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ASTM D6584-10ae1

(Test Method)

Standard Test Method for Determination of Total Monoglyceride, Total Diglyceride, Total Triglyceride, and Free and Total Glycerin in B-100 Biodiesel Methyl Esters by Gas Chromatography

Standard Test Method for Determination of Total Monoglyceride, Total Diglyceride, Total Triglyceride, and 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 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 0.100 to 1.000 mass %, for diglyceride is 0.050 to 0.500 mass %, and for triglyceride is 0.050 to 0.500 mass %. The range of quantitation for free glycerin is 0.005 to 0.05 mass % and for 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 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

Status
Historical
Publication Date
31-Oct-2010
ICS
75.160.20 - Liquid fuels
Technical Committee
D02 - Petroleum Products, Liquid Fuels, and Lubricants
Drafting Committee
D02.04.0L - Gas Chromatography Methods
Current Stage
Ref Project

Relations

Replaces
ASTM D6584-10a - Standard Test Method for Determination of Total Monoglyceride, Total Diglyceride, Total Triglyceride, and Free and Total Glycerin in B-100 Biodiesel Methyl Esters by Gas Chromatography
Effective Date
01-Nov-2010
Replaced By
ASTM D6584-13 - 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
Effective Date
01-May-2013
Referred By
ASTM D8181-19 - Standard Specification for Microemulsion Blendstock for Preparing Microemulsion Test Fuel Oils
Effective Date
01-Nov-2010
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
01-Nov-2010
Referred By
ASTM D6751-23a - Standard Specification for Biodiesel Fuel Blendstock (B100) for Middle Distillate Fuels
Effective Date
01-Nov-2010

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ASTM D6584-10ae1 - Standard Test Method for Determination of Total Monoglyceride, Total Diglyceride, Total Triglyceride, and Free and Total Glycerin in B-100 Biodiesel Methyl Esters by Gas ChromatographyASTM D6584-10ae1 - Standard Test Method for Determination of Total Monoglyceride, Total Diglyceride, Total Triglyceride, and Free and Total Glycerin in B-100 Biodiesel Methyl Esters by Gas Chromatography
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ASTM D6584-10ae1 - Standard Test Method for Determination of Total Monoglyceride, Total Diglyceride, Total Triglyceride, and Free and Total Glycerin in B-100 Biodiesel Methyl Esters by Gas Chromatography
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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
´1
Designation: D6584 − 10a
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
´ NOTE—Corrected formatting and spacing in Eqs 12-19 and added previous Summary of Changes editorially in March
2011.
1. Scope* 3. Terminology
1.1 This test method covers the quantitative determination 3.1 Definitions:
oftotalmonoglyceride,totaldiglyceride,totaltriglyceride,and 3.1.1 biodiesel (B-100), n—fuel comprised of mono-alkyl
free and total glycerin in B-100 methyl esters by gas chroma- esters of long chain fatty acids derived from vegetable oils or
tography.Therangeofquantitationformonoglycerideis0.100 animal fats.
to1.000mass%,fordiglycerideis0.050to0.500mass%,and
3.1.2 bonded glycerin, n—glycerin portion of the mono-,
for triglyceride is 0.050 to 0.500 mass %. The range of
di-, and triglyceride molecules.
quantitation for free glycerin is 0.005 to 0.05 mass % and for
3.2 Definitions of Terms Specific to This Standard:
total glycerin from 0.05 to 0.5 mass %. This procedure is not
3.2.1 total glycerin, n—sum of free and bonded glycerin.
applicable to vegetable oil methyl esters obtained from lauric
3.3 This test method makes reference to many common gas
oils, such as coconut oil and palm kernel oil.
chromatographicprocedures,terms,andrelationships.Detailed
1.2 The values stated in SI units are to be regarded as
definitions can be found in Practices E355 and E594.
standard. No other units of measurement are included in this
standard.
4. Summary of Test Method
1.3 This standard does not purport to address all of the
4.1 The sample is analyzed by gas chromatography, after
safety concerns, if any, associated with its use. It is the
silyating with N-methyl-N-trimethylsilyltrifluoracetamide
responsibility of the user of this standard to establish appro-
(MSTFA). Calibration is achieved by the use of two internal
priate safety and health practices and determine the applica-
standardsandfourreferencematerials.Mono-,di-,andtriglyc-
bility of regulatory limitations prior to use.
eride are determined by comparing to monoolein, diolein, and
triolein standards respectively. Average conversion factors are
2. Referenced Documents
appliedtomono-,di-,andtriglyceridestocalculatethebonded
2
2.1 ASTM Standards:
glycerin content of the sample.
D4307Practice for Preparation of Liquid Blends for Use as
5. Significance and Use
Analytical Standards
5.1 Free and bonded glycerin content reflects the quality of
E355PracticeforGasChromatographyTermsandRelation-
ships biodiesel.Ahigh content of free glycerin may cause problems
during storage, or in the fuel system, due to separation of the
E594Practice for Testing Flame Ionization Detectors Used
in Gas or Supercritical Fluid Chromatography 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.
1
This test method is under the jurisdiction of ASTM Committee D02 on
6. Apparatus
Petroleum Products and Lubricants and is the direct responsibility of D02.04.0L on
Gas Chromatography Methods.
6.1 Chromatographic System—See Practice E355 for spe-
Current edition approved Nov. 1, 2010. Published January 2011. Originally
cific designations and definitions.
approved in 2000. Last previous edition approved in 2010 as D6584–10. DOI:
10.1520/D6584-10A.
6.1.1 Gas Chromatograph (GC)—The system must be ca-
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
pable of operating at the conditions given in Table 1.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
6.1.2 Column, open tubular column with a 5% phenylpo-
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. lydimethylsiloxane bonded and cross linked phase internal
*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 ----------------------
´1
D6584 − 10a
TABLE 1 Operating Conditions TABLE 2 Stock Solutions
Injector Approximate Volumetric
Cool on column injection Compound CAS No. Mass (mg) Flask Size
Sample size 1 µL (mL)
Column Temperature Program Glycerin 56-81-5 25 50
Initial temperature 50°C hold 1 min 1-Mono [cis-9-octadecenoyl]-rac- 111-03-5 50 10
glycerol (m
...

