ASTM D3279-07

Standard Test Method for n-Heptane Insolubles

SIGNIFICANCE AND USE
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.
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

• Status: Historical
• Publication Date: 31-Jul-2007
• 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(2001) - Standard Test Method for n-Heptane Insolubles
• Effective Date: 01-Aug-2007
• Replaced By: ASTM D3279-12 - Standard Test Method for <emph type="ital">n</emph>-Heptane Insolubles
• Effective Date: 01-Dec-2012
• 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
• Effective Date: 01-Aug-2007
• Referred By: ASTM D6703-19 - Standard Test Method for Automated Heithaus Titrimetry
• Effective Date: 01-Aug-2007

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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 − 07
StandardTest Method for
1
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.
1. Scope 5. Apparatus and Materials
5.1 Theassemblyofthedispersingapparatusisillustratedin
1.1 This test method covers determination of the mass
Fig. 1 with details of the component parts as follows:
percent of asphaltenes as defined by insolubility in normal-
5.1.1 Erlenmeyer Flask, of 250-mL capacity adapted to an
heptane solvent. It is applicable to all solid and semi-solid
Allihn-type reflux condenser, each with a 35/25 ball joint.
petroleumasphaltscontaininglittleornomineralmatter,togas
5.1.2 Magnetic Stirrer and Magnetic-Stirrer Hot Plate,
oils, to heavy fuel oils, and to crude petroleum that has been
equipped with a voltage regulator.
topped to a cut-point of 343°C or higher.
5.1.3 Gooch Crucible, glazed inside and outside with the
1.2 The values stated in SI units are to be regarded as the
exception of the outside bottom surface. The approximate
standard.
dimensions shall be a diameter of 44 mm at the top tapering to
1.3 This standard does not purport to address all of the 36 mm at the bottom and a depth of 20–30mm.
3
safety concerns, if any, associated with its use. It is the 5.1.4 Filter Pad, glass-fiber 32 mm in diameter.
responsibility of the user of this standard to establish appro- 5.1.5 Filter Flask, heavy-wall with side tube, 500-mL
priate safety and health practices and determine the applica- capacity.
bility of regulatory limitations prior to use. See Section 7 for a 5.1.6 Filter Tube, 40 to 42 mm in inside diameter.
specific hazard statement. 5.1.7 Rubber Tubing, or adapter for holding Gooch crucible
on the filter tube.
2. Referenced Documents
NOTE 1—Other suitable assemblies permitting vacuum filtration with a
2
Gooch crucible may be used.
2.1 ASTM Standards:
C670Practice for Preparing Precision and Bias Statements
6. Solvent
for Test Methods for Construction Materials
6.1 n-Heptane, 99.0 minimum mol% (Pure Grade).
3. Summary of Test Method
7. Hazards
3.1 The sample is dispersed in n-heptane and filtered 7.1 n-Heptane has a boiling point of 98°C and a flash point
through a glass-fiber pad. The insoluble material is washed,
of −1°C, which means that it should be handled with care. It is
dried, and weighed. recommended that both the reflux dispersion and filtration
steps be conducted in a ventilated hood and away from flames
4. Significance and Use or other sources of heat.
4.1 This test method is useful in quantifying the asphaltene
8. Procedure
content of petroleum asphalts, gas oils, heavy fuel oils, and
8.1 Into the 250-mL Erlenmeyer flask, weigh to the nearest
crude petroleum. Asphaltene content is defined as those com-
0.1 mg a quantity of the sample to be tested, using 0.5 to 0.6
ponents not soluble in n-heptane.
g for airblown asphalts, 0.7 to 0.8 g for asphalt paving binders
and crude residues, and 1.0 to 1.3 g for gas oils and heavy fuel
oils(Note2).Add n-heptaneintheratio100mLofsolventper
1
This test method is under the jurisdiction of ASTM Committee D04 on Road
1 g of sample, using proportionally less or more solvent as
and Paving Materials and is the direct responsibility of Subcommittee D04.47 on
dependent upon the sample size. Unless the asphalt is in a
Miscellaneous Asphalt Tests.
granular form, heat the flask gently and turn it to cause the
Current edition approved Aug. 1, 2007. Published August 2007. Originally
approved in 1973. Last previous edition approved in 2001 as D3279–97(2001). sample to be distributed somewhat over the bottom or lower
DOI: 10.1520/D3279-07.
sides of the flask.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
3
Standards volume information, refer to the standard’s Document Summary page on Glass filter pads No. 934-AH (Huribut) may be purchased from Reeve Angel
the ASTM website. and Company, Clifton, NJ.
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D3279 − 07
FIG. 1 Dispersing Apparatus
NOTE 2—Tests show a small amount of insolubles (60.3 mass%)
8.3 Place the Gooch crucible plus one thickness of the
remainonwallsoftheprecipitationflaskdespiterepeatedwashings.When
glass-fiber filter pad in an oven at about 107°C for 15 min,
expected level of n–C insolubles is 6% or less, use of a tared 250-mL
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allow to cool in a desiccator, and then weigh to the nearest 0.1
Erle
...