Desenvolvimento de metodologia para análise de especiação de cromo em fertilizantes orgânicos
Ano de defesa: | 2022 |
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Autor(a) principal: | |
Orientador(a): | |
Banca de defesa: | , , , |
Tipo de documento: | Tese |
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: | |
Palavras-chave em Inglês: | |
Área do conhecimento CNPq: | |
Link de acesso: | http://repositorio.ufsm.br/handle/1/27560 |
Resumo: | In this work, a methodology was developed for the analysis of chromium speciation in organic fertilizer by liquid chromatography coupled to inductively coupled plasma mass spectrometry (LC-ICP-MS). For the evaluation of the methodology, different samples of organic fertilizer were used, with different contents of organic matter, where, firstly, the samples were submitted to an acid decomposition process for determination of total chromium and later conditions of extraction and determination of Cr(VI). For the initial optimizations of this work, the EPA 3060A Method was used as a reference and adaptations were made. This method consists of alkaline extraction (pH 11,5), using a solution of 0.28 mol L-1 Na2CO3 with 0.5 mol L-1 NaOH and heating at 90-95 ºC for 60 min. Speciation analysis was performed using the LC-ICP-MS technique, where liquid chromatography conditions were evaluated, such as the type of separation column, type and concentration of the mobile phase and flow rate. The dionex AG7 column and pre-column C18, the mobile phase 15 mmol L-1 HNO3 at a flow rate of 0.5 mL min-1 were optimized as the best conditions. For the validation of this methodology, some figures of merit were evaluated, such as linearity, limit of detection (LOD), limit of quantification (LOQ), precision (repeatability and intra-laboratory reproducibility), robustness and accuracy. The sample preparation conditions for the determination of Cr(VI) were also evaluated using 0.28 mol L-1 Na2CO3 with 0.5 mol L-1 NaOH, 0.02 mmol L-1 diphenylcarbazide with 2.4 mmol L-1 EDTA, 50 mmol L-1 EDTA and H2O as extracting solvents. The best extraction condition for Cr(VI) was 0.28 mol L-1 Na2CO3 with 0.5 mol L-1 NaOH, using 10 mL and 20 mg of sample. Concentrations of 0.14 mol L-1 Na2CO3 + 0.25 mol L-1 NaOH and 0.07 mol L-1 Na2CO3 + 0.125 mol L-1 NaOH were evaluated to avoid interference and possible damage to the chromatographic column. 0.07 mol L-1 Na2CO3 + 0.125 mol L-1 NaOH was the best condition, since there was no significant change between the different extractor solvent concentrations, making it suitable for use in the extraction of the other evaluations. As a comparative method, the same extracts were analyzed by ion chromatography-visible spectrophotometry (IC-Vis), for the determination of Cr(VI) based on the official EPA 218.7 method, in which a good agreement was obtained between the two techniques. |
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2023-01-11T14:38:00Z2023-01-11T14:38:00Z2022-10-28http://repositorio.ufsm.br/handle/1/27560In this work, a methodology was developed for the analysis of chromium speciation in organic fertilizer by liquid chromatography coupled to inductively coupled plasma mass spectrometry (LC-ICP-MS). For the evaluation of the methodology, different samples of organic fertilizer were used, with different contents of organic matter, where, firstly, the samples were submitted to an acid decomposition process for determination of total chromium and later conditions of extraction and determination of Cr(VI). For the initial optimizations of this work, the EPA 3060A Method was used as a reference and adaptations were made. This method consists of alkaline extraction (pH 11,5), using a solution of 0.28 mol L-1 Na2CO3 with 0.5 mol L-1 NaOH and heating at 90-95 ºC for 60 min. Speciation analysis was performed using the LC-ICP-MS technique, where liquid chromatography conditions were evaluated, such