New SPME fibre for analysis of mequinol emitted from DVDs

2011 ◽  
Vol 65 (2) ◽  
Author(s):  
Magdalena Palacz ◽  
Wiesław Wasiak

AbstractA piece of fused-silica fibre coated with silica modified with ketamine-groups was used as a solidphase microextraction (SPME) fibre and its efficiency in the qualitative and quantitative analysis of volatile organic compounds released from coloured overprinting on DVDs was evaluated. The effect of the parameters that can affect the SPME procedure, such as extraction time, extraction temperature, desorption temperature, was investigated to determine the analytical performance of this novel fibre in the qualitative and quantitative analyses of organic compounds. The optimised procedure was applied to the qualitative and quantitative analyses of organic compounds released from coloured overprinting on DVDs. The limit of detection of 4-methoxyphenol (mequinol) was 88 × 10−3 μg mL−1, while the limit of quantification (LOQ) was calculated as ten times the baseline noise, i.e. 3.1 × 10−1 μg mL−1. The proposed fibre was used successfully for preconcentration of the volatile organic compounds from the gaseous phase of DVD samples.

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.


Author(s):  
Antonia Flores ◽  
Silvia Sorolla ◽  
Concepció Casas ◽  
Rosa Cuadros ◽  
Anna Bacardit

Volatile organic compounds (VOCs) and Semi-Volatile Organic Compounds (SVOCs) arise from the chemicals used in the various stages of the leather manufacturing process. An important aim of the tanning industry is to minimize or eliminate VOCs and SVOCs, without lowering the quality of leather.   This paper shows the development of a new headspace-solid phase micro extraction coupled with gas chromatography–mass spectrometry (HS-SPME/GC-MS) method for the identification of VOCs and SVOCs emitted by newly designed polymers for the leather finishing operation. These new polymers are polyurethane resins designed to reduce the VOC and SVOC concentration. This method enables a simple and fast determination of the qualitative and semi-quantitative content of VOCs and SVOCs in polyurethane-type finishing resins. The chemicals that are of concern in this paper are the following: Dipropylene glycol Monomethyl Ether (DPGME), DBE-3 (a mixture of dibasic esters) and Triethylamine (TEA). The test conditions that have been determined to carry out the HS-SPME assay are the following: incubation time (2 hours), extraction temperature and time (40°C; 5 minutes) and the desorption conditions (280°C, 50 seconds).  Ten samples of laboratory scale resins were tested by HS-SPME followed by gas chromatography (GC-MS). DPGME and DBE-3 (a mixture of dimethyl adipate, dimethyl glutarate and dimethyl succinate) have been identified effectively. The compounds are identified by a quantitative method using external calibration curves for the target compounds. The technique is not effective to determine the TEA compound, since the chromatograms shown poor resolution peaks for the standard. 


2020 ◽  
pp. 113-120
Author(s):  
T.S. Ulanova ◽  
◽  
T.V. Nurislamova ◽  
N.A. Popova ◽  
O.A. Mal'tseva ◽  
...  

The article dwells on results obtained via experimental research on working out a gas chromatography procedure for determining trichloroethylene and tetrachloroethylene in ambient air. Experiments were performed on substances which had low limits of detection with gas-liquid chromatography with electron capture detection (GLC/ECD) when examined substances were absorbed from ambient air on Tenax TA sorbent. Optimal gas chromatography parameters were established with a hardware-software complex based on «Crystal-5000» gas chromatographer and use of a column from IDBPX-VOL series, 60m⋅0.32mm⋅1.8µm, under the following temperatures: column, 50–230о С; evaporator, 250о С; detector, 250о С. The developed capillary gas chromatography procedure allows determining trichloroethylene in concentrations ranging from 0.000146 to 0.00146 mg/m3, and tetrachloroethylene, from 0.000081 to 0.00081 mg/m3 with inaccuracy not exceeding 25.0%. We performed metrological assessment of the procedure and it allowed determining quality of analysis results for trichloroethylene and tetrachloroethylene; they were as follows: precision, 21.97% and 14.3%: repeatability, 4.22% and 3.38%; reproducibility, 5.66% and 4.9%. Limit of detection (LOD) for trichloroethylene and tetrachloroethylene was =0.0000038 mg/dm3 and =0.00000083 mg/dm3 accordingly. Limit of quantitative determination (LOQ) was =0.000013 mg/m3 for trichloroethylene, and = 0.0000028 mg/m3 for tetrachloroethylene. The developed procedure allowed detecting contents of the examined substances in ambient air near a construction site and a dry-cleaner’s, trichloroethylene in a range from 0.00001 mg/m3 to 0.0009 mg/m3, tetrachloroethylene, from 0.000011 mg/m3 to 0.00039 mg/m3. This unified high-sensitive and selective procedure is recommended for systemic control over potentially hazardous volatile organic compounds in ambient air as it allows providing objective and reliable hygienic assessment of chemical safety and quality of the environment and health risk assessment.


