Desenvolvimento e validação de procedimento analítico para a determinação de compostos organohalogenados em fertilizante orgânico empregando GC-ECD
Ano de defesa: | 2004 |
---|---|
Autor(a) principal: | |
Orientador(a): | |
Banca de defesa: | , |
Tipo de documento: | Dissertação |
Tipo de acesso: | Acesso aberto |
Idioma: | por |
Instituição de defesa: |
Universidade Federal de Santa Maria
Centro de Ciências Naturais e Exatas |
Programa de Pós-Graduação: |
Programa de Pós-Graduação em Química
|
Departamento: |
Química
|
País: |
Brasil
|
Palavras-chave em Português: | |
Área do conhecimento CNPq: | |
Link de acesso: | http://repositorio.ufsm.br/handle/1/27139 |
Resumo: | The growing worldwide concern regarding the life quality, especially regarding the preservation and appropriate use of natural resources and quality of food, has reflected on the productive systems. Inside this new tendency, the agroecology bursts as a feasible alternative. The ecological handling of the soil, through the use of animal excrements and of the direct planting, without the pesticides use, seeks the balance and the strengthening of the productive systems. The chicken manure is intensively used with that purpose. However, it is usually associated with materials from the aviaries beds, especially wood shaving, which can contain residues of authorized pesticides to be used as wood preservatives, as some organohalogenated compounds. In the present work, it was developed and validated an analytical procedure for the quantification of pentachlorofenol, 2,4,6-trichlorofenol, 2,4,6- trichloroanisol, 2,4,6-tribromofenol and 2,4,6-tribromoanisol residues in organic fertilizer using Gas Chromatography with Electron Capture Detection (GCECD). Some extraction conditions were appraised, as samples amount, volume and type of extraction solvents. Ultrasound bath and probe, as well as association of mechanical agitation with ultrasound bath, were used as extraction procedures. Several conditions for the purification stages and derivatization of the extracts were studied. The procedure that presented better recovery results was that in which it was used mechanical agitation associated to the ultrasound bath and ethanol/ acetic acid 9:1 (v/v) as solvent for the extraction of the analites. A column containing florisil® and sodium sulphate was used for the purification of the extracts. The derivatization stage was accomplished with anhydride acetic in alkaline medium. The conditions for the chromatographical analysis were: capillary column DB-5 (30 m x 0.25 mm d.i. x 0.25 μm thickness of the film); programming of the temperature of the column oven: 80 °C - 0 min, 200 °C (4 °C min-¹) - 0 min, 300 °C (40 °C min-¹) - 0 min; pressure of the carrier gas 24 psi; volume of injection 2 μL; temperature of the detector 330 °C. In the validation of the procedure they were appraised the following parameters: detection limit (LOD), quantification limit (LOQ), external calibration, linearity, precision (repeatability and intermediary precision) and recovery. LODs in the sample were between 11.3 and 22.5 mg kg-¹ and LOQs between 30.0 and 75.0 mg kg-¹. The curves presented r² > 0,99. The rehearsals of precision supplied acceptable results, with values of RDS between 0.3 and 12.4%. The recoveries were from 83.0 to 110.8%. The results obtained in the validation assays allowed to conclude that the developed procedure is quite appropriate to determine the studied organohalogenated compounds in organic fertilizer. The performance of the procedure was confirmed in commercial samples of organic fertilizer. |
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2022-11-29T17:46:13Z2022-11-29T17:46:13Z2004-02-17http://repositorio.ufsm.br/handle/1/27139The growing worldwide concern regarding the life quality, especially regarding the preservation and appropriate use of natural resources and quality of food, has reflected on the productive systems. Inside this new tendency, the agroecology bursts as a feasible alternative. The ecological handling of the soil, through the use of animal excrements and of the direct planting, without the pesticides use, seeks the balance and the strengthening of the productive systems. The chicken manure is intensively used with that purpose. However, it is usually associated with materials from the aviaries beds, especially wood shaving, which can contain residues of authorized pesticides to be used as wood preservatives, as some organohalogenated compounds. In the present work, it was developed and validated an analytical procedure for the quantification of pentachlorofenol, 2,4,6-trichlorofenol, 2,4,6- trichloroanisol, 