Standard Test Method For

Designation: D3279 – 07
Standard Test Method for

n-Heptane Insolubles1
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.
1. Scope 5.1.1 Erlenmeyer Flask, of 250-mL capacity adapted to an

1.1 This test method covers determination of the mass Allihn-type reflux condenser, each with a 35/25 ball joint.
percent of asphaltenes as defined by insolubility in normal- 5.1.2 Magnetic Stirrer and Magnetic-Stirrer Hot Plate,
heptane solvent. It is applicable to all solid and semi-solid equipped with a voltage regulator.
petroleum asphalts containing little or no mineral matter, to gas 5.1.3 Gooch Crucible, glazed inside and outside with the
oils, to heavy fuel oils, and to crude petroleum that has been exception of the outside bottom surface. The approximate
topped to a cut-point of 343°C or higher. dimensions shall be a diameter of 44 mm at the top tapering to
1.2 The values stated in SI units are to be regarded as the 36 mm at the bottom and a depth of 20–30mm.
standard. 5.1.4 Filter Pad, glass-fiber 32 mm in diameter.3
1.3 This standard does not purport to address all of the 5.1.5 Filter Flask, heavy-wall with side tube, 500-mL
safety concerns, if any, associated with its use. It is the capacity.
responsibility of the user of this standard to establish appro- 5.1.6 Filter Tube, 40 to 42 mm in inside diameter.
priate safety and health practices and determine the applica- 5.1.7 Rubber Tubing, or adapter for holding Gooch cru-
bility of regulatory limitations prior to use. See Section 7 for a cible on the filter tube.
specific hazard statement. NOTE 1—Other suitable assemblies permitting vacuum filtration with a
Gooch crucible may be used.
2. Referenced Documents
2.1 ASTM Standards:2 6. Solvent
C670 Practice for Preparing Precision and Bias Statements 6.1 n-Heptane, 99.0 minimum mol % (Pure Grade).
for Test Methods for Construction Materials
7. Hazards
3. Summary of Test Method 7.1 n-Heptane has a boiling point of 98°C and a flash point
3.1 The sample is dispersed in n-heptane and filtered of −1°C, which means that it should be handled with care. It is
through a glass-fiber pad. The insoluble material is washed, recommended that both the reflux dispersion and filtration
dried, and weighed. steps be conducted in a ventilated hood and away from flames
or other sources of heat.
4. Significance and Use
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
5. Apparatus and Materials oils (Note 2). Add n-heptane in the ratio 100 mL of solvent per
5.1 The assembly of the dispersing apparatus is illustrated in 1 g of sample, using proportionally less or more solvent as
Fig. 1 with details of the component parts as follows: dependent upon the sample size. Unless the asphalt is in a
granular form, heat the flask gently and turn it to cause the
sample to be distributed somewhat over the bottom or lower
1
This test method is under the jurisdiction of ASTM Committee D04 on Road sides of the flask.
and Paving Materials and is the direct responsibility of Subcommittee D04.47 on
Miscellaneous Asphalt Tests. NOTE 2—Tests show a small amount of insolubles (60.3 mass %)
Current edition approved Aug. 1, 2007. Published August 2007. Originally remain on walls of the precipitation flask despite repeated washings. When
approved in 1973. Last previous edition approved in 2001 as D3279 – 97 (2001). expected level of n–C7 insolubles is 6 % or less, use of a tared 250-mL
DOI: 10.1520/D3279-07.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [email protected]. 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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
D3279 – 07
Erlenmeyer flask is recommended. After all possible precipitate has been 9. Calculation and Report
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 9.1 Calculate the mass percent of normal-heptane insolubles
and 9.1. (NHI) as the percentage by weight of the original sample as
follows:
8.2 Place the Erlenmeyer flask, containing the sample plus
solvent with magnetic stirrer added, on the magnetic-stirrer hot NHI, % 5 ~A/B! 3 100 (1)
plate and secure under the reflux condenser. With the magnetic
where:
stirrer in operation, adjust for gentle refluxing for a period of
A = total mass of insolubles, and
15 to 20 min when testing paving binders, fuel oils, gas oils, or B = total mass of sample.
crude residues. For airblown asphalts, a reflux period of 25 to
For percentages of insolubles less than 1.0, report to the nearest
30 min is recommended. In all cases, allow the dispersed
0.01 %; for percentages of insolubles of 1.0 or more, report to
mixture to cool to room temperature for a period of 1 h.
the nearest 0.1 %.
8.3 Place the Gooch crucible plus one thickness of the
glass-fiber filter pad in an oven at about 107°C for 15 min,
10. Precision and Bias
allow to cool in a desiccator, and then weigh to the nearest 0.1
mg. Set up the filtering crucible plus filter pad in the suction 10.1 Precision of the method has been determined as fol-
flask and pre-wet with 5 mL of n-heptane (see Fig. 2). Warm lows:
the flask containing the sample plus solvent to 38 to 49°C on Acceptable Range of
the hot plate and pour its contents (except for the magnetic Standard DeviationA Two ResultsA
stirrer) through the filter using a gentle vacuum. Filtration will Single-operator 0.53 % NHI 1.51 % NHI
proceed most rapidly if the supernatant liquid is filtered first Multilaboratory 0.93 % NHI 2.78 % NHI
with the insolubles transferred to the filter last. Police the _____________
beaker or flask while transferring the final precipitate, using A

These numbers represent, respectively, the (1S) and (D2S) limits as described
either a rubber policeman or stainless steel spatula with a in Practice C670. The precision is for samples covering a range from 4.0 to 29.0 %
HI.
squared end. Wash the precipitate with three portions of
n-heptane of about 10 mL each, first rinsing out the flask
11. Keywords
therewith. Place the crucible in the 107°C oven for a period of
15 min, cool in a desiccator, and weigh. 11.1 asphaltenes; heptane insolubles
2
D3279 – 07
FIG. 1 Dispersing Apparatus
3
D3279 – 07
FIG. 2 Filtration Apparatus
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Designation: D3279 – 07

1. Scope 5.1.1 Erlenmeyer Flask, of 250-mL capacity adapted to an

beaker or flask while transferring the final precipitate, using A

FIG. 1 Dispersing Apparatus

FIG. 2 Filtration Apparatus

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