ASTM D6584-21

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, health, and environmental 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: Published
• Publication Date: 30-Nov-2021
• 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)

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.
Designation: D6584 − 21
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* D4307Practice for Preparation of Liquid Blends for Use as
Analytical Standards
1.1 This test method covers the quantitative determination
E355PracticeforGasChromatographyTermsandRelation-
oftotalmonoglyceride,totaldiglyceride,totaltriglyceride,and
ships
free and total glycerin in B-100 methyl esters by gas chroma-
E594Practice for Testing Flame Ionization Detectors Used
tography. The range of quantitation for monoglyceride is
in Gas or Supercritical Fluid Chromatography
0.009% to 0.77860% by mass, for diglyceride is 0.092353 %
to 0.54475% by mass, and for triglyceride is 0.00092857% to
3. Terminology
1.3881% by mass. The range of quantitation for free glycerin
is 0.0005714% to 0.019533% by mass and for total glycerin
3.1 Definitions:
from 0.0090714% to 0.42767% by mass. This procedure is
3.1.1 This test method makes reference to common
not applicable to vegetable oil methyl esters obtained from
procedures, terms, and relationships. Detailed definitions of
lauric oils, such as coconut oil and palm kernel oil.
these can be found in Practices E355 and E594, andTerminol-
1.2 The values stated in SI units are to be regarded as
ogy D4175. Several definitions for clarity are indicated below:
standard. No other units of measurement are included in this
3.1.2 biodiesel (B-100), n—fuel comprised of mono-alkyl
standard.
esters of long chain fatty acids derived from vegetable oils or
1.3 This standard does not purport to address all of the
animal fats.
safety concerns, if any, associated with its use. It is the
3.1.3 bonded glycerin, n—glycerin portion of the mono-,
responsibility of the user of this standard to establish appro-
di-, and triglyceride molecules.
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use. 3.2 Definitions of Terms Specific to This Standard:
1.4 This international standard was developed in accor-
3.2.1 total glycerin, n—sum of free and bonded glycerin.
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
4. Summary of Test Method
Development of International Standards, Guides and Recom-
4.1 The sample is analyzed by gas chromatography, after
mendations issued by the World Trade Organization Technical
silyating with N-methyl-N-trimethylsilyltrifluoracetamide
Barriers to Trade (TBT) Committee.
(MSTFA). Calibration is achieved by the use of two internal
2. Referenced Documents
standardsandfourreferencematerials.Mono-,di-,andtriglyc-
2
eride are determined by comparing to monoolein, diolein, and
2.1 ASTM Standards:
triolein standards respectively. Average conversion factors are
D4175Terminology Relating to Petroleum Products, Liquid
appliedtomono-,di-,andtriglyceridestocalculatethebonded
Fuels, and Lubricants
glycerin content of the sample.
1
This test method is under the jurisdiction of ASTM Committee D02 on
5. Significance and Use
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
D02.04.0L on Gas Chromatography Methods.
5.1 Free and bonded glycerin content reflects the quality of
Current edition approved Dec. 1, 2021. Published January 2022. Originally
biodiesel.Ahigh content of free glycerin may cause problems
approved in 2000. Last previous edition approved in 2017 as D6584–17. DOI:
10.1520/D6584-21.
during storage, or in the fuel system, due to separation of the
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
glycerin. A high total glycerin content can lead to injector
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
fouling and may also contribute to the formation of deposits at
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. injection nozzles, pistons, and valves.
*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 − 21
TABLE 1 Operating Conditions TABLE
...

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.
Designation: D6584 − 17 D6584 − 21
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*
1.1 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 safety, health, and healthenvironmental 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:
D4175 Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants
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 This test method makes reference to common procedures, terms, and relationships. Detailed definitions of these can be found
in Practices E355 and E594, and Terminology D4175. Several definitions for clarity are indicated below:
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 June 1, 2017Dec. 1, 2021. Published July 2017January 2022. Originally approved in 2000. Last previous edition approved in 20132017 as
ε1
D6584 – 13D6584 – 17. . DOI: 10.1520/D6584-17.10.1520/D6584-21.
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 − 21
TABLE 1 Operating Conditions
Injector
Cool on column injection
Sample size 1 μL
Column Temperature Program
Initial temperature 50 °C hold 1 min
Rate 1 15 °C / min to 180 °C
Rate 2 7 °C / min to 230 °C
Rate 3 30 °C / min 380 °C hold 10 min
Defector
Type Flame ionization
Temperature 380 °C
Carrier Gas
Type Hydrogen or helium measured at
50 °C
Flow rate 3 mL/min
3.1.2 biodiesel (B-100), n—fuel comprised of mono-alkyl esters of long chain fatty acids derived from vegetable oils or animal
fats.
3.1.3 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.
4. Summary of Test Method
4.1 The sample is analyzed by gas chromatography, after silyating with N-methyl-N-trimethylsilyltr
...