2,4,6-tribromofenol and 2,4,6-tribromoanisol residues in organic fertilizer using Gas Chromatography with Electron Capture Detection (GCECD). Some extraction conditions were appraised, as samples amount, volume and type of extraction solvents. Ultrasound bath and probe, as well as association of mechanical agitation with ultrasound bath, were used as extraction procedures. Several conditions for the purification stages and derivatization of the extracts were studied. The procedure that presented better recovery results was that in which it was used mechanical agitation associated to the ultrasound bath and ethanol/ acetic acid 9:1 (v/v) as solvent for the extraction of the analites. A column containing florisil® and sodium sulphate was used for the purification of the extracts. The derivatization stage was accomplished with anhydride acetic in alkaline medium. The conditions for the chromatographical analysis were: capillary column DB-5 (30 m x 0.25 mm d.i. x 0.25 μm thickness of the film); programming of the temperature of the column oven: 80 °C - 0 min, 200 °C (4 °C min-¹) - 0 min, 300 °C (40 °C min-¹) - 0 min; pressure of the carrier gas 24 psi; volume of injection 2 μL; temperature of the detector 330 °C. In the validation of the procedure they were appraised the following parameters: detection limit (LOD), quantification limit (LOQ), external calibration, linearity, precision (repeatability and intermediary precision) and recovery. LODs in the sample were between 11.3 and 22.5 mg kg-¹ and LOQs between 30.0 and 75.0 mg kg-¹. The curves presented r² > 0,99. The rehearsals of precision supplied acceptable results, with values of RDS between 0.3 and 12.4%. The recoveries were from 83.0 to 110.8%. The results obtained in the validation assays allowed to conclude that the developed procedure is quite appropriate to determine the studied organohalogenated compounds in organic fertilizer. The performance of the procedure was confirmed in commercial samples of organic fertilizer.A crescente preocupação mundial a respeito da qualidade de vida, especialmente no que se refere à preservação e uso adequado dos recursos naturais e à qualidade dos alimentos, tem-se refletido nos sistemas produtivos. Dentro dessa nova tendência, a agroecologia desponta como uma alternativa viável. O manejo ecológico do solo, através do uso de dejetos animais e do plantio direto, sem o uso de pesticidas, visa o equilíbrio e o fortalecimento dos sistemas produtivos. O esterco de galinha é bastante empregado com esse propósito, contudo, está normalmente associado a materiais constituintes das camas de aviários, especialmente maravalha de madeira, a qual pode conter resíduos de pesticidas autorizados para uso como preservantes de madeira, como alguns compostos organohalogenados. No presente trabalho foi desenvolvido e validado um procedimento analítico para a quantificação de resíduos de pentaclorofenol, 2,4,6-triclorofenol, 2,4,6-tricloroanisol, 2,4,6-tribromofenol e 2,4,6-tribromoanisol em fertilizante orgânico, empregando Cromatografia Gasosa com Detecção por Captura de Elétrons (GC-ECD). Algumas condições de extração foram avaliadas, como quantidade de amostra, volume e tipo de solventes de extração. Banho e sonda de ultra-som, bem como a associação de agitação mecânica com banho de ultrasom, foram testados como procedimentos de extração. Várias condições para as etapas de purificação e derivatização dos extratos foram estudadas. O procedimento que apresentou melhores resultados de recuperação foi aquele onde utilizou-se agitação mecânica associada ao banho de ultra-som e etanol/ácido acético 9:1 (v/v) como solvente para a extração dos analitos. Uma coluna contendo florisil® e sulfato de sódio anidro foi empregada para a purificação dos extratos. A etapa de derivatização foi realizada com anidrido acético em meio alcalino. As condições para a análise cromatográfica foram: coluna capilar DB-5 (30 m x 0,25 mm d.i. x 0,25 μm espessura de filme); programação da temperatura do forno da coluna: 80 °C – 0 min, 200 °C (4 oC min-¹) – 0 min, 300 °C (40 oC min-¹) – 0 min; pressão do gás de arraste 24 psi; volume de injeção 2 μL; temperatura do detector 330 °C. Na validação do procedimento foram avaliados os seguintes parâmetros: limite de detecção (LOD), limite de quantificação (LOQ), calibração externa, linearidade, precisão (repetitividade e precisão intermediária) e recuperação. Os LODs na amostra ficaram entre 11,3 e 22,5 μg kg-¹ e os LOQs entre 30,0 e 75,0 μg kg-¹. As curvas apresentaram r² > 0,99. Os ensaios de precisão forneceram resultados aceitáveis, com valores de RDS entre 0,3 e 12,4%. As recuperações