Asphaltene Dispersancy Test
1.0 PRINCIPLE AND DEFINITION:
1.1 This procedure was developed to perform a field screening of asphaltene content
and to demonstrate the efficacy of asphaltene dispersants. It is intended as a general procedure
to determine the presence of asphaltenes and their tendency to precipitate (asphaltene
screening), and the relative efficacy of various dispersants and solvents (ADT). It may be most
useful in determining at which point in a production system asphaltenes become destabilized,
particularly with combinations of crude streams, and finding the best relative application point
for the asphaltene dispersant.
1.2 Asphaltene content (%) is not the only factor affecting deposition, as crudes may vary
greatly in the natural stability of colloidal asphaltenes by resins.
System parameters such as temperature and pressure are not addressed by this method.
Similarly, observed volumes of sediment in this test do not directly relate to % asphaltenes in
the crude and effective dosages of product, as the appearance is also affected by the particle
size of precipitated asphaltenes. This method is intended as a qualitative tool to indicate
relative tendencies more than absolute values for precipitation or dispersancy.
1.3 Several methods exist where asphaltenes are precipitated from the crude oil before testing.
Research indicates, however, that the characteristics of the asphaltene/resin properties may be
altered by isolation. Therefore, crude oil samples diluted 50/50 in toluene (asphaltenes are
soluble) are preferred. Deposits may be dissolved 10% in toluene.
.
2.0 EQUIPMENT:
2.1 15-mL API oil tubes (centrifuge or grindout) tubes (see Note)
2.2 Centrifuge tube rack
2.3 Eppendorf or Drummond pipet (50-100μL)
2.4 Stopwatch or other suitable timer
Note: the procedures assume that 15-mL tubes will be used. If 12.5-, 50- or
100-mL tubes are available, the tests can be performed using those tubes. The changes
necessary for those tubes are given in a table at the end of the procedure.
3.0 REAGENTS:
3.1 Hexane
3.2 Toluene
3.3 Sample to test
4.0 PROCEDURE - SAMPLE PREPARATION:
4.1 Crude:
4.1.1 Prepare a sample of dry oil in toluene (50/50). Residual emulsion must be broken. In many
cases, it will be sufficient to dilute the crude oil 50/50 with toluene and let stand before
centrifuging, separating the water and solids from the crude solution to be used for the testing.
Heat and emulsion breaker can be applied, if necessary.
4.2 Deposits:
4.2.1 Soak the deposit in a sufficient volume of toluene to give a 10% solution. Paraffins and
asphaltenes should dissolve; inorganic solids may remain.
4.3 Asphaltene Screening (Blank)
4.3.1 Add 15 ml of hexane to each of four centrifuge tubes (fill to the 100% mark on the tube).
4.3.2 Dose the hexane with the desired amount of crude oil/stock solution.
Typically, the following dosages are chosen: 50, 100, 200, & 300 μL. Use an Eppendorf or
Drummond pipet to accurately measure the crude oil solution.
4.3.3 Shake the centrifuge tubes vigorously for 60 seconds.
4.3.4 Allow the tubes to stand for one hour undisturbed in the centrifuge rack. Observe and
record the percent sedimentation that occurs due to gravity. Notice that as the amount of
crude oil in the hexane increases, the amount of precipitate also increases, and the supernatant
solution gets darker.
4.3.5 To determine the volume of crude oil used for dispersant screening,observe the volume
of untreated crude solution that gives between 4 and 10% sediment (0.6 – 1.5 mL).
4.3.6 NOTE: If more than 300 μL of crude solution is required to give 4% precipitate, this
indicates that asphaltenes are not present, or are naturally well stabilized in the crude oil.
4.4 Asphaltene Dispersant (ADT) Procedure
4.4.1 Add the desired amount of dispersant to each centrifuge tube.
Typically, the following dosages are chosen: 0 (blank), 10, 50, 100, & 200 ppm. For some crudes
(i.e. California crudes), up to 1000 ppm of dispersant may be required.
Note: Prepare 1.5% (v/v) solutions of dispersant in toluene. Use the following equation to
determine the amount of chemical:
Where X is the amount of chemical to be injected
Y is the amount of oil.
For example, 300 uL of the 50% stock solution will be equivalent to 150 uL of oil. Therefore, Y =
150 uL. For 500 ppm chemical, X = 5uL.
4.4.2 Fill the balance of the centrifuge tubes with hexane to the 100% mark (total volume = 15
mL) and mix well.
4.4.3 Add sufficient crude oil or asphaltene solution to the hexane so that the blank gives
between 4 and 10% sediment (volume determined above). This typically requires about 100 μL.
Use a measuring pipet to dose the tubes.
4.4.4 Shake the centrifuge tubes vigorously for 60 seconds.
4.4.5 Allow the tubes to stand undisturbed in the centrifuge rack. Observe and record the
percent sedimentation that occurs due to gravity after 15, 30, 60, 90 and 120 minutes. Longer
times may be measured.
5.0 CALCULATIONS:
5.1 Calculate the percent dispersion from the volume of sediment in the treated sample (Streat )
and blank (Sblank ) as follows:
% Dispersed = 100 x [ (Sblank - Streat) / Sblank ]
Notice that as the amount of dispersancy increases, the amount of precipitate decreases and
the supernatant solution gets darker.
6.0 REFERENCES:
6.1 ASTM Procedure No. D-3279. Determination of Asphaltenic Content of Crude Oil.
