ASTM D6584-13
(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
Buy Standard
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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 − 13
StandardTest 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* 3.1.1 biodiesel (B-100), n—fuel comprised of mono-alkyl
esters of long chain fatty acids derived from vegetable oils or
1.1 This test method covers the quantitative determination
animal fats.
oftotalmonoglyceride,totaldiglyceride,totaltriglyceride,and
3.1.2 bonded glycerin, n—glycerin portion of the mono-,
free and total glycerin in B-100 methyl esters by gas chroma-
tography.Therangeofquantitationformonoglycerideis0.009 di-, and triglyceride molecules.
to 0.77860 mass %, for diglyceride is 0.092353 to 0.54475
3.2 Definitions of Terms Specific to This Standard:
mass %, and for triglyceride is 0.00092857 to 1.3881 mass %.
3.2.1 total glycerin, n—sum of free and bonded glycerin.
The range of quantitation for free glycerin is 0.0005714 to
3.3 This test method makes reference to many common gas
0.019533 mass % and for total glycerin from 0.0090714 to
chromatographicprocedures,terms,andrelationships.Detailed
0.42767 mass %.This procedure is not applicable to vegetable
definitions can be found in Practices E355 and E594.
oil methyl esters obtained from lauric oils, such as coconut oil
and palm kernel oil.
4. Summary of Test Method
1.2 The values stated in SI units are to be regarded as
4.1 The sample is analyzed by gas chromatography, after
standard. No other units of measurement are included in this
silyating with N-methyl-N-trimethylsilyltrifluoracetamide
standard.
(MSTFA). Calibration is achieved by the use of two internal
1.3 This standard does not purport to address all of the
standardsandfourreferencematerials.Mono-,di-,andtriglyc-
safety concerns, if any, associated with its use. It is the
eride are determined by comparing to monoolein, diolein, and
responsibility of the user of this standard to establish appro-
triolein standards respectively. Average conversion factors are
priate safety and health practices and determine the applica-
appliedtomono-,di-,andtriglyceridestocalculatethebonded
bility of regulatory limitations prior to use.
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
E355PracticeforGasChromatographyTermsandRelation-
glycerin. A high total glycerin content can lead to injector
ships
fouling and may also contribute to the formation of deposits at
E594Practice for Testing Flame Ionization Detectors Used
injection nozzles, pistons, and valves.
in Gas or Supercritical Fluid Chromatography
3. Terminology 6. Apparatus
3.1 Definitions:
6.1 Chromatographic System—See Practice E355 for spe-
cific designations and definitions.
1
This test method is under the jurisdiction of ASTM Committee D02 on
6.1.1 Gas Chromatograph (GC)—The system must be ca-
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
pable of operating at the conditions given in Table 1.
D02.04.0L on Gas Chromatography Methods.
6.1.2 Column, open tubular column with a 5% phenylpo-
Current edition approved May 1, 2013. Published May 2013. Originally
ε1
lydimethylsiloxane bonded and cross linked phase internal
approved in 2000. Last previous edition approved in 2010 as D6584–10a . DOI:
10.1520/D6584-13.
coating.Thecolumnshouldhaveanuppertemperaturelimitof
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
at least 400°C. Columns, either 10 m or 15 m in length, with a
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
0.32 mm internal diameter, and a 0.1 µm film thickness have
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. been found satisfactory.Any column with better or equivalent
*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 − 13
TABLE 1 Operating Conditions TABLE 2 Stock Solutions
Injector Approximate Volumetric
Cool on column injection Compound CAS No. Mass (mg) Flask Size
Samp
...
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 − 10a D6584 − 13
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—Corrected formatting and spacing in Eqs 12-19 and added previous Summary of Changes editorially in March
2011.
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 0.1000.009 to
1.0000.77860 mass %, for diglyceride is 0.0500.092353 to 0.5000.54475 mass %, and for triglyceride is 0.0500.00092857 to
0.5001.3881 mass %. The range of quantitation for free glycerin is 0.0050.0005714 to 0.050.019533 mass % and for total glycerin
from 0.050.0090714 to 0.50.42767 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.
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.
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 triglyceride are
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 Nov. 1, 2010May 1, 2013. Published January 2011May 2013. Originally approved in 2000. Last previous edition approved in 2010 as
ε1
D6584–10.–10a . DOI: 10.1520/D6584-10A.10.1520/D6584-13.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM 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 − 13
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
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
determined by comparing to monoolein, diolein, and tri
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.