foram de 83,0 até 110,8%. Os resultados obtidos nos ensaios de validação permitem concluir que o procedimento desenvolvido é bastante adequado para determinar os compostos organohalogenados estudados em fertilizante orgânico. O desempenho do procedimento foi confirmado em amostras comerciais de fertilizante orgânico.Conselho Nacional de Pesquisa e Desenvolvimento Científico e Tecnológico - CNPqporUniversidade Federal de Santa MariaCentro de Ciências Naturais e ExatasPrograma de Pós-Graduação em QuímicaUFSMBrasilQuímicaAttribution-NonCommercial-NoDerivatives 4.0 Internationalhttp://creativecommons.org/licenses/by-nc-nd/4.0/info:eu-repo/semantics/openAccessFertilizante orgânicoCromatografia gasosaAgrotóxicosOrganohalogenadosCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADesenvolvimento e validação de procedimento analítico para a determinação de compostos organohalogenados em fertilizante orgânico empregando GC-ECDDevelopment and validation of an analytic procedure using GC-ECD for determination of organohalogenated compounds in organic fertilizerinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisZanella, Renatohttp://lattes.cnpq.br/2541865299438479Schneider, Rosana de Cassia de SouzaAdaime, Martha Bohrerhttp://lattes.cnpq.br/3773979222960563Wickert, Cristine1006000000006006006006006000aa2baab-94e8-4d3d-bbb2-85495ba77db5d0f2d8eb-7ba0-4ada-879a-be1badf20521a7243a36-17d0-4480-aaf4-1e61e9bc4ef4a0f5a1bf-e731-4df0-9010-ddadda7ae90areponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMCC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; charset=utf-8805http://repositorio.ufsm.br/bitstream/1/27139/2/license_rdf4460e5956bc1d1639be9ae6146a50347MD52LICENSElicense.txtlicense.txttext/plain; charset=utf-81956http://repositorio.ufsm.br/bitstream/1/27139/3/license.txt2f0571ecee68693bd5cd3f17c1e075dfMD53ORIGINALDIS_PPGQUÍMICA_2004_WICKERT_CRISTINE.pdfDIS_PPGQUÍMICA_2004_WICKERT_CRISTINE.pdfDissertação de Mestradoapplication/pdf497597http://repositorio.ufsm.br/bitstream/1/27139/1/DIS_PPGQU%c3%8dMICA_2004_WICKERT_CRISTINE.pdfc269040533083d74bbf991e97a5e3775MD511/271392022-11-29 14:46:14.039oai:repositorio.ufsm.br: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 Digital de Teses e Dissertaçõeshttps://repositorio.ufsm.br/ONGhttps://repositorio.ufsm.br/oai/requestatendimento.sib@ufsm.br||tedebc@gmail.comopendoar:2022-11-29T17:46:14Biblioteca Digital de Teses e Dissertações do UFSM - Universidade Federal de Santa Maria (UFSM)false |
dc.title.por.fl_str_mv |
Desenvolvimento e validação de procedimento analítico para a determinação de compostos organohalogenados em fertilizante orgânico empregando GC-ECD |
dc.title.alternative.eng.fl_str_mv |
Development and validation of an analytic procedure using GC-ECD for determination of organohalogenated compounds in organic fertilizer |
title |
Desenvolvimento e validação de procedimento analítico para a determinação de compostos organohalogenados em fertilizante orgânico empregando GC-ECD |
spellingShingle |
Desenvolvimento e validação de procedimento analítico para a determinação de compostos organohalogenados em fertilizante orgânico empregando GC-ECD Wickert, Cristine Fertilizante orgânico Cromatografia gasosa Agrotóxicos Organohalogenados CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Desenvolvimento e validação de procedimento analítico para a determinação de compostos organohalogenados em fertilizante orgânico empregando GC-ECD |
title_full |
Desenvolvimento e validação de procedimento analítico para a determinação de compostos organohalogenados em fertilizante orgânico empregando GC-ECD |
title_fullStr |
Desenvolvimento e validação de procedimento analítico para a determinação de compostos organohalogenados em fertilizante orgânico empregando GC-ECD |
title_full_unstemmed |
Desenvolvimento e validação de procedimento analítico para a determinação de compostos organohalogenados em fertilizante orgânico empregando GC-ECD |
title_sort |
Desenvolvimento e validação de procedimento analítico para a determinação de compostos organohalogenados em fertilizante orgânico empregando GC-ECD |
author |
Wickert, Cristine |
author_facet |
Wickert, Cristine |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Zanella, Renato |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/2541865299438479 |
dc.contributor.referee1.fl_str_mv |
Schneider, Rosana de Cassia de Souza |
dc.contributor.referee2.fl_str_mv |
Adaime, Martha Bohrer |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/3773979222960563 |
dc.contributor.author.fl_str_mv |
Wickert, Cristine |
contributor_str_mv |
Zanella, Renato Schneider, Rosana de Cassia de Souza Adaime, Martha Bohrer |
