Headspace–mass spectrometry determination of benzene, toluene and the mixture of ethylbenzene and xylene isomers in soil samples using chemometrics

Esteve‐Turrillas, Francesc A.; Armenta, Sergio; Garrigues, Salvador; Pastor, Agustı́n; Guardia, M. de la

doi:10.1016/j.aca.2007.01.036

Cited by 38 publications

(50 citation statements)

References 21 publications

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“…The intermediate products during the electro/Fe 2+ /persulfate reaction were detected by headspace-gas chromatography-mass spectrometry (HS-GC-MS) (Esteve-Turrillas et al 2007). Samples for GC-MS analysis (Shimadzu GCMS-QP2010 Plus, Japan) were prepared as follows.…”

Section: Methodsmentioning

confidence: 99%

Selective oxidative degradation of toluene for the recovery of surfactant by an electro/Fe2+/persulfate process

Long

Zhang

2015

Environ Sci Pollut Res

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An electro/Fe(2+)/persulfate process has been conducted for toluene removal from surfactant (SDS) flushing solution, and the pseudo-second-order reaction rate constant (k2 value) of toluene removal has been optimized by a response surface methodology (RSM). The results indicated that in this process, the reaction between persulfate and externally added Fe(2+) generates sulfate-free radicals, and at the same time, Fe(2+) is electro-regenerated at the cathode by the reduction of Fe(3+). RSM based on Box-Behnken design (BBD) has been applied to analyze the experimental variables, of which the concentrations of persulfate and Fe(2+) showed a positive effect on the rate constant of toluene removal, whereas the concentration of SDS showed a negative effect. The interactions between pairs of variables proved to be significant, such as between SDS, persulfate, and Fe(2+) concentrations. ANOVA results confirmed that the proposed models were accurate and reliable for analysis of the variables of the electro/Fe(2+)/persulfate process. The shapes of the 3D response surfaces and contour plots showed that the SDS, persulfate, and Fe(2+) concentrations substantially affected the k2 value of toluene removal. The results indicated that increasing persulfate or Fe(2+) concentration increased the k2 value, whereas increasing SDS concentration decreased the k2 value. The reaction intermediates have been identified by GC-MS, and a plausible degradation pathway for toluene degradation is proposed.

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Section: Methodsmentioning

confidence: 99%

Selective oxidative degradation of toluene for the recovery of surfactant by an electro/Fe2+/persulfate process

Long

Zhang

2015

Environ Sci Pollut Res

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“…Several sample preparation techniques are used for BTEX determination in soil, including purgeand-trap [3,4], headspace sampling [5][6][7], and solid-phase microextraction (SPME) [8][9][10][11]. SPME is a simple, fast, solventless method of sample preparation for VOCs in soil analysis, which is capable of full automation and on-site application [12].…”

Section: Introductionmentioning

confidence: 99%

Quantification of BTEX in Soil by Headspace SPME–GC–MS Using Combined Standard Addition and Internal Standard Calibration

et al. 2017

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There is a great demand for simple, fast and accurate methods for quantification of volatile organic contaminants in soil samples. Solid-phase microextraction (SPME) has a huge potential for this purpose, but its application is limited by insufficient accuracy caused by a matrix effect. The aim of this research was to develop the method for BTEX quantification in soil using combined standard addition (SA) and internal standard (IS) calibration. Deuterated benzene (benzene-d6) was used as the internal standard for all analytes. The optimized method includes spiking replicate samples with different concentrations of BTEX standards and the same concentration of benzene-d6, equilibration of soil samples at 40 °C during 2 h, and SPME-GC-MS analysis. Precision and accuracy of IS and SA methods were compared on different soil matrices. Combined SA + IS method provided more precise calibration plots compared to the conventional SA calibration. The SA + IS calibration provided more precise and accurate results compared with a reference method based on solvent extraction followed by GC-MS when applied to BTEX quantification in real soil samples (spiked with diesel fuel and aged). Recoveries of BTEX from soil samples spiked with known concentrations of analytes using the developed method were in the range of 73-130% with RSD values less than 15% for all BTEX. The proposed simultaneous standard addition and internal standard approach can be advantageous and adopted for improved quantification of other toxic VOCs in soil.

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“…In recent years, coupled with different detectors, utilizing novel techniques of sample introduction and pretreatment, like solid-phase microextraction (SPME), HSGC analysis has been developed for the determination of benzene and toluene in different sample matrices, for example, water [6], soil [7, 8], human tissue [9], soft drinks [10], pharmaceutical products [11], and so forth. However, there are little reports about the HSGC analysis of benzene and toluene in pesticide formulations [12].…”

Section: Introductionmentioning

confidence: 99%

Simultaneous Determination of Benzene and Toluene in Pesticide Emulsifiable Concentrate by Headspace GC-MS

Cao

Jiang

Yang

et al. 2013

Journal of Analytical Methods in Chemistry

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The toxic inert ingredients in pesticide formulations are strictly regulated in many countries. In this paper, a simple and efficient headspace-gas chromatography-mass spectrometry (HSGC-MS) method using fluorobenzene as an internal standard (IS) for rapid simultaneous determination of benzene and toluene in pesticide emulsifiable concentrate (EC) was established. The headspace and GC-MS conditions were investigated and developed. A nonpolar fused silica Rtx-5 capillary column (30 m × 0.20 mm i.d. and 0.25 μm film thickness) with temperature programming was used. Under optimized headspace conditions, equilibration temperature of 120°C, equilibration time of 5 min, and sample size of 50 μL, the regression of the peak area ratios of benzene and toluene to IS on the concentrations of analytes fitted a linear relationship well at the concentration levels ranging from 3.2 g/L to 16.0 g/L. Standard additions of benzene and toluene to blank different matrix solutions 1ead to recoveries of 100.1%–109.5% with a relative standard deviation (RSD) of 0.3%–8.1%. The method presented here stands out as simple and easily applicable, which provides a way for the determination of toxic volatile adjuvant in liquid pesticide formulations.

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Headspace–mass spectrometry determination of benzene, toluene and the mixture of ethylbenzene and xylene isomers in soil samples using chemometrics

Cited by 38 publications

References 21 publications

Selective oxidative degradation of toluene for the recovery of surfactant by an electro/Fe2+/persulfate process

Selective oxidative degradation of toluene for the recovery of surfactant by an electro/Fe2+/persulfate process

Quantification of BTEX in Soil by Headspace SPME–GC–MS Using Combined Standard Addition and Internal Standard Calibration

Simultaneous Determination of Benzene and Toluene in Pesticide Emulsifiable Concentrate by Headspace GC-MS

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