An American National Standard

Designation: D 2007 – 03

Standard Test Method for

Characteristic Groups in Rubber Extender and Processing
Oils and Other Petroleum-Derived Oils by the Clay-Gel
Absorption Chromatographic Method1
This standard is issued under the fixed designation D 2007; 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 (e) indicates an editorial change since the last revision or reapproval.

1. Scope * D 5309 Specification for Cyclohexane 9994

1.1 This test method covers a procedure for classifying oil E 691 Practice for Conducting an Interlaboratory Study to
samples of initial boiling point of at least 260°C (500°F) into Determine the Precision of a Test Method5
the hydrocarbon types of polar compounds, aromatics and 3. Terminology
saturates, and recovery of representative fractions of these
types. This classification is used for specification purposes in 3.1 Definitions of Terms Specific to This Standard:
rubber extender and processing oils. 3.1.1 The following terms refer to the hydrocarbon types
and structural groups as measured by this test method:
NOTE 1—See Test Method D 2226. 3.1.2 aromatics—material that, on percolation, passes
1.2 This test method is not directly applicable to oils of through a column of adsorbent clay in a n-pentane eluent but
greater than 0.1 mass % pentane insolubles. Such oils can be adsorbs on silica gel under the conditions specified.
analyzed after removal of these materials, but precision is 3.1.3 asphaltenes, or n-pentane insolubles—insoluble mat-
degraded (see Appendix X1). ter that precipitates from a solution of oil in n-pentane under
1.3 The values stated in SI units are to be regarded as the the specified conditions.
standard. The values given in parentheses are for information 3.1.4 polar aromatics—synonym for polar compounds.
only. 3.1.5 polar compounds—material retained on adsorbent
1.4 This standard does not purport to address all of the clay after percolation of the sample in n-pentane eluent under
safety concerns, if any, associated with its use. It is the the conditions specified.
responsibility of the user of this standard to establish appro- 3.1.6 saturates—material that, on percolation in a n-pentane
priate safety and health practices and determine the applica- eluent, is not adsorbed on either the clay or silica gel under the
bility of regulatory limitations prior to use. Specific warning conditions specified.
statements are given in 6.1, Section 7, A1.4.1, and A1.5.5.
4. Summary of Test Method
2. Referenced Documents 4.1 The sample is diluted with solvent and charged to a
2.1 ASTM Standards: glass percolation column containing clay in the upper section
D 86 Test Method for Distillation of Petroleum Products at and silica gel plus clay in the lower section. n-pentane is then
Atmospheric Pressure2 charged to the double column until a definite quantity of
D 323 Test Method for Vapor Pressure of Petroleum Prod- effluent has been collected. The upper (clay) section is removed
ucts (Reid Method)2 from the lower section and washed further with n-pentane. A
D 1159 Test Method for Bromine Numbers of Petroleum toluene-acetone mixture 50 to 50 by volume is then charged to
Distillates and Commercial Aliphatic Olefins by Electro- the clay section for desorption and a specified volume of
metric Titration2 effluent collected. The lower (gel) column may be desorbed by
D 2226 Classification for Various Types of Petroleum Oils recirculation of toluene.
for Rubber Compounding Use3 4.2 The solvents are completely removed from the recov-
ered n-pentane and the toluene-acetone fractions and the
residues are weighed and calculated as saturate and polar
compounds contents. Aromatics may be calculated by differ-
1
This test method is under the jurisdiction of ASTM Committee D02 on ence, or measured following evaporation of the toluene used
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.04 on Hydrocarbon Analysis. for desorption of the gel column.
Current edition approved May 10, 2003. Published June 2003. Originally
approved in 1968. Last previous edition approved in 2002 as D 2007–02.
2 4
Annual Book of ASTM Standards, Vol 05.01. Annual Book of ASTM Standards, Vol 06.04.
3 5
Annual Book of ASTM Standards, Vol 09.01. Annual Book of ASTM Standards, Vol 14.02.

