title: Fast and simple method for determination of fatty acid methyl esters (FAME) in biodiesel blends using X-ray spectrometry.
abstract: The determination of fatty acid methyl esters (FAME) in diesel fuel blends is an important aspect of production and blending process as well as quality control of distribution operations. In this study, energy-dispersive X-ray fluorescence spectrometer (EDXRF) is used for the first time for determination of FAME in biodiesel blends. The principle of the method is based on intensity difference of X-ray radiation scattered from hydrocarbons and from FAME. The experiment shows that coherent and incoherent radiation, commonly applied for evaluation of the average atomic number of the sample with light matrix, cannot be applied for FAME determination. However, the application of scattered continuous radiation gives excellent correlation between FAME concentration and intensity of scattered radiation. The best results are obtained if continuum is collected in the range of energy between 10.5 and 15.0 keV for rhodium X-ray tube, operated at 35 kV. Linear relationship between the FAME concentration and the inverse of scattered continuous radiation is obtained with the correlation coefficients of 0.999. Standard deviation of measurement is ca. 0.46% (v/v) of FAME and detection limit is 1.2% (v/v) for 600 s counting time and 50% dead-time loss using Si-PIN detector. The investigation shows that crucial issue in determination of FAME in biodiesel blends using EDXRF spectrometer is the precision of measurements resulting from the counting statistics. Therefore, much better results (0.20% (v/v) standard deviation and 0.52% (v/v) detection limit) can be expected if higher intensity of primary radiation is applied and X-ray spectrum is collected by silicon drift detector of high input count rate. For concentration of FAME from 10 to 100% (v/v), the differences between reference method (Fourier transform infrared spectrometry) and the proposed method usually do not exceed 1% (v/v) of FAME. The proposed method is fast, simple and enables FAME determination in wide range of concentration up to 100% of FAME without any sample treatment.
authors.affiliation: Institute of Chemistry, University of Silesia, Szkolna 9, 40-006 Katowice, Poland. rafal.sitko@us.edu.pl
authors.forename: Rafal
authors.initials: R
authors.lastname: Sitko
authors.forename: Beata
authors.initials: B
authors.lastname: Zawisza
authors.forename: Zofia
authors.initials: Z
authors.lastname: Kowalewska
authors.forename: Karina
authors.initials: K
authors.lastname: Kocot
authors.forename: Marzena
authors.initials: M
authors.lastname: Polowniak
mesh_terms: D056804:Biofuels / Q000032:analysis*; D002138:Calibration; D004952:Esters; D005227:Fatty Acids / Q000032:analysis* / Q000737:chemistry*; D006838:Hydrocarbons / Q000737:chemistry; D057230:Limit of Detection; D012542:Scattering, Radiation; D013052:Spectrometry, X-Ray Emission / Q000379:methods*; D013997:Time Factors
chemical_list: D056804:Biofuels; D004952:Esters; D005227:Fatty Acids; D006838:Hydrocarbons