as the type of separation column, type and concentration of the mobile phase and flow rate. The dionex AG7 column and pre-column C18, the mobile phase 15 mmol L-1 HNO3 at a flow rate of 0.5 mL min-1 were optimized as the best conditions. For the validation of this methodology, some figures of merit were evaluated, such as linearity, limit of detection (LOD), limit of quantification (LOQ), precision (repeatability and intra-laboratory reproducibility), robustness and accuracy. The sample preparation conditions for the determination of Cr(VI) were also evaluated using 0.28 mol L-1 Na2CO3 with 0.5 mol L-1 NaOH, 0.02 mmol L-1 diphenylcarbazide with 2.4 mmol L-1 EDTA, 50 mmol L-1 EDTA and H2O as extracting solvents. The best extraction condition for Cr(VI) was 0.28 mol L-1 Na2CO3 with 0.5 mol L-1 NaOH, using 10 mL and 20 mg of sample. Concentrations of 0.14 mol L-1 Na2CO3 + 0.25 mol L-1 NaOH and 0.07 mol L-1 Na2CO3 + 0.125 mol L-1 NaOH were evaluated to avoid interference and possible damage to the chromatographic column. 0.07 mol L-1 Na2CO3 + 0.125 mol L-1 NaOH was the best condition, since there was no significant change between the different extractor solvent concentrations, making it suitable for use in the extraction of the other evaluations. As a comparative method, the same extracts were analyzed by ion chromatography-visible spectrophotometry (IC-Vis), for the determination of Cr(VI) based on the official EPA 218.7 method, in which a good agreement was obtained between the two techniques.Neste trabalho foi desenvolvida uma metodologia para análise de especiação de cromo em fertilizante orgânico por cromatografia a líquido acoplada a espectrometria de massa com plasma indutivamente acoplado (LC-ICP-MS). Para a avaliação da metodologia foram utilizadas diferentes amostras de fertilizante orgânico, com distintos teores de matéria orgânica. Primeiramente as amostras foram submetidas a um processo de decomposição ácida para a determinação de cromo total por ICP-MS e posteriormente foram avaliadas condições de extração e determinação de Cr(VI). Para as otimizações iniciais deste trabalho foi utilizado o Método EPA 3060A como referência e adaptações foram realizadas. Este método consiste na extração alcalina (pH 11,5), usando uma solução a 0,28 mol L-1 Na2CO3 com 0,5 mol L-1 NaOH e aquecimento a 90-95 ºC por 60 min. A análise de especiação foi feita pela técnica de LC-ICP-MS, onde foram avaliadas as condições da LC: tipo de coluna de separação, tipo e concentração da fase móvel e vazão. Foram escolhidas como as melhores condições a coluna dionex AG7 e pré-coluna C18 e a fase móvel de solução de HNO3 15 mmol L-1 na vazão de 0,5 mL min-1. Para a validação desta metodologia, foram avaliadas algumas figuras de mérito, como linearidade, limite de detecção (LOD), limite de quantificação (LOQ), precisão (repetitividade e reprodutibilidade intralaboratorial), robustez e exatidão. As condições de preparo de amostra para a determinação de Cr(VI) também foram avaliadas utilizando 0,28 mol L-1 Na2CO3 com 0,50 mol L-1 NaOH, 0,02 mmol L-1 difenilcarbazida com 2,40 mmol L-1 EDTA, 50 mmol L-1 EDTA e H2O como solventes extratores. A melhor condição de extração para Cr(VI) foi utilizando 25 mg de amostra e 10 mL 0,28 mol L-1 Na2CO3 com 0,50 mol L-1 NaOH. Concentrações de 0,14 mol L-1 Na2CO3 + 0,25 mol L-1 NaOH e 0,07 mol L-1 Na2CO3 + 0,125 mol L-1 NaOH foram avaliadas a fim de evitar interferências e possíveis danos a coluna cromatográfica. 0,07 mol L-1 Na2CO3 + 0,125 mol L-1 NaOH foi a melhor condição, visto que não houve alteração significativa entre as diferentes concentrações de solvente extrator, se tornando apta para o uso na extração das demais avaliações. Como método comparativo, os mesmos extratos foram analisados por cromatografia iônica-espectrofotometria no visível (IC-Vis), para a determinação de Cr(VI) baseado no método oficial EPA 218.7, na qual foi obtido uma boa concordância entre as duas técnicas.Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPESporUniversidade 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/openAccessEspeciação de cromoFertilizante orgânicoCromatografiaPreparo de amostraLegislaçãoChromium speciationOrganic fertilizerChromatographySample preparationLegislationCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADesenvolvimento de metodologia para análise de especiação de cromo em fertilizantes orgânicosMethodology development for chromium speciation analysis in organic fertilizersinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisDressler, Valderi Luizhttp://lattes.cnpq.br/4054740296547580Nogueira, Ana Rita de AraújoSantos, Clarissa Marques Moreira dosAntes, Fabiane GoldschmidtRosa, Francisco da Cunhahttp://lattes.cnpq.br/4113025616761764Heidrich, Graciela Marini10060000000060060060060060060060029c59cfe-a489-425c-88a5-18fdf7cbf2586d13e21a-180a-4275-90f9-3338c1462961a6a3c94c-0f6a-4095-8ff8-baf8716d2f6474155d13-8098-4ad4-864e-a334be1e29acbd1e6c65-ad34-4826-bfac-8a91b18e9704c2611fc3-195d-4dc8-9113-5ceb22f090b8reponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMLICENSElicense.txtlicense.txttext/plain; charset=utf-81956http://repositorio.ufsm.br/bitstream/1/27560/3/license.txt2f0571ecee68693bd5cd3f17c1e075dfMD53ORIGINALTES_PPGQUIMICA_2022_HEIDRICH_GRACIELA.pdfTES_PPGQUIMICA_2022_HEIDRICH_GRACIELA.pdfTeseapplication/pdf2078636http://repositorio.ufsm.br/bitstream/1/27560/1/TES_PPGQUIMICA_2022_HEIDRICH_GRACIELA.pdf8a7d948f1e88a82d0bf812d21b790c75MD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; charset=utf-8805http://repositorio.ufsm.br/bitstream/1/27560/2/license_rdf4460e5956bc1d1639be9ae6146a50347MD521/275602023-01-11 11:38:01.012oai: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:2023-01-11T14:38:01Biblioteca Digital de Teses e Dissertações do UFSM - Universidade Federal de Santa Maria (UFSM)false |
dc.title.por.fl_str_mv |
Desenvolvimento de metodologia para análise de especiação de cromo em fertilizantes orgânicos |
dc.title.alternative.eng.fl_str_mv |
Methodology development for chromium speciation analysis in organic fertilizers |
title |
Desenvolvimento de metodologia para análise de especiação de cromo em fertilizantes orgânicos |
spellingShingle |
Desenvolvimento de metodologia para análise de especiação de cromo em fertilizantes orgânicos Heidrich, Graciela Marini Especiação de cromo Fertilizante orgânico Cromatografia Preparo de amostra Legislação Chromium speciation Organic fertilizer Chromatography Sample preparation Legislation CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Desenvolvimento de metodologia para análise de especiação de cromo em fertilizantes orgânicos |
title_full |
Desenvolvimento de metodologia para análise de especiação de cromo em fertilizantes orgânicos |
title_fullStr |
Desenvolvimento de metodologia para análise de especiação de cromo em fertilizantes orgânicos |
title_full_unstemmed |
Desenvolvimento de metodologia para análise de especiação de cromo em fertilizantes orgânicos |
title_sort |
Desenvolvimento de metodologia para análise de especiação de cromo em fertilizantes orgânicos |
author |
Heidrich, Graciela Marini |
author_facet |
Heidrich, Graciela Marini |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Dressler, Valderi Luiz |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/4054740296547580 |
dc.contributor.referee1.fl_str_mv |
Nogueira, Ana Rita de Araújo |
dc.contributor.referee2.fl_str_mv |
Santos, Clarissa Marques Moreira dos |
dc.contributor.referee3.fl_str_mv |
Antes, Fabiane Goldschmidt |
dc.contributor.referee4.fl_str_mv |
Rosa, Francisco da Cunha |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/4113025616761764 |
dc.contributor.author.fl_str_mv |
Heidrich, Graciela Marini |
contributor_str_mv |
Dressler, Valderi Luiz Nogueira, Ana Rita de Araújo Santos, Clarissa Marques Moreira dos Antes, Fabiane Goldschmidt Rosa, Francisco da Cunha |