*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
 D 2007 – 03
4.3 When the sample contains more than 0.1 mass % of NOTE 2—Temperatures should be uniform on the top of the hot plate.
n-pentane insolubles, this test method cannot be used directly. Some laboratory hot plates benefit by the inclusion of an aluminum plate,
The insoluble matter must be removed from the sample prior to approximately 6-mm thick, included under or on top of regular plate top.
charging to the column. A method for this removal is given as 6.8 Round Bottom Flask, 3-necked, borosilicate, 500-mL
an appendix. capacity (Fig. 3).
4.4 Alternative methods are provided (1) for recovery of 6.9 Condenser, borosilicate (Fig. 3).
aromatics from the gel column, and (2) for analysis of oil with 6.10 Adapter Tube with Vigreux column (Fig. 3).6,7
high-polar content. 6.11 Flexible Joint, TFE-fluorocarbon and borosilicate,
24/40 TS ground glass joints on each end.7,8
5. Significance and Use
5.1 The composition of the oil included in rubber com- 7. Reagents and Materials
pounds has a large effect on the characteristics and uses of the
compounds. The determination of the saturates, aromatics, and 7.1 Purity of Reagents, Reagent grade chemicals shall be
polar compounds is a key analysis of this composition. used in all tests. Unless otherwise indicated, it is intended that
5.2 The determination of the saturates, aromatics, and polar all reagents shall conform to the specifications of the commit-
compounds and further analysis of the fractions produced is tee on Analytical Reagents of the American Chemical Society,
often used as a research method to aid understanding of oil where such specifications are available.9 Other grades may be
effects in rubber and other uses. used, provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without lessening the
6. Apparatus accuracy of the determination.
6.1 Beakers, Anticreep, 150-mL capacity, as illustrated in 7.2 Acetone, reagent grade, minimum purity. (Warning—
Fig. 1. (Warning—Beakers should be examined for sharp Acetone is extremely flammable.)
edges and fire polished, if necessary.) 7.3 Calcium Chloride, anhydrous granules.
6.2 Clay-Gel Column, constructed as illustrated in Fig. 2. 7.4 Clay Adsorbent, 500 to 250 µm (30 to 60 mesh)
6.3 Conical Flasks, (Erlenmeyer), 250-mL capacity. Attapulgus.7,10 Clay quality may be determined using the
6.4 Solvent Receiver, capable of collecting solvent, without azobenzene equivalence test shown in Annex A1. The azoben-
splashing or loss of material during the analysis. A wide- zene activity test measures the adsorptive characteristics of the
mouth, graduated, 500-mL capacity Erlenmeyer flask is one clay. Azobenzene equivalence value should be 30 to 35. Clay
such example that has been found suitable to use. outside of these limits should be discarded.
6.5 Filter Funnel, long stem, 125-mm diameter; for use with 7.5 Cyclohexane, conforming to Specification D 5309. (Op-
185 mm ready folded, fine-texture, rapid filter paper. tional, see 8.1.9.) (Warning—Cyclohexane is extremely flam-
6.6 Separatory Funnel, 500 mL. mable. Harmful if inhaled.)
6.7 Hot Plate, explosion proof, controlled to a surface 7.6 Pentane,7 , 11 reagent grade minimum purity.
temperature of 100 to 105°C. (Warning—n-Pentane is extremely flammable. Harmful if
inhaled.)
7.7 Silica Gel, activated, conforming to the following in-
spections:7,12

6
The sole source of supply of the adapter tube known to the committee at this
time is Owens Glass Apparatus, Inc., 128 River Road, Channelview, TX 77530..
This item can be fabricated at any scientific glassblowing shop.
7
If you are aware of alternative suppliers, please provide this information to
ASTM International Headquarters. Your comments will receive careful consider-
ation at a meeting of the responsible technical committee 1, which you may attend.
8
Cole Parmer No. 6675-40 has been found suitable for this purpose.
9
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Annual Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
MD.
10
The sole source of supply of clay adsorbent known to the committee at this
time is Forcoven Products, P.O. Box 1556, Humble, TX 77347–1556. Packaged in
moisture resistant twinned packets of 50 and 100 g (sufficient for one determina-
tion). These packets are packed 50 sets per case. It is important that extremes of
temperature be avoided on stored clay samples.
11
The sole source of supply of pentane known to the committee at this time is
Special Products Div., Phillips Petroleum Co., Bartlesville, OK.
12
The sole source of supply of silica gel meeting these specifications known to
the committee at this time is Forcoven Products, P.O. Box 1556, Humble, TX
77347-1556, packaged in 200 g moisture resistant packets. Sieve analysis should be
FIG. 1 Anticreep Beaker checked on other sources of gel.

2
 D 2007 – 03

NOTE—Check to ascertain ID is 44 mm.

