ASTM D6584-17

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 % by mass, for diglyceride is 0.092353 % to 0.54475 % by mass, and for triglyceride is 0.00092857 % to 1.3881 % by mass. The range of quantitation for free glycerin is 0.0005714 % to 0.019533 % by mass and for total glycerin from 0.0090714 % to 0.42767 % by 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.  
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

• Status: Historical
• Publication Date: 31-May-2017
• ICS: 75.160.20 - Liquid fuels
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.04.0L - Gas Chromatography Methods

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D6584 − 17
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.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope* E355PracticeforGasChromatographyTermsandRelation-
ships
1.1 This test method covers the quantitative determination
E594Practice for Testing Flame Ionization Detectors Used
oftotalmonoglyceride,totaldiglyceride,totaltriglyceride,and
in Gas or Supercritical Fluid Chromatography
free and total glycerin in B-100 methyl esters by gas chroma-
tography. The range of quantitation for monoglyceride is
3. Terminology
0.009% to 0.77860% by mass, for diglyceride is 0.092353 %
3.1 Definitions:
to 0.54475% by mass, and for triglyceride is 0.00092857% to
3.1.1 biodiesel (B-100), n—fuel comprised of mono-alkyl
1.3881% by mass. The range of quantitation for free glycerin
esters of long chain fatty acids derived from vegetable oils or
is 0.0005714% to 0.019533% by mass and for total glycerin
animal fats.
from 0.0090714% to 0.42767% by mass. This procedure is
3.1.2 bonded glycerin, n—glycerin portion of the mono-,
not applicable to vegetable oil methyl esters obtained from
di-, and triglyceride molecules.
lauric oils, such as coconut oil and palm kernel oil.
3.2 Definitions of Terms Specific to This Standard:
1.2 The values stated in SI units are to be regarded as
3.2.1 total glycerin, n—sum of free and bonded glycerin.
standard. No other units of measurement are included in this
standard.
3.3 This test method makes reference to many common gas
chromatographicprocedures,terms,andrelationships.Detailed
1.3 This standard does not purport to address all of the
definitions can be found in Practices E355 and E594.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Summary of Test Method
priate safety and health practices and determine the applica-
4.1 The sample is analyzed by gas chromatography, after
bility of regulatory limitations prior to use.
silyating with N-methyl-N-trimethylsilyltrifluoracetamide
1.4 This international standard was developed in accor-
(MSTFA). Calibration is achieved by the use of two internal
dance with internationally recognized principles on standard-
standardsandfourreferencematerials.Mono-,di-,andtriglyc-
ization established in the Decision on Principles for the
eride are determined by comparing to monoolein, diolein, and
Development of International Standards, Guides and Recom-
triolein standards respectively. Average conversion factors are
mendations issued by the World Trade Organization Technical
appliedtomono-,di-,andtriglyceridestocalculatethebonded
Barriers to Trade (TBT) Committee.
glycerin content of the sample.
2. Referenced Documents
5. Significance and Use
2
2.1 ASTM Standards:
5.1 Free and bonded glycerin content reflects the quality of
D4307Practice for Preparation of Liquid Blends for Use as
biodiesel.Ahigh content of free glycerin may cause problems
Analytical Standards
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 Committee D02 on
fouling and may also contribute to the formation of deposits at
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
injection nozzles, pistons, and valves.
D02.04.0L on Gas Chromatography Methods.
CurrenteditionapprovedJune1,2017.PublishedJuly2017.Originallyapproved
6. Apparatus
ε1
in 2000. Last previous edition approved in 2013 as D6584–13 . DOI: 10.1520/
D6584-17.
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 [e-mail]. 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
1

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D6584 − 17
TABLE 1 Operating Conditions TABLE 2 Stock Solutions
Injector Approximate Volumetric
Cool on column injection Compound CAS No. Mass (mg) Flask Size
Sampl
...

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.
´1
Designation: D6584 − 13 D6584 − 17
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
ε NOTE—The formats of Eq 11 and Eq 16 were editorially corrected in April 2014.
1. 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 %,0.009 % to 0.77860 % by mass, for diglyceride is 0.092353 to 0.54475 mass %,% to 0.54475 % by mass, and for
triglyceride is 0.00092857 to 1.3881 mass %.0.00092857 % to 1.3881 % by mass. The range of quantitation for free glycerin is
0.00057140.0005714 % to 0.019533 0.019533 % by mass % and for total glycerin from 0.0090714 to 0.42767 mass
%.0.0090714 % to 0.42767 % by 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.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
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.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 total glycerin, n—sum of free and bonded glycerin.
3.3 This test method makes reference to many common gas chromatographic procedures, terms, and relationships. Detailed
definitions can be found in Practices E355 and E594.
1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of D02.04.0L
on Gas Chromatography Methods.
Current edition approved May 1, 2013June 1, 2017. Published May 2013July 2017. Originally approved in 2000. Last previous edition approved in 20102013 as
ε1
D6584D6584 – 13–10a . DOI: 10.1520/D6584-13E01.10.1520/D6584-17.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. 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 − 17
TABLE 1 Operating Conditions
Injector
Cool on column injection
Sample size 1 μL
Column Temperature Program
Initial temperature 50°C hold 1 min
Initial temperature 50 °C hold 1 min
Rate 1 15°C / min to 180°C
Rate 1 15 °C / min to 180 °C
Rate 2 7°C / min to 230°C
Rate 2 7 °C / min to 230 °C
Rate 3 30°C / min 380°C hold 10 min
Rate 3 30 °C / min 380 °C hold 10 min
Defector
Type Flame ionization
Temperature 380°C
Temperature 380 °C
Carrier Gas
Type Hydrogen or helium measured at 50°C
Type Hydrogen or helium measured at
50 °C
Flow rate 3 mL/min
4. Summary of Test Method
4.1 The sample is analyzed by gas chromatography, after
...