ASTM D6584-08
(Test Method)Standard Test Method for Determination of Free and Total Glycerin in B-100 Biodiesel Methyl Esters By Gas Chromatography
Standard Test Method for Determination of 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 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:D6584–08
Standard Test Method for
Determination of Free and Total Glycerin in B-100 Biodiesel
1
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. Terminology
1.1 This test method covers the quantitative determination 3.1 Definitions:
of free and total glycerin in B-100 methyl esters by gas 3.1.1 biodiesel (B-100), n—fuel comprised of mono-alkyl
chromatography. The range of detection for free glycerin is esters of long chain fatty acids derived from vegetable oils or
0.005 to 0.05 mass %, and total glycerin from 0.05 to 0.5 mass animal fats.
%. This procedure is not applicable to vegetable oil methyl 3.1.2 bonded glycerin, n—glycerin portion of the mono-,
esters obtained from lauric oils, such as coconut oil and palm di-, and triglyceride molecules.
kernel oil. 3.1.3 total glycerin, n—sum of free and bonded glycerin.
1.2 The values stated in SI units are to be regarded as 3.2 This test method makes reference to many common gas
standard. No other units of measurement are included in this chromatographicprocedures,terms,andrelationships.Detailed
standard. definitions can be found in Practices E355 and E594.
1.3 This standard does not purport to address all of the
4. Summary of Test Method
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 4.1 The sample is analyzed by gas chromatography, after
silyating with N-methyl-N-trimethylsilyltrifluoracetamide
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. (MSTFA). Calibration is achieved by the use of two internal
standards and four reference materials. Mono-, di-, and trig-
2. Referenced Documents
lycerides are determined by comparing to monoolein, diolein,
2
2.1 ASTM Standards: and triolein standards respectively.Average conversion factors
D4307 Practice for Preparation of Liquid Blends for Use as are applied to the mono-, di-, and triglycerides to calculate the
Analytical Standards bonded glycerin content of the sample.
E355 Practice for Gas Chromatography Terms and Rela-
5. Significance and Use
tionships
E594 Practice for Testing Flame Ionization Detectors Used 5.1 Free and bonded glycerin content reflects the quality of
biodiesel. A high content of free glycerin may cause problems
in Gas or Supercritical Fluid Chromatography
during storage, or in the fuel system, due to separation of the
glycerin. A high total glycerin content can lead to injector
1
This test method is under the jurisdiction of ASTM CommitteeD02 on
fouling and may also contribute to the formation of deposits at
Petroleum Products and Lubricants and is the direct responsibility of D02.04.0L on
injection nozzles, pistons, and valves.
Gas Chromatography Methods.
Current edition approved Oct. 15, 2008. Published November 2008. Originally
6. Apparatus
approved in 2000. Last previous edition approved in 2007 as D6584–07. DOI:
10.1520/D6584-08.
6.1 Chromatographic System—See Practice E355 for spe-
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
cific designations and definitions.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
6.1.1 Gas Chromatograph (GC)—The system must be ca-
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. pable of operating at the conditions given in Table 1.
*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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D6584–08
TABLE 2 Stock Solutions
6.1.2 Column, open tubular column with a 5 % phenylpoly-
dimethylsiloxane bonded and cross linked phase internal coat- Approximate Volumetric
Compound CAS No. Mass (mg) Flask Size
ing. The column should have an upper temperature limit of at
(mL)
least 400°C. Columns, either 10 m or 15 m in length, with a
Glycerin 56-81-5 25 50
0.32 mm internal diameter, and a 0.1 µm film thickness have
1-Mono [cis-9-octadecenoyl]-rac- 111-03-5 50 10
been found satisfactory. Any column with better or equivalent
glycerol (monoolein)
1,3-Di [cis-octadecenoyl]glycerol 2465-32-9 50 10
chromatographic efficiency and selectivity can be used. It is
(diolein)
recommended thata2to5 metre 0.53 mm high temperature
1,2,3-Tri [cis-octadecenoyl]glycerol 122-32-7 50 10
guard column be installed from the injector to the analytical
(triolein)
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM 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.
An American National Standard
Designation:D6584–07 Designation:D6584–08
Standard Test Method for
Determination of Free and Total Glycerin in B-100 Biodiesel
1
Methyl Esters Byby Gas Chromatography
This standard is issued under the fixed designation D 6584; 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*
1.1 This test method covers the quantitative determination of 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
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:
D 4307 Practice for Preparation of Liquid Blends for Use as Analytical Standards
E 355 Practice for Gas Chromatography Terms and Relationships
E 594 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—is the glycerin—glycerin portion of the mono-, di-, and triglyceride molecules.
3.1.3 total glycerin, n—is the sum of free and bonded glycerin. —sum of free and bonded glycerin.
3.2 This test method makes reference to many common gas chromatographic procedures, terms, and relationships. Detailed
definitions can be found in Practices E 355 and E 594.
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.
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 nozzles, pistons, and valves.
6. Apparatus
6.1 Chromatographic System—See Practice E 355 for specific designations and definitions.
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.
´1
Current edition approved Jan. 1, 2007. Published February 2007. Originally approved in 2000. Last previous edition approved in 2000 as D6584–00 .
Current edition approved Oct. 15, 2008. Published November 2008. Originally approved in 2000. Last previous edition approved in 2007 as D 6584–07.
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 ----------------------
D6584–08
6.1.1 Gas Chromatograph (GC)—The system must be capable of operating at the conditions given in Table 1.
6.1.2 Column,opentubularcolumnwitha5 %phenylpolydimethylsiloxanebondedandcrosslinkedphaseinternalcoating.The
column should have an upper temperature limit of at least 400°C. Columns, either 10 m or 15 m in length, with a 0.32 mm internal
diameter, and a 0.1 µm film thickness have been found satisfactory. Any column with better or equivalent chroma
...
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