ASTM D3279-97(2001)

Standard Test Method for n-Heptane Insolubles

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 650°F (343°C) or higher.  
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 problems 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

• Status: Historical
• Publication Date: 09-Aug-1997
• ICS: 91.100.50 - Binders. Sealing materials
• ICS: 93.080.20 - Road construction materials
• Technical Committee: D04 - Road and Paving Materials
• Drafting Committee: D04.47 - Miscellaneous Asphalt Tests

Relations

• Replaces: ASTM D3279-97 - Standard Test Method for n-Heptane Insolubles
• Effective Date: 10-Aug-1997
• Replaced By: ASTM D3279-07 - Standard Test Method for n-Heptane Insolubles
• Effective Date: 01-Aug-2007
• Referred By: ASTM D6703-19 - Standard Test Method for Automated Heithaus Titrimetry
• Effective Date: 10-Aug-1997
• Referred By: ASTM D7996-15 - Standard Test Method for Measuring Visible Spectrum of Asphaltenes in Heavy Fuel Oils and Crude Oils by Spectroscopy in a Microfluidic Platform (Withdrawn 2024)
• Effective Date: 10-Aug-1997

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
Designation:D3279–97 (Reapproved 2001)
Standard Test Method for
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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope 5.1.2 Magnetic Stirrer and Magnetic-Stirrer Hot Plate,
equipped with a voltage regulator.
1.1 This test method covers determination of the mass
5.1.3 Gooch Crucible, glazed inside and outside with the
percent of asphaltenes as defined by insolubility in normal-
exception of the outside bottom surface. The approximate
heptane solvent. It is applicable to all solid and semi-solid
dimensions shall be a diameter of 44 mm at the top tapering to
petroleumasphaltscontaininglittleornomineralmatter,togas
36 mm at the bottom and a depth of 28 mm.
oils, to heavy fuel oils, and to crude petroleum that has been
5.1.4 Filter Pad, glass-fiber 32 mm in diameter.
topped to a cut-point of 343°C or higher.
5.1.5 Filter Flask, heavy-wall with side tube, 500-mL
1.2 The values stated in SI units are to be regarded as the
capacity.
standard.
5.1.6 Filter Tube, 40 to 42 mm in inside diameter.
1.3 This standard does not purport to address all of the
5.1.7 Rubber Tubing, or adapter for holding Gooch cru-
safety concerns, if any, associated with its use. It is the
cible on the filter tube.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
NOTE 1—Other suitable assemblies permitting vacuum filtration with a
bility of regulatory limitations prior to use. See Section 7 for a
Gooch crucible may be used.
specific hazard statement.
6. Solvent
2. Referenced Documents
6.1 n-Heptane, 99.0 minimum mol% (Pure Grade).
2.1 ASTM Standards:
7. Hazards
C670 Practice for Preparing Precision and Bias Statements
7.1 n-Heptane has a boiling point of 98°C and a flash point
for Test Methods for Construction Materials
of −1°C, which means that it should be handled with care. It is
3. Summary of Test Method
recommended that both the reflux dispersion and filtration
3.1 The sample is dispersed in n-heptane and filtered steps be conducted in a ventilated hood and away from flames
through a glass-fiber pad. The insoluble material is washed, or other sources of heat.
dried, and weighed.
8. Procedure
4. Significance and Use
8.1 Into the 250-mL Erlenmeyer flask, weigh to the nearest
4.1 This test method is useful in quantifying the asphaltene 0.1 mg a quantity of the sample to be tested, using 0.5 to 0.6
content of petroleum asphalts, gas oils, heavy fuel oils, and g for airblown asphalts, 0.7 to 0.8 g for asphalt paving binders
crude petroleum. Asphaltene content is defined as those com- and crude residues, and 1.0 to 1.3 g for gas oils and heavy fuel
ponents not soluble in n-heptane. oils(Note2).Add n-heptaneintheratio100mLofsolventper
1 g of sample, using proportionally less or more solvent as
5. Apparatus and Materials
dependent upon the sample size. Unless the asphalt is in a
5.1 Theassemblyofthedispersingapparatusisillustratedin granular form, heat the flask gently and turn it to cause the
Fig. 1 with details of the component parts as follows:
sample to be distributed somewhat over the bottom or lower
5.1.1 Erlenmeyer Flask, of 250-mLcapacity adapted to an sides of the flask.
Allihn-type reflux condenser, each with a 35/25 ball joint.
NOTE 2—Tests show a small amount of insolubles (60.3 mass%)
remainonwallsoftheprecipitationflaskdespiterepeatedwashings.When
expected level of n–C insolubles is 6% or less, use of a tared 250-mL
1 7
This test method is under the jurisdiction of ASTM Committee D04 on Road
Erlenmeyer flask is recommended.After all possible precipitate has been
and Paving Materials and is the direct responsibility of Subcommittee D04.47 on
Miscellaneous Asphalt Tests.
Current edition approved Aug. 10, 1997. Published April 1998. Originally
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