Infrared Spectroscopy of FAME in Biodiesel Following DIN 14078

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Application Note Infrared Spectroscopy of FAME in Biodiesel following DIN 14078 Quantification of Ester –FAME- in Biodiesel Blends European agriculture produces a lot of plants containing oil which will be used for commercial purposes. For the food market the rape seed oil is used as salad oil or as main part of margarine. Actual the rapeseed oil is also a discussion point for the biodiesel aspects. The quality of such biofuel and the blends of it are controlled by the Biodiesel regulation. One
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   Application Note Infrared Spectroscopy of FAME inBiodiesel following DIN 14078 Quantification of Ester –FAME- in Biodiesel Blends European agriculture produces a lot of plantscontaining oil which will be used for commercial purposes. For the food marketthe rape seed oil is used as salad oil or asmain part of margarine. Actual the rapeseed oil is also a discussionpoint for the biodiesel aspects.The quality of such biofuel and the blends of it are controlled by the Biodiesel regulation.One aspect of the control is the FAME (Fattyacid methyl ester) contents.Fig. 1: Transesterification of tri-glycerides toFAMEBiodiesel like rape seed oil is rich on fatmolecules which are treated in atransesterification process to contain a varietyof esters. The tranesterification is necessarybecause motors cannot run with the naturalrape seed oil which is too viscose.In the figure1 the chemical treatment isshown in a short graph. The huge molecule of a tri-glycerol is cracked into the glycerinemolecule and diverse FAME.The blends of the biofuel are important to becontrolled. This is possible with infraredspectroscopy. The reason is the simpleidentification of the mixtures. In the figure 2the infrared spectrum of a mineral oil and abiodiesel are presented. The most importantsignal the ester related carbonyl bond atapprox. 1745cm -1 is quantified in the manner to classify the blend of mineral oil andbiodiesel. This part is regulated by the DINEN 14078 norm. 5007501000125015001750200025003000350040004500 1/cm00.10.20.3 AbsRapeseed biodiesel5007501000125015001750200025003000350040004500 1/cm00.10.20.3 AbsMineraloil source unknown  Fig. 2: Comparsion of Biodiesel and mineraloil – significant difference is to see in theester signal at 1750cm -1   Content of DIN EN 14078 The ester -CO signal is target of DIN EN14078 from March 2004 and has the title“Liquid petroleum products -Determination of fatty acid methyl esters (FAME) in middledistillates- infrared spectroscopy method” ã The norm will focus on themeasurement range of 1670 to1820cm -1 and the signal of interest isat about 1745cm -1 . ã A cell with a thickness of 0.5mm andwindows prepared from KBr, NaCl or CaF 2 should be used. ã For dilution and cleaning the solventcyclohexane is to use. ã A calibration is to establish with1,2,4,6 and 10g/l of FAME incyclohexane Sample preparation In this application a KBr flow cell from Specacwas used. The sample thickness was -asdefined from DIN EN 14078- 0.5 mm in SCA_110_036 www.shimadzu.de  length. As recommended from the norm 6standards were prepared and measured. Themeasurement was done in the way thatcyclohexane was used as reference andagainst this reference the sample wasmeasured. For analysis only the part of thecarbonyl bond was used for the calibration(Fig. 3). _____________________________________________________________________________ 1680169517101725174017551770178518001815 1/cm00.20.40.60.81 Abs1,4 g/l = 1,6 % (V/V) FAME   Shimadzu Europa GmbH www.shimadzu.deEuropean Headquarters Albert-Hahn-Str.6-10, 47269 Duisburg Fig. 3: Infrared spectrum of ester signal of 6standard blends in the range of 1 to 11%V/VTable 1: Standard tableNo. Weight[g/L]Volume[%V/V]Unit[Abs]1 1.4 1.6 0.1542 2.3 2.6 0.2563 3.96 4.5 0.4394 6.4 7.3 0.7025 7.9 9.0 0.8766 9.7 11 1.071Density of FAME d=880 kg/m 3  The correlation coefficient is calculated tor2=0.999954. The result fulfilled the normwhich requested a value higher 0.99.One sample was checked against thecalibration. The sample was declared with5.26%V/V and the calibration found5.37%V/V. Procedure: The solutions prepared from cyclohexanewere transferred into the sample cell (3 times).Each time before sample was used thesolvent was send through the system for rinsing and cleaning (3 times). The control of the baseline showed that no contamination of the cell was visible. Instrumentation: IRPrestige-21 with IRsolution SoftwareCell Specac, KBr-window, 0.5mm pathlengthSample preparation time: 5min incl. rinse timesMeasurement technique: Transmission  
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