dc.subject.por.fl_str_mv |
Especiação de cromo Fertilizante orgânico Cromatografia Preparo de amostra Legislação |
topic |
Especiação de cromo Fertilizante orgânico Cromatografia Preparo de amostra Legislação Chromium speciation Organic fertilizer Chromatography Sample preparation Legislation CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Chromium speciation Organic fertilizer Chromatography Sample preparation Legislation |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
In this work, a methodology was developed for the analysis of chromium speciation in organic fertilizer by liquid chromatography coupled to inductively coupled plasma mass spectrometry (LC-ICP-MS). For the evaluation of the methodology, different samples of organic fertilizer were used, with different contents of organic matter, where, firstly, the samples were submitted to an acid decomposition process for determination of total chromium and later conditions of extraction and determination of Cr(VI). For the initial optimizations of this work, the EPA 3060A Method was used as a reference and adaptations were made. This method consists of alkaline extraction (pH 11,5), using a solution of 0.28 mol L-1 Na2CO3 with 0.5 mol L-1 NaOH and heating at 90-95 ºC for 60 min. Speciation analysis was performed using the LC-ICP-MS technique, where liquid chromatography conditions were evaluated, such as the type of separation column, type and concentration of the mobile phase and flow rate. The dionex AG7 column and pre-column C18, the mobile phase 15 mmol L-1 HNO3 at a flow rate of 0.5 mL min-1 were optimized as the best conditions. For the validation of this methodology, some figures of merit were evaluated, such as linearity, limit of detection (LOD), limit of quantification (LOQ), precision (repeatability and intra-laboratory reproducibility), robustness and accuracy. The sample preparation conditions for the determination of Cr(VI) were also evaluated using 0.28 mol L-1 Na2CO3 with 0.5 mol L-1 NaOH, 0.02 mmol L-1 diphenylcarbazide with 2.4 mmol L-1 EDTA, 50 mmol L-1 EDTA and H2O as extracting solvents. The best extraction condition for Cr(VI) was 0.28 mol L-1 Na2CO3 with 0.5 mol L-1 NaOH, using 10 mL and 20 mg of sample. Concentrations of 0.14 mol L-1 Na2CO3 + 0.25 mol L-1 NaOH and 0.07 mol L-1 Na2CO3 + 0.125 mol L-1 NaOH were evaluated to avoid interference and possible damage to the chromatographic column. 0.07 mol L-1 Na2CO3 + 0.125 mol L-1 NaOH was the best condition, since there was no significant change between the different extractor solvent concentrations, making it suitable for use in the extraction of the other evaluations. As a comparative method, the same extracts were analyzed by ion chromatography-visible spectrophotometry (IC-Vis), for the determination of Cr(VI) based on the official EPA 218.7 method, in which a good agreement was obtained between the two techniques. |
publishDate |
2022 |
dc.date.issued.fl_str_mv |
2022-10-28 |
dc.date.accessioned.fl_str_mv |
2023-01-11T14:38:00Z |
dc.date.available.fl_str_mv |
2023-01-11T14:38:00Z |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/doctoralThesis |
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doctoralThesis |
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publishedVersion |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/27560 |
url |
http://repositorio.ufsm.br/handle/1/27560 |
dc.language.iso.fl_str_mv |
por |
language |
por |
dc.relation.cnpq.fl_str_mv |
100600000000 |
dc.relation.confidence.fl_str_mv |
600 600 600 600 600 600 600 |
dc.relation.authority.fl_str_mv |
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dc.rights.driver.fl_str_mv |
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/ |
eu_rights_str_mv |
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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