dc.subject.por.fl_str_mv |
Fertilizante orgânico Cromatografia gasosa Agrotóxicos Organohalogenados |
topic |
Fertilizante orgânico Cromatografia gasosa Agrotóxicos Organohalogenados CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
The growing worldwide concern regarding the life quality, especially regarding the preservation and appropriate use of natural resources and quality of food, has reflected on the productive systems. Inside this new tendency, the agroecology bursts as a feasible alternative. The ecological handling of the soil, through the use of animal excrements and of the direct planting, without the pesticides use, seeks the balance and the strengthening of the productive systems. The chicken manure is intensively used with that purpose. However, it is usually associated with materials from the aviaries beds, especially wood shaving, which can contain residues of authorized pesticides to be used as wood preservatives, as some organohalogenated compounds. In the present work, it was developed and validated an analytical procedure for the quantification of pentachlorofenol, 2,4,6-trichlorofenol, 2,4,6- trichloroanisol, 2,4,6-tribromofenol and 2,4,6-tribromoanisol residues in organic fertilizer using Gas Chromatography with Electron Capture Detection (GCECD). Some extraction conditions were appraised, as samples amount, volume and type of extraction solvents. Ultrasound bath and probe, as well as association of mechanical agitation with ultrasound bath, were used as extraction procedures. Several conditions for the purification stages and derivatization of the extracts were studied. The procedure that presented better recovery results was that in which it was used mechanical agitation associated to the ultrasound bath and ethanol/ acetic acid 9:1 (v/v) as solvent for the extraction of the analites. A column containing florisil® and sodium sulphate was used for the purification of the extracts. The derivatization stage was accomplished with anhydride acetic in alkaline medium. The conditions for the chromatographical analysis were: capillary column DB-5 (30 m x 0.25 mm d.i. x 0.25 μm thickness of the film); programming of the temperature of the column oven: 80 °C - 0 min, 200 °C (4 °C min-¹) - 0 min, 300 °C (40 °C min-¹) - 0 min; pressure of the carrier gas 24 psi; volume of injection 2 μL; temperature of the detector 330 °C. In the validation of the procedure they were appraised the following parameters: detection limit (LOD), quantification limit (LOQ), external calibration, linearity, precision (repeatability and intermediary precision) and recovery. LODs in the sample were between 11.3 and 22.5 mg kg-¹ and LOQs between 30.0 and 75.0 mg kg-¹. The curves presented r² > 0,99. The rehearsals of precision supplied acceptable results, with values of RDS between 0.3 and 12.4%. The recoveries were from 83.0 to 110.8%. The results obtained in the validation assays allowed to conclude that the developed procedure is quite appropriate to determine the studied organohalogenated compounds in organic fertilizer. The performance of the procedure was confirmed in commercial samples of organic fertilizer. |
publishDate |
2004 |
dc.date.issued.fl_str_mv |
2004-02-17 |
dc.date.accessioned.fl_str_mv |
2022-11-29T17:46:13Z |
dc.date.available.fl_str_mv |
2022-11-29T17:46:13Z |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/masterThesis |
format |
masterThesis |
status_str |
publishedVersion |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/27139 |
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http://repositorio.ufsm.br/handle/1/27139 |
dc.language.iso.fl_str_mv |
por |
language |
por |
dc.relation.cnpq.fl_str_mv |
100600000000 |
dc.relation.confidence.fl_str_mv |
600 600 600 600 600 |
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Attribution-NonCommercial-NoDerivatives 4.0 International http://creativecommons.org/licenses/by-nc-nd/4.0/ info:eu-repo/semantics/openAccess |
rights_invalid_str_mv |
Attribution-NonCommercial-NoDerivatives 4.0 International http://creativecommons.org/licenses/by-nc-nd/4.0/ |
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openAccess |
dc.publisher.none.fl_str_mv |
Universidade Federal de Santa Maria Centro de Ciências Naturais e Exatas |
dc.publisher.program.fl_str_mv |
Programa de Pós-Graduação em Química |
dc.publisher.initials.fl_str_mv |
UFSM |
dc.publisher.country.fl_str_mv |
Brasil |
dc.publisher.department.fl_str_mv |
Química |
publisher.none.fl_str_mv |
Universidade Federal de Santa Maria Centro de Ciências Naturais e Exatas |
dc.source.none.fl_str_mv |
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