Analysis of chlorobenzenes in soils by headspace solid-phase microextraction and gas chromatography-ion trap mass spectrometry

Santos, F.J.; Sarrión, M.N; Galcerán, M.T.

doi:10.1016/s0021-9673(97)00132-5

Cited by 54 publications

(28 citation statements)

References 36 publications

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“…When the volume of acetone was higher than 20 μL, the responses of all of the compounds were observed to drop. The increase in the ECD response when a small volume of acetone is added can be explained by the solvent molecules helping to liberate the analytes from active sites in the soil and hence to drag them from the matrix into the gas phase [2]. However, too much solvent creates an additional phase in Fig.…”

Section: Effect Of Adding Solventsmentioning

confidence: 99%

“…Due to their widespread use over several decades, chlorobenzenes have become very common in the environment. They are found in water, soil, sediments, sewage sludges and aquatic biota [1,2]. These compounds have high octanol-water partition coefficients [3], so biological accumulation can be expected in the aquatic ecosystem.…”

Section: Introductionmentioning

confidence: 99%

“…Due to the low concentration levels targeted, an initial enrichment step is usually needed. The solid-phase microextraction (SPME) technique has demonstrated a variety of inherent advantageous features and superior performance over traditional pretreatment methods for the analysis of chlorobenzenes in air [6,7] and soil matrices [1,2,8]. Although satisfactory results have been obtained using commercial poly(dimethylsiloxane) (PDMS) coatings [1,2,7,8], different commercial SPME fiber coatings (PDMS, Carboxen-PDMS, PDMSdivinylbenzene (DVB) and polyacrylate (PA) were eval-uated by Barro et al in order to optimize the extraction [6], and the PDMS-DVB fiber was selected for further analysis of chlorobenzenes.…”

Section: Introductionmentioning

confidence: 99%

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A solid-phase microextraction fiber coated with diglycidyloxycalix[4]arene yields very high extraction selectivity and sensitivity during the analysis of chlorobenzenes in soil

Zeng

2006

Anal Bioanal Chem

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A novel fiber coated with sol-gel (5,11,17,23-tetra-tert-butyl-25,27-dihydroxy-26,28-diglycidyloxycalix [4]arene/hydroxy-terminated silicone oil; diglycidyloxy-C[4]/OH-TSO) was prepared for use with headspace solidphase microextraction (HS-SPME) combined with gas chromatography (GC) and electron capture detection (ECD), which was applied in order to determine nine chlorobenzenes in soil matrices. Due to the improved fiber preparation, which increases the percentage of calixarene in the coating, the new calixarene fiber exhibits very high extraction selectivity and sensitivity to chlorine-substituted compounds. Various parameters affecting the extraction efficiency were optimized in order to maximize the sensitivity during the chlorobenzene analysis. Interferences from different soil matrices with different characteristics were investigated, and the amount extracted was strongly influenced by the matrix. Therefore, a standard addition protocol was performed on the real soil samples. The linear ranges of detection for the chlorobenzenes tested covered three orders of magnitude, and correlation coefficients >0.9976 and relative standard deviations (RSD) <8% were observed. The detection limits were found at sub-ng/g of soil levels, which were about an order of magnitude lower than those given by the commercial poly(dimethylsiloxane) (PDMS) coating for most of the compounds. The recoveries ranged from 64 to 109.6% for each analyte in the real kaleyard soil matrix when different concentration levels were determined over the linear range, which confirmed the reliability and feasibility of the HS-SPME/ GC-ECD approach using the fiber coated with diglycidyloxy-C[4]/OH-TSO for the ultratrace analysis of chlorobenzenes in complex matrices.

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Section: Effect Of Adding Solventsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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A solid-phase microextraction fiber coated with diglycidyloxycalix[4]arene yields very high extraction selectivity and sensitivity during the analysis of chlorobenzenes in soil

Zeng

2006

Anal Bioanal Chem

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“…Volatile halogenated organic compounds (VHOCs) and chlorobenzenes have received special attention as soil pollutants (2)(3)(4)(5). They have been used as solvents, cleaning and degreasing agents, polymerization modifiers, and heat-exchange fluids (6).…”

Section: Introductionmentioning

confidence: 99%

“…This group of compounds includes several suspected carcinogens; for example, tetrachloroethylene has been classified as probable human carcinogen (class 2A) by the International Agency for Research on Cancer (7,8). Chlorobenzenes are also introduced into the environment in considerable amounts through their use as solvents, dielectric fluids, deodorants, and as intermediates in the manufacture of other chemical products such as pesticides, phenols, and dyestuffs (3,9). They are prevalent in both solid and liquid industrial effluents and in atmospheric discharges.…”

