ASTM D6584 Total Glycerides & Glycerin Testing in Biodiesel (FAME)
ASTM D6584 involves quantitative measurement of total monoglyceride, total diglyceride, total triglyceride, free and total glycerin in B-100 methyl esters by gas chromatography. Their properties and applications are covered by this test technique. The values stated in SI are considered as standard.
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- Overview
- Scope, Applications, and Benefits
- Test Process
- Specifications
- Instrumentation
- Results and Deliverables
Overview
ASTM D6584 is a standard test method for determining free and total glycerin, as well as mono-, di-, and triglycerides in biodiesel (fatty acid methyl esters, FAME) by gas chromatography. These compounds are by-products or unreacted feedstock components remaining from the transesterification process used to produce biodiesel.
Excess glycerin and glycerides can cause fuel filter plugging, injector deposits, and engine performance issues. This method is therefore a critical quality control tool in biodiesel production and is referenced in ASTM D6751, the standard specification for biodiesel fuel blends.
Scope, Applications, and Benefits
Scope
ASTM D6584 measures:
- Free glycerin content in biodiesel
- Monoglyceride, diglyceride, and triglyceride concentrations
- Total glycerin (combined free and bound glycerin)
- Compliance with biodiesel fuel quality specifications
Applications
- Biodiesel production quality control
- Compliance testing per ASTM D6751 and EN 14105
- Feedstock and transesterification process optimization
- Fuel blending and distribution quality assurance
- Research and development of alternative fuels
Benefits
- Ensures biodiesel meets regulatory fuel quality limits
- Prevents fuel system deposits and filter plugging
- Supports process optimization to maximize conversion efficiency
- Provides accurate, reproducible quantitative data
- Required for commercial biodiesel specification compliance
Test Process
Sample Preparation
Biodiesel sample is dissolved in an appropriate solvent and treated with a silylating agent to derivatize glycerides for GC analysis.
1GC Analysis
The derivatized sample is injected into a gas chromatograph with a high-temperature capillary column and FID detector.
2Peak Identification & Quantification
Chromatographic peaks corresponding to glycerin, mono-, di-, and triglycerides are identified and quantified using internal standards.
3Reporting
Free glycerin, total glycerin, and individual glyceride contents (% mass) are calculated and reported.
4Technical Specifications
| Parameter | Details |
|---|---|
| Standard | ASTM D6584 |
| Test Principle | Gas chromatography with FID after silylation derivatization |
| Applicable Materials | Biodiesel (FAME) samples |
| Measured Outputs | Free glycerin, mono/di/triglycerides, total glycerin (% mass) |
| Detection Method | Flame ionization detector (FID) |
| Column Type | High-temperature capillary GC column |
Instrumentation Used for Testing
- Gas chromatograph with high-temperature capillary column
- Flame ionization detector (FID)
- Silylating agent and derivatization equipment
- Analytical balance and volumetric pipettes
- Internal and external reference standards
- Data integration and reporting software
Results and Deliverables
- Free glycerin content (% mass)
- Mono-, di-, and triglyceride contents (% mass)
- Total glycerin content (% mass)
- Chromatograms with peak assignments
- Compliance assessment against ASTM D6751 limits
- Quality control and batch release reports
Frequently Asked Questions
Incomplete conversion during transesterification leaves mono-, di-, and triglycerides in the product. These can cause filter plugging, injector deposits, and cold-weather performance problems in engines.
ASTM D6751 specifies a maximum of 0.020% mass for free glycerin and 0.240% mass for total glycerin in finished biodiesel.
Glycerol and glycerides have high boiling points and poor volatility. Silylation converts hydroxyl groups into volatile trimethylsilyl derivatives, making them detectable by standard GC-FID.
Yes. High triglyceride levels indicate the presence of unreacted vegetable oil, which effectively signals incomplete transesterification or intentional adulteration.
Both ASTM D6584 and EN 14105 measure glycerides and glycerin in biodiesel by GC, and while procedural details differ slightly, results are broadly comparable for quality control purposes.
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