Desenvolvimento de metodologias eletroanalíticas para determinação de potássio e fósforo em biodiesel
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Data
2009-07-17
Autores
Castilho, Michelle de Souza [UNESP]
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Editor
Universidade Estadual Paulista (Unesp)
Resumo
Este trabalho descreve metodologias eletroanalíticas para determinação de potássio e fósforo em biodiesel de soja. O potássio existente no biodiesel é proveniente do catalisador (hidróxido de potássio) utilizado na reação de transesterificação. Apesar de ser muito importante na reação, resíduos de potássio no biodiesel podem causar problemas como a formação de partículas sólidas, entupimento dos injetores e corrosão do motor. O fósforo presente no biodiesel é proveniente dos fosfolipídios e sua presença no biodiesel causa danos à conversão catalítica e provoca um aumento na emissão de partículas. Para a determinação potenciométrica de potássio em biodiesel utilizou-se um eletrodo quimicamente modificado com hexacianoferrato de níquel. A curva analítica para a determinação de potássio mostrou um intervalo linear de concentração de 4,0 x 10-5 a 1,0 x 10-2 mol L-1, cujo coeficiente angular da reta é 55,2 mV e o limite de detecção igual a 1,9 x 10-5 mol L-1. Para a determinação de íons potássio em biodiesel, primeiramente realizou-se extração líquido – liquido com ácido clorídrico 0,10 mol L-1 e a determinação de potássio foi realizada no extrato aquoso, sendo que a concentração de potássio encontrada foi de 0,96 mg kg-1. O fósforo foi determinado em biodiesel por voltametria cíclica utilizando eletrodo de pasta de grafite quimicamente modificado com 12 molibdofosfato. O método apresentou um intervalo linear de concentração de 1,0 x 10-6 a 1,5 x 10-4 mol L-1 e um limite de detecção igual a 1,0 x 10-6 mol L-1. Os íons fosfato foram determinados em uma amostra real de biodiesel de soja, utilizando o eletrodo de pasta de grafite modificado com filme de 12 molibdofosfato e a concentração de fosfato encontrada foi igual a 1,0 x 10-5 mol L-1 com desvio padrão relativo de 5%. Nesse trabalho também foi estudado outro método...
This work describes an electroanalytical methodology to determine potassium and phosphorus in biodiesel of soy. The potassium existing in biodiesel is proceeding from the catalyst (potassium hydroxide) used in the transesterification reaction. Although the potassium is very important to the reaction, the presence of potassium’s residue in biodiesel can form deposits in fuel injection system components and corrosion of the engine. The phosphorus presents in biodiesel comes from phospholipids and it provokes damages the catalytic conversion and an increase in the emission of particles. For the potentiometric determination of potassium in biodiesel it was used a nickel hexacyanoferrate modified electrode. The analytical curve showed a linear response to potassium ions in the concentration range of 4,0 x 10−5 to 1,0 x 10−2 mol L−1, the average slope was 55,2 mV per decade and the limit detection was 1,9 x 10−5 mol L−1. The potassium ion was determined in biodiesel, but firstly, liquid–liquid extraction was done using hydrochloric acid 0,10 mol L-1 and the determination it was done in the aqueous extract and the concentration of potassium found was 0,96 mg kg-1. The phosphorus was determined in biodiesel using a 12 molybdophosphate modified carbon paste electrode by cyclic voltammetry. The method showed a linear response in the concentration range of 1,0 x 10-5 a 1,5 x 10-4 mol L-1 and limit of detection was 4,9 x 10-6 mol L-1. The phosphorus was determined biodiesel using the 12 molybdophosphate modified carbon paste electrode and the concentration found was 1,0 x 10-5 mol L-1 and the relative standard deviation was 5%. In this work it was studied nickel foil electrode modified with iron oxide nanoparticle to determine phosphorus. Although the phosphorus is adsorbed in iron oxide surface, others anions are adsorbed too and can interfering in the phosphorus analysis
This work describes an electroanalytical methodology to determine potassium and phosphorus in biodiesel of soy. The potassium existing in biodiesel is proceeding from the catalyst (potassium hydroxide) used in the transesterification reaction. Although the potassium is very important to the reaction, the presence of potassium’s residue in biodiesel can form deposits in fuel injection system components and corrosion of the engine. The phosphorus presents in biodiesel comes from phospholipids and it provokes damages the catalytic conversion and an increase in the emission of particles. For the potentiometric determination of potassium in biodiesel it was used a nickel hexacyanoferrate modified electrode. The analytical curve showed a linear response to potassium ions in the concentration range of 4,0 x 10−5 to 1,0 x 10−2 mol L−1, the average slope was 55,2 mV per decade and the limit detection was 1,9 x 10−5 mol L−1. The potassium ion was determined in biodiesel, but firstly, liquid–liquid extraction was done using hydrochloric acid 0,10 mol L-1 and the determination it was done in the aqueous extract and the concentration of potassium found was 0,96 mg kg-1. The phosphorus was determined in biodiesel using a 12 molybdophosphate modified carbon paste electrode by cyclic voltammetry. The method showed a linear response in the concentration range of 1,0 x 10-5 a 1,5 x 10-4 mol L-1 and limit of detection was 4,9 x 10-6 mol L-1. The phosphorus was determined biodiesel using the 12 molybdophosphate modified carbon paste electrode and the concentration found was 1,0 x 10-5 mol L-1 and the relative standard deviation was 5%. In this work it was studied nickel foil electrode modified with iron oxide nanoparticle to determine phosphorus. Although the phosphorus is adsorbed in iron oxide surface, others anions are adsorbed too and can interfering in the phosphorus analysis
Descrição
Palavras-chave
Eletroanalítica, Quimica analitica, Biodiesel, Potassio, Fósforo, Analytical chemistry
Como citar
CASTILHO, Michelle de Souza. Desenvolvimento de metodologias eletroanalíticas para determinação de potássio e fósforo em biodiesel. 2009. 113 f. Tese (doutorado) - Universidade Estadual Paulista, Instituto de Química, 2009.