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5.1 Some acids can be present in aviation turbine fuels due either to the acid treatment during the refining process or to naturally occurring organic acids. Significant acid contamination is not likely to be present because of the many check tests made during the various stages of refining. However, trace amounts of acid can be present and are undesirable because of the consequent tendencies of the fuel to corrode metals that it contacts or to impair the water separation characteristics of the aviation turbine fuel.  
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5.1 The tendency of a fuel to vaporize in automotive engine fuel systems is indicated by the vapor-liquid ratio of the fuel.  
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5.1 Wear due to excessive friction resulting in shortened life of engine components such as fuel pumps and fuel controls has sometimes been ascribed to lack of lubricity in an aviation fuel.  
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5.3 The wear scar generated in the ball-on-cylinder lubricity evaluator (BOCLE) test is sensitive to contamination of the fluids and test materials, the presence of oxygen and water in the atmosphere, and the temperature of the test. Lubricity measurements are also sensitive to trace materials acquired during sampling and storage. Containers specified in Practice D4306 shall be used.  
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1.1 This test method covers assessment of the wear aspects of the boundary lubrication properties of aviation turbine fuels on rubbing steel surfaces.  
1.1.1 This test method incorporates two procedures, one using a semi-automated instrument and the second a fully automated instrument. Either of the two instruments may be used to carry out the test.  
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 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.  
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ASTM D7398-23(Test Method)
Standard Test Method for Boiling Range Distribution of Fatty Acid Methyl Esters (FAME) in the Boiling Range from 100 °C to 615 °C by Gas Chromatography

SIGNIFICANCE AND USE
5.1 The boiling range distribution of FAMES provides an insight into the composition of product related to the transesterification process. This gas chromatographic determination of boiling range can be used to replace conventional distillation methods for product specification testing with the mutual agreement of interested parties.  
5.2 Biodiesel (FAMES) exhibits a boiling point rather than a distillation curve. The fatty acid chains in the raw oils and fats from which biodiesel is produced are mainly comprised of straight chain hydrocarbons with 16 to 18 carbons that have similar boiling temperatures. The atmospheric boiling point of biodiesel generally ranges from 330 °C to 357 °C. The Specification D6751 value of 360 °C max at 90 % off by Test Method D1160 was incorporated as a precaution to ensure the fuel has not been adulterated with high boiling contaminants.
SCOPE
1.1 This test method covers the determination of the boiling range distribution of fatty acid methyl esters (FAME). This test method is applicable to FAMES (biodiesel, B100) having an initial boiling point greater than 100 °C and a final boiling point less than 615 °C at atmospheric pressure as measured by this test method.  
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1.6 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.  
1.7 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.  
1.8 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.

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5.1 This test method was developed to assess the performance of a heavy-duty engine oil in controlling engine wear under operating conditions selected to accelerate soot production and valve-train wear in a turbocharged and aftercooled four-cycle diesel engine with sliding tappet followers equipped with exhaust gas recirculation hardware.  
5.2 The design of the engine used in this test method is representative of many, but not all, modern diesel engines. This factor, along with the accelerated operating conditions, shall be considered when extrapolating test results.
SCOPE
1.1 This test method, commonly referred to as the Cummins ISB Test, covers the utilization of a modern, 5.9 L, diesel engine equipped with exhaust gas recirculation and is used to evaluate oil performance with regard to valve-train wear.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.2.1 Exceptions—SI units are provided for all parameters except where there is no direct equivalent such as the units for screw threads, National Pipe Threads/diameters, tubing size, or where there is a sole source of supply equipment specification.  
1.2.2 See also A7.1 for clarification; it does not supersede 1.2 and 1.2.1.  
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. See Annex A1 for general safety precautions.  
1.4 Table of Contents:    
Section  
Scope  
1  
Referenced Documents  
2  
Terminology  
3  
Summary of Test Method  
4  
Significance and Use  
5  
Apparatus  
6  
Engine Fluids and Cleaning Solvents  
7  
Preparation of Apparatus  
8  
Engine/Stand Calibration and Non-Reference Oil Tests  
9  
Test Procedure  
10  
Calculations, Ratings, and Test Validity  
11  
Report  
12  
Precision and Bias  
13  
Annexes  
Safety Precautions  
Annex A1  
Intake Air Aftercooler  
Annex A2  
The Cummins ISB Engine Build Parts Kit  
Annex A3  
Sensor Locations and Special Hardware  
Annex A4  
External Oil System  
Annex A5  
Cummins Service Publications  
Annex A6  
Specified Units and Formats  
Annex A7  
Oil Analyses  
Annex A8  
Alternate Fuel Approval Process  
Annex A9  
1.5 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.

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