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.

Designation: D6560 − 22

Designation: IP 143 ⁄21

Standard Test Method for

Determination of Asphaltenes (Heptane Insolubles) in Crude
Petroleum and Petroleum Products1,2
This standard is issued under the fixed designation D6560; 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* 2. Referenced Documents

1.1 This test method covers a procedure for the determina- 2.1 ASTM Standards:3
tion of the heptane insoluble asphaltene content of gas oil, D86 Test Method for Distillation of Petroleum Products and
diesel fuel, residual fuel oils, lubricating oil, bitumen, and Liquid Fuels at Atmospheric Pressure
crude petroleum that has been topped to an oil temperature of D1298 Test Method for Density, Relative Density, or API
260 °C (see A1.2.1.1). Gravity of Crude Petroleum and Liquid Petroleum Prod-
1.2 The precision is applicable to values between ucts by Hydrometer Method
0.50 % m ⁄m and 30.0 % m ⁄m. Values outside this range may D4052 Test Method for Density, Relative Density, and API
still be valid but may not give the same precision values. Gravity of Liquids by Digital Density Meter
D4057 Practice for Manual Sampling of Petroleum and
1.3 Oils containing additives may give erroneous results. Petroleum Products
1.4 The values stated in SI units are to be regarded as D4175 Terminology Relating to Petroleum Products, Liquid
standard. No other units of measurement are included in this Fuels, and Lubricants
standard. D4177 Practice for Automatic Sampling of Petroleum and
Petroleum Products
1.5 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 2.2 Energy Institute Standard:4
responsibility of the user of this standard to establish appro- Specifications for IP Standard Thermometers
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use. 3. Terminology
1.6 This international standard was developed in accor- 3.1 Definitions:
dance with internationally recognized principles on standard- 3.1.1 For definitions of terms used in this test method, refer
ization established in the Decision on Principles for the to Terminology D4175.
Development of International Standards, Guides and Recom-
3.1.2 asphaltenes, n—(rarely used in the singular) — in
mendations issued by the World Trade Organization Technical
petroleum technology, represent an oil fraction that is soluble
Barriers to Trade (TBT) Committee.
in a specified aromatic solvent but separates upon addition of
an excess of a specified paraffinic solvent.
3.1.2.1 Discussion—In this test method, the aromatic sol-
1
This test method is under the jurisdiction of ASTM International Committee vent is hot toluene and the paraffinic solvent is heptane.
D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct
responsibility of ASTM Subcommittee D02.14 on Stability, Cleanliness and 3.1.2.2 Discussion—Historically, benzene was the aromatic
Compatibility of Liquid Fuels. The technically equivalent standard as referenced is solvent, but benzene is not typically used now for health
under the jurisdiction of the Energy Institute Subcommittee SC-B-5. reasons. The precision of this test method when using toluene
Current edition approved June 1, 2022. Published July 2022. Originally approved
in 2000. Last previous edition approved in 2017 as D6560 – 17. DOI: 10.1520/ has been found to be the same as when using benzene.
D6560-22.
2
This standard is based on material published in the IP Standard methods for
Analysis and Testing of Petroleum and Related Products and British Standard 2000
3
Parts, copyright Energy Institute, 61 New Cavendish Street, London, W1M 8AR. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Adapted with permission of Energy Institute. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
This test method has been developed through the cooperative effort between Standards volume information, refer to the standard’s Document Summary page on
ASTM and the Energy Institute, London. ASTM and IP standards were approved by the ASTM website.
4
ASTM and EI technical committees as being technically equivalent but that does not Available from Energy Institute, 61 New Cavendish St., London, WIM 8AR,
imply both standards are identical. UK.

*A Summary of Changes section appears at the end of this standard

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

1
 D6560 − 22
4. Summary of Test Method
4.1 A test portion of the sample is mixed with heptane and
the mixture heated under reflux, and the precipitated
asphaltenes, waxy substances, and inorganic material are
collected on a filter paper. The waxy substances are removed
by washing with hot heptane in an extractor.
4.2 After removal of the waxy substances, the asphaltenes
are separated from the inorganic material by dissolution in hot
toluene, the extraction solvent is evaporated, and the as-
phaltenes weighed.

