ASTM D3279-12e1
(Test Method)Standard Test Method for n-Heptane Insolubles
Standard Test Method for <emph type="ital">n</emph>-Heptane Insolubles
SIGNIFICANCE AND USE
4.1 This test method is useful in quantifying the asphaltene content of petroleum asphalts, gas oils, heavy fuel oils, and crude petroleum. Asphaltene content is defined as those components not soluble in n-heptane.
SCOPE
1.1 This test method covers determination of the mass percent of asphaltenes as defined by insolubility in normal-heptane solvent. It is applicable to all solid and semi-solid petroleum asphalts containing little or no mineral matter, to gas oils, to heavy fuel oils, and to crude petroleum that has been topped to a cut-point of 343°C or higher.
1.2 The values stated in SI units are to be regarded as the 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. See Section 7 for a specific hazard statement.
General Information
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Standards Content (Sample)
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Designation: D3279 − 12
Standard Test Method for
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n-Heptane Insolubles
This standard is issued under the fixed designation D3279; 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.
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ε NOTE—Section 8.1 was editorially corrected in March 2016.
1. Scope 5. Apparatus and Materials
1.1 This test method covers determination of the mass
5.1 Theassemblyofthedispersingapparatusisillustratedin
percent of asphaltenes as defined by insolubility in normal-
Fig. 1 with details of the component parts as follows:
heptane solvent. It is applicable to all solid and semi-solid
5.1.1 Erlenmeyer Flask, of 250-mL capacity adapted to an
petroleumasphaltscontaininglittleornomineralmatter,togas
Allihn-type reflux condenser.
oils, to heavy fuel oils, and to crude petroleum that has been
5.1.2 Magnetic Stirrer and Magnetic-Stirrer Hot Plate
topped to a cut-point of 343°C or higher.
5.1.3 Bitumen Crucible or Gooch Crucible, glazed inside
1.2 The values stated in SI units are to be regarded as the
and outside with the exception of the outside bottom surface.
standard. No other units of measurement are included in this
The approximate dimensions shall be a diameter of 44 mm at
standard.
the top tapering to 36 mm at the bottom and a depth of
20–30mm.
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 5.1.4 Glass Microfiber Filter Pad, 32–34 mm in diameter
fine porosity, fast flow rate, 1.5υm particle retention.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
5.1.5 Filter Flask, heavy-wall with side tube, 500-mL
bility of regulatory limitations prior to use. See Section 7 for a
capacity.
specific hazard statement.
5.1.6 Filter Tube, 40 to 42 mm in inside diameter.
5.1.7 Rubber Tubing, or adapter for holding Gooch crucible
2. Referenced Documents
on the filter tube.
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2.1 ASTM Standards:
NOTE 1—Other suitable assemblies permitting vacuum filtration with a
C670Practice for Preparing Precision and Bias Statements
crucible may be used.
for Test Methods for Construction Materials
5.1.8 Oven, capable of maintaining a temperature of 110 6
3. Summary of Test Method
5ºC.
3.1 The sample is dispersed in n-heptane and filtered
through a glass-fiber pad. The insoluble material is washed, 6. Reagent
dried, and weighed.
6.1 n-Heptane, 99.0 minimum mol% (Pure Grade).
4. Significance and Use
7. Hazards
4.1 This test method is useful in quantifying the asphaltene
7.1 n-Heptane has a boiling point of 98°C and a flash point
content of petroleum asphalts, gas oils, heavy fuel oils, and
crude petroleum. Asphaltene content is defined as those com- of −1°C, which means that it should be handled with care. It is
recommended that both the reflux dispersion and filtration
ponents not soluble in n-heptane.
steps be conducted in a ventilated hood and away from flames
or other sources of heat.
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This test method is under the jurisdiction of ASTM Committee D04 on Road
and Paving Materials and is the direct responsibility of Subcommittee D04.47 on
Miscellaneous Asphalt Tests. 8. Preparation of Crucible
Current edition approved Dec. 1, 2012. Published December 2012. Originally
8.1 PlacetheGoochcrucibleplusonethicknessfilterpadin
approved in 1973. Last previous edition approved in 2007 as D3279–07. DOI:
10.1520/D3279-12E01.
an oven at about 110 6 5ºC for 30 min, allow to cool in a
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For referenced ASTM standards, visit the ASTM website, www.astm.org, or
desiccator for 30 6 5 min, and then determine the mass to the
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
nearest 0.1 mg. Designate this mass asA. Store in a desiccator
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. until ready for use.
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D3279 − 12
9. Sample Preparation the hot plate and pour its contents (except for the magnetic
stirrer) through the filter using a gentle vacuum. Filtration will
9.1 If the sample is not fluid, heat to any convenient
proceed most rapidly if the supernatant liquid is filtered first
temperature, but in any case not more than 100ºC above the
with the insolubles transferred to the filter last. Police the
softening point.
beaker or flask while transferring the final precipitate, using
either a rubber policeman or stainless steel spatula with a
10. Procedure
squared end. Wash the precipitate with three portions of
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