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ASTM D6584 - 13 Standard Test Method for Determination of Total Monoglycerides, TotalDiglycerides, Total Triglycerides, and Free and Total Glycerin in B-100 Biodiesel Methyl Estersby Gas ChromatographyInstrument: Perkin Elmer Clarus 500 GC with FID and AutoSamplerSignificance and Use5.1 Free and bonded glycerin content reflects the quality of biodiesel. A high content of free glycerinmay cause problems during storage, or in the fuel system, due to separation of the glycerin. A high totalglycerin content can lead to injector fouling and may also contribute to the formation of deposits atinjection nozzles, pistons, and valves.1. Scope1.1 This test method covers the quantitative determination of total monoglyceride, total diglyceride,total triglyceride, and free and total glycerin in B-100 methyl esters by gas chromatography. The rangeof quantitation for monoglyceride is 0.009 to 0.77860 mass %, for diglyceride is 0.092353 to 0.54475mass %, and for triglyceride is 0.00092857 to 1.3881 mass %. The range of quantitation for free glycerinis 0.0005714 to 0.019533 mass % and for total glycerin from 0.0090714 to 0.42767 mass %. Thisprocedure is not applicable to vegetable oil methyl esters obtained from lauric oils, such as coconut oiland palm kernel oil.1.2 The values stated in SI units are to be regarded as standard. No other units of measurement areincluded in this standard.1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. Itis the responsibility of the user of this standard to establish appropriate safety and health practices anddetermine the applicability of regulatory limitations prior to use.2. Practical ApplicationInstrumentation: Perkin Elmer Clarus 500 GC with FID and AutoSamplerColumn: Elite-Biodiesel M, 14 m x 530 µm x 0.16 µm filmPre-Column: Built-in 2 m Integra-GapInjection Mode: On-columnInlet Program Initial Temperature: 60 CHold Time 1: 1.00 minRamp 1: 15 C/minInlet Program Intermediate Temperature: 300 CHold Time 2: 0.00 minRamp 2: 30 C/minInlet Program Final Temperature: 380 CColumn Flow: 3 mL/min
Injection volume: 1 µLCarrier Gas: HeliumOven Program Initial Temperature 1: 50 C, Hold Time 1.00 min, Ramp 15 C/minOven Program Temperature 2: 180 C, Hold Time 0.00 min, Ramp 7 C/minOven Program Temperature 3: 230 C, Hold Time 0.00 min, Ramp 10 C/minOven Program Temperature 4: 370 C, Hold Time 5.00 minEquilibration Time: 0.0 minFID temperature: 380 CH2 flow: 45 mL/minAir flow: 450 mL/minRange: 1Attenuation: -5Standard and Sample Preparation: The calibration and internal standards are prepared in pyridine,according to the EN and ASTM procedure. The derivatization procedure for both standards andsamples is identical. Weigh approximately 100 mg of sample or standard into a vial and record the actualweight. Internal standards are added according to the EN or ASTM specification, and 100 μL MSTFA(derivatization reagent) is finally added. The samples and standards are allowed to stand for 20 min atroom temperature to allow the derivatization reaction to complete. Following derivatization, heptane isadded and the vial is capped and shaken.Summary of Calibration Results for Free and Total Glycerol Following Both EN and ASTM Methodology.GlycerolTotal MonoglyceridesTotal DiglyceridesTotal TriglyceridesCalibration SummaryLinearity (R2)Linearity (R2)EN 14110ASTM D6584(4-Point Calibration)(5-Point 99850.9945
3. Referenced DocumentsASTM StandardsD4307 Practice for Preparation of Liquid Blends for Use as Analytical StandardsE355 Practice for Gas Chromatography Terms and RelationshipsE594 Practice for Testing Flame Ionization Detectors Used in Gas or Supercritical Fluid 4-74153APP GlycerinBiodiesel.pdf
according to the EN and ASTM procedure. The derivatization procedure for both standards and samples is identical. Weigh approximately 100 mg of sample or standard into a vial and record the actual weight. Internal standards are added according to the EN or ASTM specification, and 100 μL MSTFA (derivatization reagent) is finally added. The samples and standards are allowed to stand for 20 min atFile Size: 307KBPage Count: 5
