SIMULTANEOUS DETERMINATION OF FREE AND TOTAL GLYCEROL, MONO-, DI- AND TRIGLYCERIDES IN ETHYLIC BIODIESEL OF SUNFLOWER, CASTOR OIL AND TALLOW/SOYBEAN MIXTURE USING GC-FID / DETERMINAÇÃO SIMULTÂNEA DE GLICEROL LIVRE E TOTAL, MONO-, DI- E TRIGLICERÍDEOS EM BIODIESEL ETÍLICO DE GIRASSOL, MAMONA E DA MISTURA DE SEBO E SOJA EMPREGANDO GC-FID

AUTOR(ES)
DATA DE PUBLICAÇÃO

2010

RESUMO

The biodiesel produced to be marketed in Brazil should be according to the quality standards established by the Resolution of February 4, 2010 of the Agência Nacional do Petróleo, Gás Natural e do Biocombustível (ANP, 04/2010). In this work, the application of the methods ASTM D 6584 e EN 14105 for castor oil biodiesel and biodiesel from ethylic routes was studied. Both the methods use Gas Chromatography with Flame Ionization Detection and silylation reaction with N-Methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA). The compounds were identified by the retention times, and for di- and triglycerides were used bands of retention time. The validation parameters were: analytical curve, linearity, sensibility, robustness, precision and accuracy. The methods ASTM D 6584 e EN 14105 showed similar sensitivity for all the compounds. The chromatographic conditions established by the method ASTM D 6584 were chosen because it is faster than the method EN14105. The method presented good linearity with r greater than 0,999 for all analytical curves. The silylation reaction was optimized for the ethylic castor biodiesel because of its different chemical composition. A volume of 500 μL of MSTFA was chosen for the realization of the precision and accuracy assays. The accuracy values were between 67.0 and 145.9% with precision values lower than 11%. The matrix effect occurrence for ethylic castor oil biodiesel was evaluated. The effect was considered low for glycerol, mono- and diolein and it was considered media for triolein. But, the analytical curves were prepared in solvent even though the matrix effect. The method was robust regarding variations of the matrix chemical composition. In the application of the method, this proved to be suitable to the samples of ethylic biodiesel of castor oil, sunflower and tallow/soybean mixture.

ASSUNTO(S)

glicerol tallow/soybean glycerol girassol glicerídeos glycerides gc-fid sebo e soja ethylic biodiesel mamona castor oil gc-fid quimica analitica biodiesel etílico sunflower

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