ASTM D6584-13e1
(Test Method)Standard Test Method for Determination of Total Monoglycerides, Total Diglycerides, Total Triglycerides, and Free and Total Glycerin in B-100 Biodiesel Methyl Esters by Gas Chromatography
Standard Test Method for Determination of Total Monoglycerides, Total Diglycerides, Total Triglycerides, and Free and Total Glycerin in B-100 Biodiesel Methyl Esters by Gas Chromatography
SIGNIFICANCE AND USE
5.1 Free and bonded glycerin content reflects the quality of biodiesel. A high content of free glycerin may cause problems during storage, or in the fuel system, due to separation of the glycerin. A high total glycerin content can lead to injector fouling and may also contribute to the formation of deposits at injection nozzles, pistons, and valves.
SCOPE
1.1 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 range of quantitation for monoglyceride is 0.009 to 0.77860 mass %, for diglyceride is 0.092353 to 0.54475 mass %, and for triglyceride is 0.00092857 to 1.3881 mass %. The range of quantitation for free glycerin is 0.0005714 to 0.019533 mass % and for total glycerin from 0.0090714 to 0.42767 mass %. This procedure is not applicable to vegetable oil methyl esters obtained from lauric oils, such as coconut oil and palm kernel oil.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
General Information
Relations
Standards Content (Sample)
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Designation: D6584 − 13
Standard Test Method for
Determination of Total Monoglycerides, Total Diglycerides,
Total Triglycerides, and Free and Total Glycerin in B-100
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Biodiesel Methyl Esters by Gas Chromatography
This standard is issued under the fixed designation D6584; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
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ε NOTE—The formats of Eq 11 and Eq 16 were editorially corrected in April 2014.
1. Scope* 3. Terminology
1.1 This test method covers the quantitative determination 3.1 Definitions:
oftotalmonoglyceride,totaldiglyceride,totaltriglyceride,and 3.1.1 biodiesel (B-100), n—fuel comprised of mono-alkyl
free and total glycerin in B-100 methyl esters by gas chroma- esters of long chain fatty acids derived from vegetable oils or
tography.Therangeofquantitationformonoglycerideis0.009 animal fats.
to 0.77860 mass %, for diglyceride is 0.092353 to 0.54475
3.1.2 bonded glycerin, n—glycerin portion of the mono-,
mass %, and for triglyceride is 0.00092857 to 1.3881 mass %.
di-, and triglyceride molecules.
The range of quantitation for free glycerin is 0.0005714 to
3.2 Definitions of Terms Specific to This Standard:
0.019533 mass % and for total glycerin from 0.0090714 to
3.2.1 total glycerin, n—sum of free and bonded glycerin.
0.42767 mass %.This procedure is not applicable to vegetable
3.3 This test method makes reference to many common gas
oil methyl esters obtained from lauric oils, such as coconut oil
and palm kernel oil. chromatographicprocedures,terms,andrelationships.Detailed
definitions can be found in Practices E355 and E594.
1.2 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
4. Summary of Test Method
standard.
4.1 The sample is analyzed by gas chromatography, after
1.3 This standard does not purport to address all of the
silyating with N-methyl-N-trimethylsilyltrifluoracetamide
safety concerns, if any, associated with its use. It is the
(MSTFA). Calibration is achieved by the use of two internal
responsibility of the user of this standard to establish appro-
standardsandfourreferencematerials.Mono-,di-,andtriglyc-
priate safety and health practices and determine the applica-
eride are determined by comparing to monoolein, diolein, and
bility of regulatory limitations prior to use.
triolein standards respectively. Average conversion factors are
appliedtomono-,di-,andtriglyceridestocalculatethebonded
2. Referenced Documents
glycerin content of the sample.
2
2.1 ASTM Standards:
D4307Practice for Preparation of Liquid Blends for Use as
5. Significance and Use
Analytical Standards
5.1 Free and bonded glycerin content reflects the quality of
E355PracticeforGasChromatographyTermsandRelation-
biodiesel.Ahigh content of free glycerin may cause problems
ships
during storage, or in the fuel system, due to separation of the
E594Practice for Testing Flame Ionization Detectors Used
glycerin. A high total glycerin content can lead to injector
in Gas or Supercritical Fluid Chromatography
fouling and may also contribute to the formation of deposits at
injection nozzles, pistons, and valves.
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This test method is under the jurisdiction of ASTM Committee D02 on
6. Apparatus
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
D02.04.0L on Gas Chromatography Methods.
6.1 Chromatographic System—See Practice E355 for spe-
Current edition approved May 1, 2013. Published May 2013. Originally
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cific designations and definitions.
approved in 2000. Last previous edition approved in 2010 as D6584–10a . DOI:
10.1520/D6584-13E01.
6.1.1 Gas Chromatograph (GC)—The system must be ca-
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
pable of operating at the conditions given in Table 1.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
6.1.2 Column, open tubular column with a 5% phenylpo-
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. lydimethylsiloxane bonded and cross linked phase internal
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D6584 − 13
TABLE 1 Operating Conditions TABLE 2 Stock Solutions
Injector Approximate Volumetric
Cool on column injection Compound CAS No. Mass (mg) Flask Size
Sample size 1 µL (mL)
Column Temperature Program Glycerin 56-81-5 25 50
Initial temperature 50°C hold 1 min 1-Mono [cis-9-octadecenoyl]-rac- 111-03-
...
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