Experimental and statistical validation of SPME-GC–MS analysis of phenol and chlorophenols in raw and treated water

Simões, Natércia Guerra; Cardoso, Vítor Vale; Ferreira, Elisabete; Benoliel, Maria João; Almeida, Cristina

doi:10.1016/j.chemosphere.2006.12.057

Cited by 89 publications

(37 citation statements)

References 19 publications

Supporting

Mentioning

Contrasting

Unclassified

Order By: Relevance

“…Phenolic compounds have been determined using different strategies, mainly exploiting separation techniques, e.g., gas chromatography and liquid chromatography [12,13]. Liquid chromatography is one of the most used techniques since derivatization of analytes is avoided [13,14].…”

Section: Introductionmentioning

confidence: 99%

Determination of priority phenolic pollutants exploiting an in-syringe dispersive liquid–liquid microextraction–multisyringe chromatography system

2015

View full text Add to dashboard Cite

An automatic phenolic compounds analyzer is presented. The system performs online magnetic-stirring-assisted dispersive liquid-liquid microextraction before multisyringe chromatography (MSC) using a monolithic Chromolith Flash RP-18e column. The extraction behavior of the following phenolic pollutants: phenol, 2-nitrophenol, 4-nitrophenol, 2-chlorophenol, 2,4-diclorophenol, and 2,4,6-trichlorophenol, has been studied. A critical comparison of extractants (tributyl phosphate, acetonitrile, hexane, and 1-chlorobutane) and disperser solvents (acetone, acetonitrile, ethanol, methanol, 1-propanol, and 2-propanol) was made. Tributyl phosphate and acetonitrile were chosen as the extractant and the disperser solvent, respectively, since these showed the best performance. Phenols were online back-extracted into NaOH and neutralized before multi-isocratic chromatographic separation. The proposed analyzer can be applied for wide linear working ranges, i.e., between 40 and 20,000 μg L(-1). The precision of the developed system has been proved, with maximum values for the intraday and interday precision of 4.4 % and 5.2 %, respectively, expressed as relative standard deviation, and high preconcentration factors (9.3-10.5) for most of the compounds studied. The method developed was successfully applied to natural water samples.

show abstract

Section: Introductionmentioning

confidence: 99%

Determination of priority phenolic pollutants exploiting an in-syringe dispersive liquid–liquid microextraction–multisyringe chromatography system

2015

View full text Add to dashboard Cite

show abstract

“…The solid‐phase microextraction (SPME) technique has been used successfully for the determination of phenols and chlorophenols in different matrices such as water 13–19, urine 20, landfill leachate 21, 22, wine 23, 24, soil 25, 26, cork macerate 26 and honey 27 samples. To the best of our knowledge, there is no study reported in the literature on the use of SPME for the determination of phenols and chlorophenols in a leather matrix.…”

Section: Introductionmentioning

confidence: 99%

Application of solid‐phase microextraction and gas chromatography‐mass spectrometry for the determination of chlorophenols in leather

Silveira¹,

Martendal²,

Soldi³

et al. 2012

J of Separation Science

View full text Add to dashboard Cite

This paper proposes a new analytical procedure based on the headspace solid-phase microextraction (HS-SPME) technique and gas chromatography-selected ion monitoring-mass spectrometry (GC-SIM-MS) for the determination of 16 phenols extracted from leather samples. The optimized conditions for the HS-SPME were obtained through two experimental designs - a two-level fractional factorial design followed by a central composite design - using the commercial SPME fiber polyacrylate 85 μm (PA). The best extraction conditions were as follows: 200 μL of derivatizing agent (acetic anhydride), 20 mL of saturated aqueous NaCl solution and extraction time and temperature of 50 min and 75°C, respectively. All optimized conditions were obtained with fixed leather sample mass (250 mg), vial volume (40 mL) and phosphate buffer pH (12) and concentration (50 mmol/L). Detection limits ranging from 0.03 to 0.20 ng/g, and relative standard deviation (RSD) lower than 10.23% (n=6) for a concentration of 800 ng/g (chlorophenols) and 1325 ng/g (2-phenylphenol) in the splitless mode were obtained. The recovery was studied at three concentration levels by adding different amounts of phenols to the leather sample and excellent recoveries ranging from 90.0 to 107.2% were obtained. The validated method was shown to be suitable for the quantification of phenols in leather samples, as it is simple, relatively fast and sensitive.

