ASTM D6584-07
(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 &solely-SI-units;
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
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Standards Content (Sample)
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An American National Standard
Designation:D6584–07
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 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope* 3.1.2 bonded glycerin, n—is the glycerin portion of the
mono-, di-, and triglyceride molecules.
1.1 This test method covers the quantitative determination
3.1.3 total glycerin, n—is the sum of free and bonded
of free and total glycerin in B-100 methyl esters by gas
glycerin.
chromatography. The range of detection for free glycerin is
3.2 This test method makes reference to many common gas
0.005 to 0.05 mass %, and total glycerin from 0.05 to 0.5 mass
chromatographicprocedures,terms,andrelationships.Detailed
%. This procedure is not applicable to vegetable oil methyl
definitions can be found in Practices E 355 and E 594.
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
standards and four reference materials. Mono-, di-, and trig-
safety concerns, if any, associated with its use. It is the
lycerides are determined by comparing to monoolein, diolein,
responsibility of the user of this standard to establish appro-
and triolein standards respectively.Average conversion factors
priate safety and health practices and determine the applica-
are applied to the mono-, di-, and triglycerides to calculate the
bility of regulatory limitations prior to use.
bonded 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
D 4307 Practice for Preparation of Liquid Blends for Use as
biodiesel. A high content of free glycerin may cause problems
Analytical Standards
during storage, or in the fuel system, due to separation of the
E 355 Practice for Gas Chromatography Terms and Rela-
glycerin. A high total glycerin content can lead to injector
tionships
fouling and may also contribute to the formation of deposits at
E 594 Practice for Testing Flame Ionization Detectors Used
injection nozzles, pistons, and valves.
in Gas or Supercritical Fluid Chromatography
6. Apparatus
3. Terminology
6.1 Chromatographic System—See Practice E 355 for spe-
3.1 Definitions:
cific designations and definitions.
3.1.1 biodiesel (B-100), n—fuel comprised of mono-alkyl
6.1.1 Gas Chromatograph (GC)—The system must be ca-
esters of long chain fatty acids derived from vegetable oils or
pable of operating at the conditions given in Table 1.
animal fats.
6.1.2 Column, open tubular column with a 5 % phenylpoly-
dimethylsiloxane bonded and cross linked phase internal coat-
1
This test method is under the jurisdiction of ASTM CommitteeD02 on
ing. The column should have an upper temperature limit of at
Petroleum Products and Lubricants and is the direct responsibility of D02.04.0L on
least 400°C. Columns, either 10 m or 15 m in length, with a
Gas Chromatography Methods.
0.32 mm internal diameter, and a 0.1 µm film thickness have
Current edition approved Jan. 1, 2007. Published February 2007. Originally
e1
approved in 2000. Last previous edition approved in 2000 as D 6584–00 .
been found satisfactory. Any column with better or equivalent
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
chromatographic efficiency and selectivity can be used. It is
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
recommended thata2to5 metre 0.53 mm high temperature
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.
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D6584–07
TABLE 1 Operating Conditions
check for leaks throughout the system. If leaks are found,
Injector tightenorreplacefittingsandrecheckforleaksbeforeproceed-
Cool on column injection
ing.
Sample size 1 µL
Column Temperature Program
9. Calibration and Standardization
Initial temperature 50°C hold 1 min
Rate 1 15°C / min to 180°C
9.1 Prepar
...
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