5. Significance and Use

5.1 Asphaltenes are the organic molecules of highest mo-
lecular mass and carbon-hydrogen ratio normally occurring in
crude petroleum and petroleum products containing residual
material. They may give problems during storage and handling
if the suspension of asphaltene molecules is disturbed through
excess stress or incompatibility. They are also the last mol-
ecules in a product to combust completely, and thus may be
one indicator of black smoke propensity. Their composition
normally includes a disproportionately high quantity of the
sulfur, nitrogen, and metals present in the crude petroleum or
petroleum product.
FIG. 1 Extractor
6. Apparatus
TABLE 1 Test Portion Size, Flask, and Heptane Volumes
6.1 General—Ground-glass joints from different sources
may have one of two diameter to length ratios. For the Estimated Asphaltene Test Portion
Content Size Flask Volume Heptane Volume
purposes of this test method, either is suitable, and for some % m/m g mL mL
applications, the diameter itself can be one of two. However, it Less than 0.5 10 ± 2 1000 300 ± 60
is critical that the male and female parts of each joint are from 0.5 to 2.0 8±2 500 240 ± 60
Over 2.0 to 5.0 4±1 250 120 ± 30
the same series to avoid recession or protuberance. Over 5.0 to 10.0 2±1 150 60 ± 15
Over 10.0 to 25.0 0.8 ± 0.2 100 25 to 30
6.2 Condenser, with a coil or double surface, fitted with a Over 25.0 0.5 ± 0.2 100 25 ± 1
34/45 or 34/35 ground-glass joint at the bottom to fit the top of
the extractor. Minimum length is 300 mm.
6.3 Reflux Extractor, conforming to the dimensions given in
6.8 Filter Papers, Whatman5 Grade 42, 110 mm or 125 mm
Fig. 1. Tolerances are 61 mm on the height and outer diameter
diameter.
(OD) of the extractor body and 60.5 mm on all other dimen-
sions. The female ground-glass joint at the top shall match the 6.9 Analytical Balance, capable of weighing with an accu-
male at the bottom of the condenser, and the male ground-glass racy of 0.1 mg.
joint at the bottom shall match the female of the conical flask. 6.10 Forceps, of stainless steel, spade ended.
6.4 Conical Flasks, of borosilicate glass of appropriate 6.11 Timing Device, electronic or manual, accurate to 1.0 s.
capacity (see 11.2 and Table 1), with ground-glass joints to fit 6.12 Oven, capable of maintaining a temperature from
the bottom of the extractor. 100 °C to 110 °C.
NOTE 1—Sizes 24/39, 24/29, 29/43, or 29/32 are suitable. 6.13 Graduated Cylinders, of 50 mL and 100 mL capacity.
6.5 Stopper, of borosilicate glass of a size to fit the conical 6.14 Stirring Rods, of glass or polytetrafluoroethylene
flask. (PTFE), 150 mm by 3 mm diameter.
6.6 Evaporating Vessel, of borosilicate glass. Either a hemi- 6.15 Cooling Vessel, consisting of either a dessicator with-
spherical dish of approximately 90 mm diameter, or another out desiccant, or another suitable tightly-stoppered vessel.
suitable vessel used in conjunction with a rotovapor.
NOTE 2—A rotovapor in conjunction with a nitrogen atmosphere 5
The sole source of supply of the filter papers known to the committee at this
reduces the hazard of toluene evaporation (see 11.7). time is Whatman Int. Ltd., Maidstone, UK. If you are aware of alternative suppliers,
please provide this information to ASTM International Headquarters. Your com-
6.7 Filter Funnel, of borosilicate glass, approximately ments will receive careful consideration at a meeting of the responsible technical
100 mm diameter. committee,1 which you may attend.

