ASTM D6584-00e1

Standard Test Method for Determination of Free and Total Glycerin in B-100 Biodiesel Methyl Esters By Gas Chromatography

SCOPE
1.1 This test method provides for 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 palmkernel oil.
1.2 The values stated in SI units are to be regarded as the 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

• Status: Historical
• Publication Date: 09-Aug-2000
• ICS: 75.160.40 - Biofuels
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.04.0L - Gas Chromatography Methods

Relations

• Replaces: ASTM D6584-00 - Test Method for Determination of Free and Total Glycerine in B-100 Biodiesel Methyl Esters by Gas Chromatography
• Effective Date: 10-Aug-2000
• Replaced By: ASTM D6584-07 - Standard Test Method for Determination of Free and Total Glycerin in B-100 Biodiesel Methyl Esters By Gas Chromatography
• Effective Date: 01-Jan-2007
• Referred By: ASTM D6751-23a - Standard Specification for Biodiesel Fuel Blendstock (B100) for Middle Distillate Fuels
• Effective Date: 10-Aug-2000
• Referred By: ASTM D8144-22 - Standard Test Method for Separation and Determination of Aromatics, Nonaromatics, and FAME Fractions in Middle Distillates by Solid-Phase Extraction and Gas Chromatography
• Effective Date: 10-Aug-2000
• Referred By: ASTM D8181-19 - Standard Specification for Microemulsion Blendstock for Preparing Microemulsion Test Fuel Oils
• Effective Date: 10-Aug-2000

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
An American National Standard
e1
Designation:D6584–00
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
e NOTE—Corrected CAS number in Table 2 editorially in December 2005.
1. Scope 3.1.2 bonded glycerin, n—is the glycerin portion of the
mono-, di-, and triglyceride molecules.
1.1 This test method provides for the quantitative determi-
3.1.3 total glycerin, n—is the sum of free and bonded
nation 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
palmkernel oil.
4. Summary of Test Method
1.2 The values stated in SI units are to be regarded as the
4.1 The sample is analyzed by gas chromatography, after
standard.
silyating with N-methyl-N-trimethylsilyltrifluoracetamide
1.3 This standard does not purport to address all of the
(MSTFA). Calibration is achieved by the use of two internal
safety concerns, if any, associated with its use. It is the
standards and four reference materials. Mono-, di-, and trig-
responsibility of the user of this standard to establish appro-
lycerides are determined by comparing to monoolein, diolein,
priate safety and health practices and determine the applica-
and triolein standards respectively.Average conversion factors
bility of regulatory limitations prior to use.
are applied to the mono-, di-, and triglycerides to calculate the
2. Referenced Documents bonded glycerin content of the sample.
2.1 ASTM Standards:
5. Significance and Use
D 4307 Practice for Preparation of Liquid Blends for Use as
2 5.1 Free and bonded glycerin content reflects the quality of
Analytical Standards
biodiesel. A high content of free glycerin may cause problems
E 355 Practice for Gas Chromatography Terms and Rela-
3 during storage, or in the fuel system, due to separation of the
tionships
glycerin. A high total glycerin content can lead to injector
E 594 Practice for Testing Flame Ionization Detectors Used
3 fouling and may also contribute to the formation of deposits at
in Gas or Supercritical Fluid Chromatography
injection nozzles, pistons, and valves.
3. Terminology
6. Apparatus
3.1 Definitions:
6.1 Chromatographic System—See Practice E 355 for spe-
3.1.1 biodiesel (B-100), n—fuel comprised of mono-alkyl
cific designations and definitions.
esters of long chain fatty acids derived from vegetable oils or
6.1.1 Gas Chromatograph (GC)—the system must be ca-
animal fats.
pable of operating at the conditions given in Table 1.
6.1.2 Column, open tubular column with a 5 % phenylpoly-
1
dimethylsiloxane bonded and cross linked phase internal coat-
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of D02.04 on
ing. The column should have an upper temperature limit of at
Hydrocarbon Analysis.
least 400°C. Columns, either 10 m or 15 m in length, with a
Current edition approved Aug. 10, 2000. Published September 2000.
2 0.32 mm internal diameter, and a 0.1 µm film thickness have
Annual Book of ASTM Standards, Vol 05.02.
3
Annual Book of ASTM Standards, Vol 14.02. been found satisfactory. Any column with better or equivalent
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D6584–00
TABLE 1 Operating Conditions
8. Preparation of Apparatus
Injector
8.1 Install and condition the column in accordance with
Cool on column injection
manufacturer or supplier’s instructions. After conditioning,
Sample size 1 µl
Column Temperature Program
attach column outlet to flame ionization detector inlet and
Initial temperature 50°C hold 1 min
check for leaks throughout the system. If leaks are found,
Rate 1 15°C / min to 180°C
tightenorreplacefittingsandrecheckforleaksbeforeproceed-
Rate 2 7°C / min to 230°C
Rate 3 30°C / min 380°C hold 10 min ing.
Defector
Type Flame ionization
9. Calibration and Standardization
Temperature 380°C
Carrier Gas
9.1 Preparation of Calibration Standards—Prepare stan-
Type Hydrogen or helium measur
...