ASTM D3279-97

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
• Technical Committee: D04 - Road and Paving Materials
• Drafting Committee: D04.47 - Miscellaneous Asphalt Tests

Relations

• Replaced By: ASTM D3279-97(2001) - Standard Test Method for n-Heptane Insolubles
• Effective Date: 10-Aug-1997
• 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Measuring Visible Spectrum of Asphaltenes in Heavy Fuel Oils and Crude Oils by Spectroscopy in a Microfluidic Platform (Withdrawn 2024)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NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 3279 – 97
Standard Test Method for
n -Heptane Insolubles
This standard is issued under the fixed designation D 3279; 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. Scope 5.1.3 Gooch Crucible, glazed inside and outside with the
exception of the outside bottom surface. The approximate
1.1 This test method covers determination of the mass
dimensions shall be a diameter of 44 mm at the top tapering to
percent of asphaltenes as defined by insolubility in normal-
36 mm at the bottom and a depth of 28 mm.
heptane solvent. It is applicable to all solid and semi-solid
5.1.4 Filter Pad, glass-fiber 32 mm in diameter.
petroleum asphalts containing little or no mineral matter, to gas
5.1.5 Filter Flask, heavy-wall with side tube, 500-mL ca-
oils, to heavy fuel oils, and to crude petroleum that has been
pacity.
topped to a cut-point of 343°C or higher.
5.1.6 Filter Tube, 40 to 42 mm in inside diameter.
1.2 The values stated in SI units are to be regarded as the
5.1.7 Rubber Tubing or adapter for holding Gooch crucible
standard.
on the filter tube.
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
NOTE 1—Other suitable assemblies permitting vacuum filtration with a
responsibility of the user of this standard to establish appro-
Gooch crucible may be used.
priate safety and health practices and determine the applica-
6. Solvent
bility of regulatory limitations prior to use. See Section 7 for a
6.1 n-Heptane, 99.0 minimum mol % (Pure Grade).
specific hazard statement.
2. Referenced Documents 7. Hazards
7.1 n-Heptane has a boiling point of 98°C and a flash point
2.1 ASTM Standards:
C 670 Practice for Preparing Precision and Bias Statements of −1°C, which means that it should be handled with care. It is
recommended that both the reflux dispersion and filtration
for Test Methods for Construction Materials
steps be conducted in a ventilated hood and away from flames
3. Summary of Test Method
or other sources of heat.
3.1 The sample is dispersed in n-heptane and filtered
8. Procedure
through a glass-fiber pad. The insoluble material is washed,
8.1 Into the 250-mL Erlenmeyer flask, weigh to the nearest
dried, and weighed.
0.1 mg a quantity of the sample to be tested, using 0.5 to 0.6
4. Significance and Use
g for airblown asphalts, 0.7 to 0.8 g for asphalt paving binders
4.1 This test method is useful in quantifying the asphaltene and crude residues, and 1.0 to 1.3 g for gas oils and heavy fuel
content of petroleum asphalts, gas oils, heavy fuel oils, and oils (Note 2). Add n-heptane in the ratio 100 mL of solvent per
crude petroleum. Asphaltene content is defined as those com- 1 g of sample, using proportionally less or more solvent as
ponents not soluble in n-heptane. dependent upon the sample size. Unless the asphalt is in a
granular form, heat the flask gently and turn it to cause the
5. Apparatus and Materials
sample to be distributed somewhat over the bottom or lower
5.1 The assembly of the dispersing apparatus is illustrated in sides of the flask.
Fig. 1 with details of the component parts as follows:
NOTE 2—Tests show a small amount of insolubles (60.3 mass %)
5.1.1 Erlenmeyer Flask of 250-mL capacity adapted to an
remain on walls of the precipitation flask despite repeated washings. When
Allihn-type reflux condenser, each with a 35/25 ball joint.
expected level of n–C insolubles is 6 % or less, use of a tared 250-mL
5.1.2 Magnetic Stirrer and Magnetic-Stirrer Hot Plate
Erlenmeyer flask is recommended. After all possible precipitate has been
equipped with a voltage regulator. washed from the flask to the filtering crucible in 8.3, include the flask with
the crucible for the drying, weighing, and calculation procedures in 8.3
and 9.1.
This test method is under the jurisdiction of ASTM Committee D-4 on Road
8.2 Place the Erlenmeyer flask, containing the sample plus
...