ASTM D6584-10a
(Test Method)Standard Test Method for Determination of Total Monoglyceride, Total Diglyceride, Total Triglyceride, and Free and Total Glycerin in B-100 Biodiesel Methyl Esters by Gas Chromatography
Standard Test Method for Determination of Total Monoglyceride, Total Diglyceride, Total Triglyceride, and Free and Total Glycerin in B-100 Biodiesel Methyl Esters by Gas Chromatography
SIGNIFICANCE AND USE
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 monoglycerides, total diglycerides, total triglycerides, and free and total glycerin in B-100 methyl esters by gas chromatography. The range of detection for free glycerin is 0.005 to 0.05 mass %, and total glycerin from 0.05 to 0.5 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.
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Designation: D6584 – 10a
Standard Test Method for
Determination of Total Monoglycerides, Total Diglycerides,
Total Triglycerides, and Free and Total Glycerin in B-100
1
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. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope* 3.1.2 bonded glycerin, n—glycerin portion of the mono-,
di-, and triglyceride molecules.
1.1 This test method covers the quantitative determination
3.1.3 total glycerin, n—sum of free and bonded glycerin.
of total monoglycerides, total diglycerides, total triglycerides,
3.2 This test method makes reference to many common gas
and free and total glycerin in B-100 methyl esters by gas
chromatographicprocedures,terms,andrelationships.Detailed
chromatography. The range of detection for free glycerin is
definitions can be found in Practices E355 and E594.
0.005 to 0.05 mass %, and total glycerin from 0.05 to 0.5 mass
%. This procedure is not applicable to vegetable oil methyl
4. Summary of Test Method
esters obtained from lauric oils, such as coconut oil and palm
4.1 The sample is analyzed by gas chromatography, after
kernel oil.
silyating with N-methyl-N-trimethylsilyltrifluoracetamide
1.2 The values stated in SI units are to be regarded as
(MSTFA). Calibration is achieved by the use of two internal
standard. No other units of measurement are included in this
standards and four reference materials. Mono-, di-, and trig-
standard.
lycerides are determined by comparing to monoolein, diolein,
1.3 This standard does not purport to address all of the
and triolein standards respectively.Average conversion factors
safety concerns, if any, associated with its use. It is the
are applied to the mono-, di-, and triglycerides to calculate the
responsibility of the user of this standard to establish appro-
bonded glycerin content of the sample.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
5. Significance and Use
5.1 Free and bonded glycerin content reflects the quality of
2. Referenced Documents
2 biodiesel. A high content of free glycerin may cause problems
2.1 ASTM Standards:
during storage, or in the fuel system, due to separation of the
D4307 Practice for Preparation of Liquid Blends for Use as
glycerin. A high total glycerin content can lead to injector
Analytical Standards
fouling and may also contribute to the formation of deposits at
E355 Practice for Gas Chromatography Terms and Rela-
injection nozzles, pistons, and valves.
tionships
E594 Practice for Testing Flame Ionization Detectors Used
6. Apparatus
in Gas or Supercritical Fluid Chromatography
6.1 Chromatographic System—See Practice E355 for spe-
cific designations and definitions.
3. Terminology
6.1.1 Gas Chromatograph (GC)—The system must be ca-
3.1 Definitions:
pable of operating at the conditions given in Table 1.
3.1.1 biodiesel (B-100), n—fuel comprised of mono-alkyl
6.1.2 Column, open tubular column with a 5 % phenylpoly-
esters of long chain fatty acids derived from vegetable oils or
dimethylsiloxane bonded and cross linked phase internal coat-
animal fats.
ing. The column should have an upper temperature limit of at
least 400°C. Columns, either 10 m or 15 m in length, with a
1
This test method is under the jurisdiction of ASTM CommitteeD02 on
0.32 mm internal diameter, and a 0.1 µm film thickness have
Petroleum Products and Lubricants and is the direct responsibility of D02.04.0L on
been found satisfactory. Any column with better or equivalent
Gas Chromatography Methods.
chromatographic efficiency and selectivity can be used. It is
Current edition approved Nov. 1, 2010. Published January 2011. Originally
approved in 2000. Last previous edition approved in 2010 as D6584–10a. DOI: recommended thata2to5 metre 0.53 mm high temperature
10.1520/D6584-10A.
guard column be installed from the injector to the analytical
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
column.This allows the use of autoinjectors and also increases
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
column life.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
*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.
1
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D6584 – 10a
TABLE 1 Operating Conditions TABLE 2 Stock Solutions
Injector Approximate Volumetric
Coo
...
This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation:D6584–10 Designation: D6584 – 10a
Standard Test Method for
Determination of Total Monoglycerides, Total Diglycerides,
Total Triglycerides, and Free and Total Glycerin in B-100
1
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. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope*
1.1This 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 0.100 to 1.000
mass %, for diglyceride is 0.050 to 0.500 mass %, and for triglyceride is 0.050 to 0.500 mass %. The range of quantitation for
free glycerin is 0.005 to 0.05 mass % and for total glycerin from 0.05 to 0.5 mass %.This procedure is not applicable to vegetable
oil methyl esters obtained from lauric oils, such as coconut oil and palm kernel oil.
1.1 This test method covers the quantitative determination of total monoglycerides, total diglycerides, total triglycerides, and
freeandtotalglycerininB-100methylestersbygaschromatography.Therangeofdetectionforfreeglycerinis0.005to0.05mass
%, and total glycerin from 0.05 to 0.5 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.
2. Referenced Documents
2
2.1 ASTM Standards:
D4307 Practice for Preparation of Liquid Blends for Use as Analytical Standards
E355 Practice for Gas Chromatography Terms and Relationships
E594 Practice for Testing Flame Ionization Detectors Used in Gas or Supercritical Fluid Chromatography
3. Terminology
3.1 Definitions:
3.1.1 biodiesel (B-100), n—fuel comprised of mono-alkyl esters of long chain fatty acids derived from vegetable oils or animal
fats.
3.1.2 bonded glycerin, n—glycerin portion of the mono-, di-, and triglyceride molecules.
3.2Definitions of Terms Specific to This Standard:
3.2.1
3.1.3 total glycerin, n—sum of free and bonded glycerin.
3.3This3.2 This test method makes reference to many common gas chromatographic procedures, terms, and relationships.
Detailed definitions can be found in Practices E355 and E594.
4. Summary of Test Method
4.1 The sample is analyzed by gas chromatography, after silyating with N-methyl-N-trimethylsilyltrifluoracetamide (MSTFA).
Calibration is achieved by the use of two internal standards and four reference materials. Mono-, di-, and triglycerides are
determined by comparing to monoolein, diolein, and triolein standards respectively.Average conversion factors are applied to the
mono-, di-, and triglycerides to calculate the bonded glycerin content of the sample.
1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of D02.04.0L on Gas
Chromatography Methods.
Current edition approved Aug.Nov. 1, 2010. Published August 2010.January 2011. Originally approved in 2000. Last previous edition approved in 20082010 as
D6584–08.D6584–10a. DOI: 10.1520/D6584-10A.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
*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.
1
---------------------- Page: 1 ----------------------
D6584 – 10a
5. Significance and Use
5.1 Freeandbondedglycerincontentreflectsthequalityofbiodiesel.Ahighcontentoffreeglycerinmaycauseproblemsduring
storage, or in the fuel system, due to separation of the glycerin.Ahigh total glycerin content can lead to injector fouling and may
also contribute to the formation of deposits at injection
...
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