2020 ◽  
pp. 113-120
Author(s):  
T.S. Ulanovа ◽  
◽  
T.V. Nurislamova ◽  
N.A. Popova ◽  
O.A. Mal'tseva ◽  
...  

The article dwells on results obtained via experimental research on working out a gas chromatography procedure for determining trichloroethylene and tetrachloroethylene in ambient air. Experiments were performed on substances which had low limits of detection with gas-liquid chromatography with electron capture detection (GLC/ECD) when examined substances were absorbed from ambient air on Tenax TA sorbent. Optimal gas chromatography parameters were established with a hardware-software complex based on «Crystal-5000» gas chromatographer and use of a column from IDBPX-VOL series, 60m⋅0.32mm⋅1.8µm, under the following temperatures: column, 50–230о С; evaporator, 250о С; detector, 250о С. The developed capillary gas chromatography procedure allows determining trichloroethylene in concentrations ranging from 0.000146 to 0.00146 mg/m3, and tetrachloroethylene, from 0.000081 to 0.00081 mg/m3 with inaccuracy not exceeding 25.0%. We performed metrological assessment of the procedure and it allowed determining quality of analysis results for trichloroethylene and tetrachloroethylene; they were as follows: precision, 21.97% and 14.3%: repeatability, 4.22% and 3.38%; reproducibility, 5.66% and 4.9%. Limit of detection (LOD) for trichloroethylene and tetrachloroethylene was =0.0000038 mg/dm3 and =0.00000083 mg/dm3 accordingly. Limit of quantitative determination (LOQ) was =0.000013 mg/m3 for trichloroethylene, and = 0.0000028 mg/m3 for tetrachloroethylene. The developed procedure allowed detecting contents of the examined substances in ambient air near a construction site and a dry-cleaner’s, trichloroethylene in a range from 0.00001 mg/m3 to 0.0009 mg/m3, tetrachloroethylene, from 0.000011 mg/m3 to 0.00039 mg/m3. This unified high-sensitive and selective procedure is recommended for systemic control over potentially hazardous volatile organic compounds in ambient air as it allows providing objective and reliable hygienic assessment of chemical safety and quality of the environment and health risk assessment.


2020 ◽  
Vol 20 (6) ◽  
pp. 4013-4029 ◽  
Author(s):  
Alexander B. Thames ◽  
William H. Brune ◽  
David O. Miller ◽  
Hannah M. Allen ◽  
Eric C. Apel ◽  
...  

Abstract. The hydroxyl radical (OH) reacts with thousands of chemical species in the atmosphere, initiating their removal and the chemical reaction sequences that produce ozone, secondary aerosols, and gas-phase acids. OH reactivity, which is the inverse of OH lifetime, influences the OH abundance and the ability of OH to cleanse the atmosphere. The NASA Atmospheric Tomography (ATom) campaign used instruments on the NASA DC-8 aircraft to measure OH reactivity and more than 100 trace chemical species. ATom presented a unique opportunity to test the completeness of the OH reactivity calculated from the chemical species measurements by comparing it to the measured OH reactivity over two oceans across four seasons. Although the calculated OH reactivity was below the limit of detection for the ATom instrument used to measure OH reactivity throughout much of the free troposphere, the instrument was able to measure the OH reactivity in and just above the marine boundary layer. The mean measured value of OH reactivity in the marine boundary layer across all latitudes and all ATom deployments was 1.9 s−1, which is 0.5 s−1 larger than the mean calculated OH reactivity. The missing OH reactivity, the difference between the measured and calculated OH reactivity, varied between 0 and 3.5 s−1, with the highest values over the Northern Hemisphere Pacific Ocean. Correlations of missing OH reactivity with formaldehyde, dimethyl sulfide, butanal, and sea surface temperature suggest the presence of unmeasured or unknown volatile organic compounds or oxygenated volatile organic compounds associated with ocean emissions.


