ASTM D3279-19

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Designation: D3279 − 12 D3279 − 19
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. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
ε NOTE—Section 8.1 was editorially corrected in March 2016.
1. 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°C343 °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 The text of this standard references notes and footnotes which provide explanatory material. These notes and footnotes
(excluding those in tables and figures) shall not be considered as requirements of the standard.
1.4 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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. See Section 7 for a specific hazard statement.
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.
2. Referenced Documents
2.1 ASTM Standards:
C670 Practice for Preparing Precision and Bias Statements for Test Methods for Construction Materials
3. Summary of Test Method
3.1 The sample is dispersed in n-heptane and filtered through a glass-fiber pad. The insoluble material is washed, dried, and
weighed.
4. 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.
5. Apparatus and Materials
5.1 The assembly of the dispersing apparatus is illustrated in Fig. 1 with details of the component parts as follows:
5.1.1 Erlenmeyer Flask, of 250-mL capacity adapted to an Allihn-type reflux condenser.
5.1.2 Magnetic Stirrer and Magnetic-Stirrer Hot PlatePlate.
5.1.3 Bitumen Crucible or Gooch Crucible, glazed inside and outside with the exception of the outside bottom surface. The
approximate dimensions shall be a diameter of 44 mm at the top tapering to 36 mm at the bottom and a depth of 20–30 mm.20
to 30 mm.
5.1.4 Glass Microfiber Filter Pad, 32–34 32 to 34 mm in diameter, fine porosity, fast flow rate, 1.5υm1.5-μm particle retention.
5.1.5 Filter Flask, heavy-wall with side tube, 500-mL capacity.
5.1.6 Filter Tube, 40 to 42 mm in inside diameter.
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.
Current edition approved Dec. 1, 2012June 15, 2019. Published December 2012June 2019. Originally approved in 1973. Last previous edition approved in 20072012 as
D3279 – 07.D3279 – 12. DOI: 10.1520/D3279-12E01.10.1520/D3279-19.
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volume information, refer to the standard’s Document Summary page on the ASTM website.
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D3279 − 19
5.1.7 Rubber Tubing, or adapter for holding Gooch crucible on the filter tube.
NOTE 1—Other suitable assemblies permitting vacuum filtration with a crucible may be used.
5.1.8 Oven, Oven, capable of maintaining a temperature of 110 6 5ºC.5 °C.
5.1.9 Desicator, of suitable size, charged with an effective desiccant.
5.1.10 Balance, capable of making the required measurements to an accuracy of at least 0.0001 g.
6. Reagent
6.1 n-Heptane, 99.0 minimum mol % (Pure Grade).(pure grade).
7. Hazards
7.1 n-Heptane has a boiling point of 98°C98 °C and a flash point of −1°C,−1 °C, which means that it should be handled with
care. It is recommended that both the reflux dispersion and filtration steps be conducted in a ventilated hood and away from flames
or other sources of heat.
8. Preparation of Crucible
8.1 Place the Gooch crucible plus one thickness filter pad in an oven at about 110 6 5ºC5 °C for 30 min, allow to cool in a
desiccator for 30 6 5 min, and then determine the mass to the nearest 0.1 mg. Designate this mass as A. Store in a desiccator until
ready for use.
9. Sample Preparation
9.1 If the sample is not fluid, heat to any convenient temperature, but in any case not more than 100ºC100 °C above the
softening point.
10. Procedure
10.1 Note Safetysafety precautions in Section 7. Transfer into the tare
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