2
 D6560 − 22
6.16 Mixer, high-speed, nonaerating. expected asphaltene content of above 25 % m ⁄m, a minimum
heptane volume of 25 mL shall be used (see Table 1).
7. Reagents 11.3 Boil the mixture under reflux for 60 min 6 5 min.
7.1 Toluene (methylbenzene) [C6H5CH3], analytical reagent Remove the flask and contents at the end of this period, cool,
or nitration grade. close with a stopper (see 6.5), and store in a dark cupboard for
7.2 Heptane [C7H16], analytical reagent grade. 90 min to 150 min, calculated from the time of removal from
reflux.
8. Sampling 11.4 Place the filter paper, folded as shown in Fig. 2 (so as
8.1 Unless otherwise specified, take samples by the proce- to prevent loss of asphaltenes by creeping), in the filter funnel,
dures described in Practice D4057 or D4177. using forceps. Thereafter, handle the filter paper only with
forceps. Without agitation, decant the liquid into the filter
9. Test Portion Preparation paper, and then transfer the residue in the flask as completely
as possible with successive quantities of hot heptane, using the
9.1 Test portions from the laboratory samples shall be
stirring rod (see 6.14) as necessary. Give the flask a final rinse
drawn after thorough mixing and subdivision. Heat viscous
with hot heptane, and pour the rinsings through the filter. Set
samples of residual fuels to a temperature that renders the
the flask aside, without washing, for use as specified in 11.6.
sample liquid, but not above 80 °C, and homogenize, using the
mixer (see 6.16) as necessary. 11.5 Remove the filter paper and contents from the funnel,
and place in the reflux extractor (see 6.3). Using a flask
9.2 Heat samples of penetration grade bitumens to a tem-
different from that used initially, reflux with heptane (see 7.2)
perature not exceeding 120 °C, and stir well before taking an
at a rate of 2 drops ⁄s to 4 drops ⁄s from the end of the condenser
aliquot.
for an extraction period of not less than 60 min, or until a few
9.3 Samples of hard bitumens shall be ground to a powder drops of heptane from the bottom of the extractor leave no
before an aliquot is taken. residue on evaporation on a glass slide.
9.4 Samples of crude petroleum shall be prepared in accor- 11.6 Replace the flask by the one used initially, and to which
dance with the procedure described in the Annex A1, unless it has been added 30 mL to 60 mL of toluene (see 7.1), and
is known that the crude petroleum contains negligible quanti- continue refluxing until all the asphaltenes have been dissolved
ties of material boiling below 80 °C. from the paper.

10. Apparatus Preparation 11.7 Transfer the contents of the flask to a clean and dry (see
Section 10) evaporating vessel (see 6.6), weighed to the nearest
10.1 Clean all glass flasks (see 6.4) and dishes (see 6.6) by 0.2 mg by tare against a similar dish. Wash out the flask with
a means that matches the cleanliness obtained by the use of a successive small quantities of toluene to a total not exceeding
strongly oxidizing agent, such as ammonium peroxydisulfate 30 mL. Remove the toluene by evaporation on a boiling water
in concentrated sulfuric acid at approximately 8 g ⁄L, or sulfu- bath, or by evaporation in a rotovapor under an atmosphere of
ric acid itself, soaking for at least 12 h, followed by rinses in nitrogen. (Warning—Perform the evaporation in a fume
tap water, distilled water, and the acetone, using forceps only hood.)
for handling. Strong oxidizing acid cleaning solutions are
highly corrosive and potentially hazardous in contact with 11.8 Dry the dish and contents in the oven (see 6.12) at
organic materials. 100 °C to 110 °C for 30 min. Cool in the cooling vessel (see
6.15) for 30 min to 60 min and reweigh by tare against the dish
10.2 For routine analysis, use a proprietary laboratory used previously for this purpose, and which has been subjected
detergent to clean the glassware, followed by the rinses to the same heating and cooling procedure as was the dish
described in 10.1. When the detergent cleaning no longer containing asphaltenes.
matches the cleanliness required based on visual appearance,
use a strong oxidizing agent. NOTE 3—Asphaltenes are very susceptible to oxidation, and it is
important that the procedure specified in the final drying stage is adhered
10.3 After rinsing, place the glassware in the oven (see to exactly as regards to temperature and time 61 min.
6.12) for 30 min, and cool in the cooling vessel (see 6.15) for
30 min before weighing.

11. Procedure
11.1 Estimate the asphaltene content of the sample, or
residue obtained from the procedure in Annex A1, and weigh
the quantity, to the nearest 1 mg for masses above 1 g and to
the nearest 0.1 mg for masses of 1 g and below (see Table 1),
into a flask (see 6.4) of appropriate capacity (see Table 1).
11.2 Add heptane (see 7.2) to the test portion in the flask at
a ratio of 30 mL to each 1 g of sample if the expected
asphaltene content is below 25 % m ⁄m. For samples with an FIG. 2 Filter Paper