Section: Introductionmentioning

confidence: 99%

Development of an environmentally friendly methodological approach to determine chlorinated hydrocarbons and chlorobenzenes in soils

Casas-Ferreira

Laespada

Pavón

et al. 2014

Green Chemistry Letters and Reviews

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A modified version of the quick, easy, cheap, efficient, rugged, and safe method is proposed for the determination of chlorinated pollutants in soil samples. Measurements were collected using a programmed temperature vaporizer coupled to a gas chromatograph and a µ-electron capture detector. The optimization and validation of this extraction technique for these compounds in soils have been performed in order to provide an alternative tool for determining these kinds of pollutants in soils. Advantages over conventional extraction techniques include the applicability to compounds of very different volatilities and polarities, the low cost of the reagents employed, and the possibility of being used by nonspecialist operators, with standard analytical tools. This method can be considered more environmentally friendly, due to the reduction of solvent and energy consumption and to the elimination of harmful organic solvents, reducing the negative impact of chemical analyses on the environment (principles of green analytical chemistry).

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Investigation by solid-phase micro-extraction and gas chromatography/mass spectrometry of organic films on stone monuments

Angelis

Tullio

Mellerio

et al. 1999

Rapid Commun. Mass Spectrom.

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Deposition of organic chemicals on historical buildings is a well-known phenomenon. Such material originates from airborne pollution, from human activity, and from natural sources, and it tends to accumulate over long times on the surfaces in the form of a black film which covers considerable portions of the monument surface. Analysis is generally performed on grams of particulate, removed with obvious serious detriment to the monument itself; this material is then conventionally extracted with solvents and analyzed by gas chromatography/mass spectrometry (GC/MS). We propose here a new analytical strategy which takes advantage of the dry solid-phase micro-extraction headspace technique coupled with GC/MS. For this purpose, we used samples of no more than 100 mg of powdered material for each measurement. The black crusts coating the stone surfaces of ancient monuments, dating back to the 13-17th centuries and located in small towns, between high mountains and far away from urban (polluted) environments, have been analyzed. Despite their locations, organic chemicals connected with human activity from our contemporary age, hydrocarbons, PAHs, oxy-PAHs, and herbicides have been revealed. In addition fatty acid residues, probably due to microorganism growths, as well as a large number of mono-and sesquiterpenes reasonably arising from local natural sources, have been detected. The technique we describe, which has been used for the first time in a cultural heritage context, is rapid and not detrimental to the piece of art. The chromatograms thus obtained are characterized by a low background level and a high signal to noise ratio. Copyright # 1999 John Wiley & Sons, Ltd. Received 11 March 1999; Accepted 14 March 1999A significant part of our cultural heritage is made of stone, and most of it is constituted by buildings and outdoor exposed monuments. They inexorably suffer from ageing and decay processes, which are mainly due both to atmospheric phenomena and to the activities of human beings; particularly in recent times, atmospheric pollution threatens even their very existence. In our contemporary age, we are almost accustomed to seeing their grey surfaces, which turn to black especially in the chiselled parts or those protected from the direct impact of rain. The monument surface, in fact, acts as a repository of organic chemicals, which originate from airborne pollution and human activity in general, from aerosols and plant vapours, from natural fires, from growth of microorganisms and, finally, from the ageing of a possible chemical treatment used by the artist who originally polished the stone surface.1 The wet and dry organic deposition is apparent as a black crust and, besides being responsible for its unpleasant aspect and primarily for the monument decay, from a different point of view is also a chemical record of the history of the monument itself and of the geographic area where it is located.The combined action on a carbonate surface of the many physical and chemical agents, such as temperature, sun irradi...

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Analysis of chlorobenzenes in soils by headspace solid-phase microextraction and gas chromatography-ion trap mass spectrometry

Cited by 54 publications

References 36 publications

A solid-phase microextraction fiber coated with diglycidyloxycalix[4]arene yields very high extraction selectivity and sensitivity during the analysis of chlorobenzenes in soil

A solid-phase microextraction fiber coated with diglycidyloxycalix[4]arene yields very high extraction selectivity and sensitivity during the analysis of chlorobenzenes in soil

Development of an environmentally friendly methodological approach to determine chlorinated hydrocarbons and chlorobenzenes in soils

Investigation by solid-phase micro-extraction and gas chromatography/mass spectrometry of organic films on stone monuments

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