraction and desorption were optimized and evaluated. The developed technique was compared to the headspace solid-phase microextraction method for the analysis of soil samples containing BTEX (Benzene, Toluene, Ethylbenzene and Xylene). The relative standard deviation values are below 8% and detection limits as low as 1.2 ng g−1 were obtained for BTEX by ASCNTD.

Separations ◽  
2020 ◽  
Vol 7 (4) ◽  
pp. 75
Author(s):  
Natalia Manousi ◽  
Erwin Rosenberg ◽  
George A. Zachariadis

A novel sample preparation method based on the use of the Arrow solid-phase microextraction device was used to extract and preconcentrate volatile organic compounds (VOCs) from milk samples prior to their determination by gas chromatography–mass spectrometry (GC-MS). The experimental parameters of the solid-phase microextraction (SPME) Arrow method were evaluated in terms of fiber type, sample volume, extraction temperature, extraction time, stirring rate and salt addition. Under the optimum extraction conditions, the SPME Arrow was compared with conventional SPME fibers to evaluate the effectiveness of the SPME Arrow method. Evaluation of the conventional SPME procedure was also performed under optimized conditions, for appropriate method comparison. Due to the larger sorption phase volume of SPME Arrow, a higher sensitivity and reproducibility were observed for the determined chromatographic peaks in comparison with conventional SPME fibers. The use of Carbon wide range (WR) SPME Arrow/polydimethylsiloxane (CAR/PDMS) SPME Arrow fibers leads to a compound-dependent improvement of a factor of 4–5x over the classical SPME setup. Moreover, the relative standard deviation (RSD) of the total volatiles for a conventional SPME procedure was 12.5%, while for SPME Arrow it was 6.2%. Finally, the novel method was successfully employed for the analysis of commercially available milk samples. The findings of this study indicate that SPME Arrow can be effectively used for the determination of volatile organic compounds in complex food matrixes.


Separations ◽  
2019 ◽  
Vol 6 (4) ◽  
pp. 51 ◽  
Author(s):  
Olga P. Ibragimova ◽  
Nassiba Baimatova ◽  
Bulat Kenessov

Current standard approaches for quantitation of volatile organic compounds (VOCs) in outdoor air are labor-intensive and/or require additional equipment. Solid-phase microextraction (SPME) is a simpler alternative; however, its application is often limited by complex calibration, the need for highly pure gases and the lack of automation. Earlier, we proposed the simple, automated and accurate method for quantitation of benzene, toluene, ethylbenzene and xylenes (BTEX) in air using 20 mL headspace vials and standard addition calibration. The aim of present study was to expand this method for quantitation of >20 VOCs in air. Twenty-five VOCs were chosen for the method development. Polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber provided better combination of detection limits and relative standard deviations of calibration slopes than other studied fibers. Optimal extraction time was 10 min. For quantification of all analytes except n-undecane, crimp top vials with samples should not stand on the autosampler tray for >8 h, while 22 most stable analytes can be quantified during 24 h. The developed method was successfully tested for automated quantification of VOCs in outdoor air samples collected in Almaty, Kazakhstan. Relative standard deviations (RSDs) of the responses of 23 VOCs were below 15.6%. Toluene-to-benzene concentration ratios were below 1.0 in colder days, indicating that most BTEX originated from non-transport-related sources.


2020 ◽  
Vol 16 (4) ◽  
pp. 404-412 ◽  
Author(s):  
Ihab Alnajim ◽  
Manjree Agarwal ◽  
Tao Liu ◽  
YongLin Ren

Background: The red flour beetle, Tribolium castaneum (Herbst) (Coleoptera: Tenebrionidae) is one of the world’s most serious stored grain insect pests. A method of early and rapid identification of red flour beetle in stored products is urgently required to improve control options. Specific chemical signals identified as Volatile Organic Compounds (VOCs) that are released by the beetle can serve as biomarkers. Methods: The Headspace Solid Phase Microextraction (HS-SPME) technique and the analytical conditions with GC and GCMS were optimised and validated for the determination of VOCs released from T. castaneum. Results: The 50/30 μm DVB/CAR/PDMS SPME fibre was selected for extraction of VOCs from T. castaneum. The efficiency of extraction of VOCs was significantly affected by the extraction time, temperature, insect density and type of SPME fibre. Twenty-three VOCs were extracted from insects in 4 mL flask at 35 ± 1°C for four hours of extraction and separated and identified with gas chromatography-mass spectroscopy. The major VOCs or chemical signals from T. castaneum were 1-pentadecene, p-Benzoquinone, 2-methyl- and p-Benzoquinone, 2-ethyl. Conclusion: This study showed that HS-SPME GC technology is a robust and cost-effective method for extraction and identification of the unique VOCs produced by T. castaneum. Therefore, this technology could lead to a new approach in the timely detection of T. castaneum and its subsequent treatment.


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