3
 D6560 − 22
12. Calculation carried out in 1975 to confirm the precision. No data from the
12.1 Calculate the asphaltene content, A, in % m/m, of 1956 evaluation program can be found.
petroleum products as follows: NOTE 4—A recent (1998) interlaboratory program in France on four
samples with asphaltene contents in the range from 0.50 % m ⁄m to
A 5 100 ~ M/G ! (1) 22.0 % m ⁄m resulted in estimated precision values very similar to those
given in 14.2 and 14.3, except for the reproducibility at very low levels
where: (<2.0 % m ⁄m), which was significantly worse.
M = is the mass of asphaltenes, in grams, and 14.2 Repeatability—The difference between two successive
G = is the mass of test portion, in grams.
test results obtained by the same operator with the same
12.2 Calculate the asphaltene content, C, in % m/m, of apparatus under constant operating conditions on identical test
crude petroleum prepared in the manner described in the material would, in the normal and correct operation of the test
Annex, as follows: method, exceed the value below in only 1 case in 20.
C 5 100 ~ MR/GD! (2) r 5 0.1 A (3)
where: where A is the average result, in % m/m.
M = is the mass of asphaltenes, in grams, 14.3 Reproducibility—The difference between two single
R = is the mass of the residue from distillation, in grams, and independent results obtained by different operators work-
G = is the mass of the residue aliquot, in grams, and ing in different laboratories on nominally identical test material
D = is the mass of crude petroleum sample distilled, in would, in the normal and correct operation of the test method,
grams. exceed the value below in only 1 case in 20.
R 5 0.2 A (4)
13. Report
where A is the average result, in % m/m.
13.1 Report the following information:
13.1.1 The heptane insoluble asphaltene content of values 14.4 Bias—Since heptane insoluble asphaltenes are defined
less than 1.00 % m ⁄m, to the nearest 0.05 % m ⁄m, by Test by this test method, no bias can be assigned. The term
Method D6560. asphaltenes may be associated with other similar procedures
13.1.2 The heptane insoluble asphaltene content of values using alkanes as precipitating agents other than heptane. In
of 1.0 % m ⁄m and greater, to the nearest 0.1 % m ⁄m, by Test general, lighter alkanes will give higher results and heavier
Method D6560. alkanes will give lower results than heptane, but no consistent
ratio can be assigned.
14. Precision and Bias 15. Keywords
14.1 Precision—The precision values were determined in an 15.1 asphaltenes; bitumen; crude petroleum; diesel fuel; gas
interlaboratory program, using benzene as solvent, in 1956. A oil; heptane insoluble residues; lubricating oil; residual fuel
second interlaboratory program, using toluene as solvent, was oils

ANNEX

(Mandatory Information)

A1. PREPARATION OF CRUDE PETROLEUM RESIDUE BY DISTILLATION

A1.1 Scope

A1.1.1 This annex covers a procedure for the preparation of A1.3 Summary of Test Method
a crude petroleum residue (topped to an oil temperature of
A1.3.1 A weighed test portion of the crude petroleum
260 °C) suitable for the determination of asphaltene content
sample is distilled in specified glass apparatus under specified
(see 9.4).
conditions of heat input and rate of distillation. The distillation
A1.2 Terminology is stopped at an oil temperature of 260 °C and the mass of the
residue determined.
A1.2.1 Definitions:
A1.2.1.1 crude petroleum residue, n—residue from distilla-
A1.4 Apparatus
tion to an oil temperature of 260 °C carried out under condi-
tions of this specific preparatory procedure. A1.4.1 Distillation Apparatus:

4
 D6560 − 22
A1.4.1.1 Residue Distillation Apparatus, conforming to the A1.5.1.5 Distil off the water with the more volatile hydro-
requirements of Test Method D86, with the exception of the carbons in the apparatus described in A1.4.1.2. Charge the
temperature sensor. The temperature sensor shall be a liquid- flask with 300 mL of sample, and place the temperature sensor
in-glass thermometer of total immersion type of total length such that the sensing point (bulb) is immersed in the sample.
300 mm to 320 mm, with a temperature range from −4 °C to Heat the flask gently so that the oil temperature rises slowly to
360 °C, and a maximum scale error of 2 °C, or an alternative 150 °C, vaporizing into the condenser by means of a small gas
temperature measurement device or system of at least equiva- flame any drops of water that collect on the walls of the flask.
lent accuracy. A transparent bath, maintained at 15 °C 6 3 °C, Stop the distillation when no more water passes over in the
is mandatory for the receiver. distillate. Allow the residue to cool, run off the water collected
in the separating funnel, and add the oily distillate back to the
NOTE A1.1—A suitable thermometer is an IP 4C, as specified in
Appendix A of Specifications for IP Standard Thermometers. residue and mix thoroughly. If visible water is still present,
filter by the method described in A1.5.1.2.
A1.4.1.2 Drying Distillation Apparatus, conforming to
A1.4.1.1, with the exception of a 500 mL distillation flask A1.6 Procedure
instead of the flask specified, and a 200 mL separating funnel A1.6.1 Determine the density at 15 °C of the crude petro-
immersed in broken ice instead of the receiver. leum by Test Method D1298 or D4052.
A1.4.2 Drying Apparatus, consisting of one of the follow- A1.6.2 Weigh the distillation flask to the nearest 0.1 g, and
ing: charge it with a mass equivalent to 100 mL of sample at 15 °C
A1.4.2.1 Centrifuge. to within 0.1 g, ensuring that no oil flows down the vapor tube
A1.4.2.2 Filter Apparatus, operating at increased pressure. during this operation. Record the mass of oil (D). Place the
A1.4.2.3 Steel Container, capable of withstanding 1000 kPa liquid-in-glass thermometer so that the bottom of the bulb is
pressure and of being heated to 200 °C. 2.0 mm 6 0.5 mm from the bottom of the flask, or the
A1.4.2.4 Cottrell-type Electrostatic Separator. alternative temperature sensor to a position established to give
identical temperature readings.
A1.5 Sample Preparation NOTE A1.2—The position of the temperature sensor in the holder may
A1.5.1 If the crude petroleum contains sufficient water to be premarked before addition of the test portion to the flask.
cause difficulties in distillation (excessive foaming), dry the A1.6.3 Swab out the condenser tube, and assemble the
sample by a method that avoids the loss of volatile compo- apparatus with the vapor tube of the flask extending into the
nents. The methods given in A1.5.1.1 – A1.5.1.5 are suitable. condenser tube a distance of between 25 mm and 50 mm.
A1.5.1.1 Separate the water by gravity or by centrifuging in Make the connection between flask and condenser tight by
a closed container at the lowest practicable temperature. means of a stopper or bung through which the vapor tube
A1.5.1.2 Filter the sample at the lowest practicable tempera- passes.
ture and applied pressure, through anhydrous calcium chloride, A1.6.4 Place a clean dry receiver at the outlet of the
sodium sulfate, or other suitable drying agent, in a closed condenser such that the condenser tube or adaptor extends into
vessel. it at least 25 mm, but not below the 100 mL mark. Immerse the
A1.5.1.3 Heat the sample in a closed steel container (see receiver up to the 100 mL mark in the transparent bath (see
A1.4.2.3) fitted with a temperature sensor and pressure sensor. A1.4.1.1). Cover the top of the receiver closely during the
Fill the container to approximately 70 % capacity, and heat it distillation with a piece of paper weighted to restrict volatile
until the oil reaches a temperature of 200 °C, or until the losses and also to overcome the buoyancy of the receiver in the
pressure reaches 700 kPa. Allow the container to cool to water bath. Circulate ice-cold (below 4 °C) water through the
ambient temperature, and then decant the oil from the sepa- condenser.
rated water.
A1.6.5 Apply heat to the flask, and distil the crude petro-
A1.5.1.4 Construct a Cottrell-type separator from a tall
leum at a rate not exceeding 2.5 mL ⁄min until it ceases to
glass beaker with a brass gauze cylinder, lined with flannel that
foam, after which keep the rate of distillation constant at
has been saturated with water, and then squeezed out to leave
2.0 mL ⁄min to 2.5 mL ⁄min (approximately 1 drop ⁄s). Continue
it damp, fitted tightly inside. A brass gauze cylinder mounted
the distillation without interruption to 260 °C. Remove the
on the glass spindle of a laboratory stirrer, rotated at approxi-
heat, and allow the condenser to drain into the receiver.
mately 30 rev ⁄min, forms the central electrode. Pour the
sample into the beaker, and apply a voltage to the electrodes. A1.6.6 Allow the residue in the flask to cool, remove the
Interrupt the water precipitation at intervals to prevent the loss temperature sensor, and weigh the flask and residue. Record
of volatile components, and allow the oil to cool. Separate the the mass of the residue (R).
oil from the water that has coalesced and run down the flannel A1.6.7 Use this residue to carry out the procedure (see
lining. Section 11) for the determination of asphaltene content.

5
 D6560 − 22
SUMMARY OF CHANGES

Subcommittee D02.14 has identified the location of selected changes to this standard since the last issue
(D6560 – 17) that may impact the use of this standard. (Approved June 1, 2022.)

(1) Added reference to Terminology D4175 in Sections 2 and

3.

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