show abstract

“…20,[53][54][55][56][57][58][59][60][61][62][63][64][65][66][67][68][69] Todos os trabalhos reportados na literatura apresentam modificações peculiares no processo de extração com o objetivo de melhorar a análise e os resultados. Um exemplo é o método analítico descrito por Santana et al, 66 no qual a MEFS com dessorção em meio micelar foi aplicada para determinação de cloro-fenóis em amostras de esgoto tratado e águas subterrâneas, utilizando CLAE e um detector com arranjo de diodos (DAD).…”

Section: Microextração Em Fase Sólidaunclassified

Alternativas verdes para o preparo de amostra e determinação de poluentes fenólicos em água

Rodrigues¹,

Silva²,

Silva³

2010

Quím. Nova

View full text Add to dashboard Cite

Recebido em 8/10/09; aceito em 11/3/10; publicado na web em 20/7/10 GREEN ALTERNATIVES FOR SAMPLE PREPARATION AND DETERMINATION OF PHENOLIC POLLUTANTS IN WATER. The restricted availability of water sources suitable for consumption and high costs for obtaining potable water has caused an increase of the conscience concerning the use. Thus, there is a high demand for "environmentally safe methods" which are according to the principles of Green Chemistry. Moreover, these methods should be able to provide reliable results for the analysis of water quality for various pollutants, such as phenol. In this work, greener alternatives for sample preparation for phenol determination in aqueous matrices are presented, which include: liquid phase microextraction, solid phase microextraction, flow analysis, cloud point extraction and aqueous two-phase systems.Keywords: phenols; green chemistry; water. INTRODUÇÃONas últimas décadas, devido às consequências negativas do grande crescimento industrial e populacional, que provoca graves danos à saúde humana e à natureza, o aumento da responsabilidade ambiental tem sido visível. Diversos países têm voltado seus esforços para a busca do desenvolvimento auto-sustentável, que pode ser definido como o progresso industrial que atenda às necessidades do presente sem comprometer a capacidade das futuras gerações de satisfazerem suas próprias necessidades. 1 Inevitavelmente, essa demanda teve influência decisiva na Quí-mica. Pesquisadores têm buscado, cada vez mais, desenvolver novos métodos, 2,3 elaborar novas sínteses, 4,5 criar novas ferramentas, 6,7 que reduzam ou eliminem componentes indesejáveis de uma análise química, como, produção de resíduos, uso de reagentes tóxicos, desperdício de energia em processos industriais, etc. Química verde (QV): definição e princípiosA partir da década de 90, surge uma nova tendência em como conduzir as análises químicas, com o intuito de reduzir o impacto ambiental das mesmas. Essa nova visão é denominada Green Chemistry, ou química verde, química limpa, química ambientalmente benigna, ou ainda, química auto-sustentável. O conceito da química verde, que inclui 12 princípios básicos, é definido como o projeto, desenvolvimento e a aplicação de produtos e processos químicos com o objetivo de reduzir ou eliminar o uso ou a geração de substâncias nocivas à saúde humana e ao ambiente.8 A partir disso, iniciaram-se diversas pesquisas com o objetivo de desenvolver métodos ambientalmente seguros.Um dos principais alvos dos estudos envolvendo química verde e preocupação ambiental é o monitoramento da qualidade das águas, haja vista o papel fundamental desempenhado pela água na manutenção de todos outros segmentos da natureza. Para que esse monitoramento (não apenas da água, mas como de outras matrizes, como solos, atmosfera, etc.) fosse realizado de forma eficaz, diversas agências de controle ambiental foram criadas. Dentre elas, destacamse a Environmental Protection Agency (EPA) que, atualmente, é um dos principais órgãos de controle ambiental do mundo e, em ...

show abstract

Experimental and statistical validation of SPME-GC–MS analysis of phenol and chlorophenols in raw and treated water

Cited by 89 publications

References 19 publications

Determination of priority phenolic pollutants exploiting an in-syringe dispersive liquid–liquid microextraction–multisyringe chromatography system

Determination of priority phenolic pollutants exploiting an in-syringe dispersive liquid–liquid microextraction–multisyringe chromatography system

Application of solid‐phase microextraction and gas chromatography‐mass spectrometry for the determination of chlorophenols in leather

Alternativas verdes para o preparo de amostra e determinação de poluentes fenólicos em água

Contact Info

Product

Resources

About