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Doctoral Thesis
DOI
https://doi.org/10.11606/T.46.2005.tde-28022007-091600
Document
Author
Full name
José Carlos Pires Penteado
E-mail
Institute/School/College
Knowledge Area
Date of Defense
Published
São Paulo, 2005
Supervisor
Committee
Carvalho, Lilian Rothchild Franco de (President)
Augusto, Fábio
Freire, Renato Sanches
Massaro, Sergio
Poppi, Ronei Jesus
Title in Portuguese
Desenvolvimento e aplicação do método analítico para determinação de LABs em detergentes por SPME-GC/MS
Keywords in Portuguese
Análise univariada
Detergente
LAS
Quimiometria
Abstract in Portuguese
O alquil benzeno sulfonato linear (LAS) é o principal tensoativo aniônico, largamente utilizado em detergentes. O alquil benzeno linear (LAB), um subproduto, faz uma associação ao tensoativo devido a sulfonação incompleto do LAS. Recentemente tem tido grande interesse de usá-lo como marcador de efluente doméstico no ambiente aquático. Neste estudo, um novo método para determinação de LAB em detergentes envolvendo cromatografia a gás acoplado a espectrometria de massa em combinação com microextração em fase sólida (SPME) é proposto. O planejamento fatorial foi utilizado para obter valores ótimos para os principais parâmetros de análises de LAB em detergentes usando SPME direto como etapa de pré-concentração. SPME-GC/MS combinada com análise de componentes principais (PCA) e empregada para avaliar os parâmetros que afetam a SPME. O método otimizado foi aplicado nas amostras de detergentes comerciais (0,97 a 3,67 mg.g-1 LAB totais) e LAS (24,7 mg.g-1 LAB totais). Um perfil similar foi encontrado entre as amostras de detergentes e o LAS indicando que os tensoativos são idênticos. E algumas amostras, os LAB não foram encontrados (limite de detecção < 0,2 µg.mL-1).
Title in English
Development and application method for determination of LAB in detergents by SPME-GC/MS
Keywords in English
Chemometrics
Detergents
LAS
Univariable analysis
Abstract in English
Linear Alkylbenzene Sulfonated (LAS) is the main anionic surfactant, wide used in detergents. The Linear Alkylbenzene (LAB), a by-product, makes association with the surfactant, due the incomplete sulfonation of the LAS. Recently there has been widespread interest in their use as markers tracers of domestic waste in the aquatic environment. In this study, a new method for determination of LAB in detergents involving gas chromatography coupled to mass spectrometry (GC-MS) in combination with Solid Phase Microextraction (SPME) is proposed. A factorial design was utilized to obtain the optimum values for the main operation parameters in the analysis of LAB in detergents using direct SPME in the pre-concentration step. SPME-GC/MS in combination whit principal component analysis (PCA) was employed to evaluate the parameters that affect on SPME. The optimized method was applied to commercial detergents (0.97 and 3.67 mg.g-1 of total LAB) and LAS ( 24.47 mg.g-1 of total LAB) samples. Similar profiles of LAB congeners were found for the detergents and LAS samples indicating that identical surfactants. In some samples, LAB were not found (limit of detection < 0.2 mg.mL-1).
 
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TeseJosePenteado.pdf (517.38 Kbytes)
Publishing Date
2007-03-13
 
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