2020 ◽  
Vol 14 (2) ◽  
pp. 61
Author(s):  
Rozita Osman

Headspace solid phase microextraction (HS-SPME) was employed for the extraction of volatile organic compounds (VOCs) in MD2 pineapple (Ananas comosus L. var. comosus cv. MD2). Optimisation of HS-SPME operating parameters was conducted using three-factor, three-level Box–Behnken response surface experimental design to evaluate the interactive effects of temperature (30 – 50 ºC), extraction time (10 – 30 min) and salting effect (1 – 3 g of salt addition) on the amount of selected VOCs. Determination of VOCs was done using gas chromatography with spectrometry detector (GC-MSD). Extraction temperature was found to be significant (p < 0.05) in increasing the amount of selected VOCs (ethyl acetate, methyl isobutyrate and butanoic acid methyl ester). Based on the maximum amount of these VOCs, the optimum operating extraction conditions for HS-SPME were set up at temperature of 30 °C, time of 29 min and salt addition of 1 g. The optimized HS-SPME conditions were employed for the extraction of VOCs from pineapple of different varieties.


2010 ◽  
Vol 17 (4) ◽  
pp. 637-649 ◽  
Author(s):  
Jacek Gębicki ◽  
Adam Kloskowski

Electrochemical Sensor for Measurement of Volatile Organic Compounds Employing Square Wave Perturbation VoltageThe paper presents the results of investigation on a prototype sensor for measurement of benzaldehyde in air. Sensitivity and limit of quantification of the sensor were determined for different internal electrolytes using square wave voltammetry (SWV) as the detection technique. The working and counter electrodes were made of platinum. Ionic liquids 1-hexyl, 3-methylimidazolium chloride, 1-hexyl, 3-methylimidazolium bis (trifluoro-methanesulfonyl) imide and 1-butyl, 3-methylimidazolium tricyanomethan constituted the internal electrolyte. A polydimethylsiloxane (PDMS) membrane separated the gaseous medium from the electrolyte.


2019 ◽  
Author(s):  
Alexander B. Thames ◽  
William H. Brune ◽  
David O. Miller ◽  
Hannah M. Allen ◽  
Eric C. Apel ◽  
...  

Abstract. The hydroxyl radical (OH) reacts with thousands of chemical species in the atmosphere, initiating their removal and the chemical reaction sequences that produce ozone, secondary aerosols, and gas-phase acids. OH reactivity, which is the inverse of OH lifetime, influences the OH abundance and the ability of OH to cleanse the atmosphere. The NASA Atmospheric Tomography (ATom) campaign used instruments on the NASA DC-8 aircraft to measure OH reactivity and more than 100 trace chemical species. ATom presented a unique opportunity to test the completeness of the OH reactivity calculated from the chemical species measurements by comparing it to the measured OH reactivity over two oceans across four seasons. Although the calculated OH reactivity was below the OH reactivity instrument's limit-of-detection for much of the free troposphere, the OHR instrument was able to measure the OH reactivity in and just above the marine boundary layer. The average measured value of OH reactivity in the marine boundary layer across all latitudes and all ATom phases was 1.9 s−1, which 0.5 s−1 larger than the average calculated OH reactivity. Concurrently, missing OH reactivity, the difference between the measured and calculated OH reactivity, was measured to be ~ 0.5–2.0 s−1 at some locations in the tropics and midlatitudes. Correlations of missing OH reactivity with formaldehyde, dimethyl sulfide, butanal, and sea surface temperature suggest the presence of unmeasured or unknown volatile organic compounds or oxygenated volatile organic compounds associated with ocean emissions.


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