FIG. 2 Clay-Gel Percolating Column

Sieve analysis >30 sieve size, 5 % (mass) maximum; eluent solvents. Join the columns (clay over gel) after lubri-
>50 sieve size, 45 % (mass) min cating the joint with hydrocarbon-insoluble grease. It is impor-
>100 sieve size, 80 % (mass) min
>200 sieve size, 94 % (mass) min
tant that the adsorbents in each column be packed to a constant
level. A minimum of ten taps with a soft rubber hammer at
7.7.1 Gel should be activated for 4 h in an air oven at 190°C different points up and down and 25 taps on top of each column
in a shallow pan. should be employed to achieve constant level. A suitable
7.8 Toluene, reagent grade minimum purity. (Warning— rubber hammer may be assembled by fastening two No. 7 or 8
Toluene is flammable. Vapor harmful.) rubber stoppers on one end of a small rod about 200-mm long.
7.9 Toluene-Acetone Mixture (50 to 50 by volume), mix Use fresh adsorbents for each determination.
equal volumes of toluene and acetone. 8.1.2 If n-pentane insolubles were not determined, select the
7.10 In order to obtain results that are consistent with those appropriate sample size in accordance with the following polar
obtained elsewhere, it is very important that only the reagents content ranges, if the proper range can be anticipated; other-
and materials described in this section be used. wise, use a 10 6 0.5 g sample.
Polar Content Range,
8. Procedure mass percent Sample Size, g
8.1 Fractionation: 0–20 10 6 0.5
Above 20 5 6 0.2
8.1.1 Prepare the adsorption column (Fig. 2) by placing 100
g of clay adsorbent in the upper section of the column and 200 8.1.3 Dilute with 25 mL of n-pentane solvent and mix well
g of silica gel plus 50 g of clay on top of the gel in the lower to ensure a uniform solution of the sample. The sample should
section (Note 4). Place a piece of glass wool (of about 25-mm not display precipitate or flocculate at this point. If a precipitate
loose thickness) over the top surface of the clay in the upper is present asphaltenes may be removed by the procedure of
column to prevent agitation of the clay while charging the Appendix X1, however, the precision statement no longer

3
 D 2007 – 03

FIG. 3 Extraction Apparatus

applies. It is important that the polar content result obtained be 8.1.5 When nearly all of the washings have entered the clay,
not greater than that for the sample size as specified above, charge n-pentane to the column and maintain a head level well
since the capacity of the clay for retaining polar constituents above the clay beds (Note 4) to wash the saturate portion of the
becomes limited at these concentrations. If results exceed this sample from the adsorbents. Recover 280 6 10 mL of the first
specification, repeat the test using a smaller sample. Partition- n-pentane effluent from the column in a graduated, 500-mL
ing between aromatics and polar compounds is affected by wide-mouth conical flask.
sample size. Results using different sample size may not be NOTE 4—Columns may be briefly separated, if necessary, to give a
equivalent. solvent head 5- to 10-mm deep in the second (lower) column. Loss of the
NOTE 3—For viscous oils, dilutions of the sample with 25 mL of head will give channeling in the lower column, with inaccurate results.
cyclohexane is more convenient and does not affect the results. Cyclo- NOTE 5—With long use, the frits in the absorption columns become
hexane used in this manner will not detect small quantities of asphaltenes, progressively less porous. If the time for percolation doubles over that for
however. a new column, the slow columns are to be discarded.
8.1.4 Add 25 mL of n-pentane to the top of the clay portion NOTE 6—If only saturates are to be determined, proceed to 8.3 and
subsequent calculation of saturates.
of the assembled column and allow to percolate into the clay.
As soon as nearly all of the n-pentane has entered the clay, 8.1.6 Disconnect the two sections. Allow the lower section
charge to the column the diluted sample of 8.1.3. Wash the to drain into a receiver. Continue washing the upper clay
sample beaker (or flask) with n-pentane and add the washings section with n-pentane. Maintain a moderate liquid head level
to the column. After nearly all of this material has entered the above the clay during this wash and adjust n-pentane additions
clay, wash the walls of the column above the clay free of so that the level is about 25 mm when 150 mL have been
sample with n-pentane. The sample and eluent solvent can be collected in the receiver. Discontinue additions at this point and
added to the column through a 65-mm diameter, wide-stem allow the liquid to essentially drain from the column. The
funnel (the funnel can be left on top of the column). At no time quantity in the receiver should then be about 200 mL. The
during the run should air be allowed to enter the clay bed. n-pentane from this step and from the draining of the lower

4
 D 2007 – 03
column should be discarded if aromatics are to be determined and this n-pentane added to the respective anti-creep beakers.
by difference. This n-pentane should be added to the aromatics To avoid a potential safety incident, it is recommended that the
solution from the gel column during solvent evaporation (8.3) anti-creep beakers be temporarily removed from the hot plate
if aromatics are to be recovered. when transfers are made, such as when the n-pentane rinsings
are added, before placing the anti-creep beakers back onto the
NOTE 7—This extra n-pentane washing of the clay section is necessary
in order to ensure complete removal of aromatics from the clay. hot plate.
8.3.2 When essentially all the solvent is evaporated, weigh
8.1.7 After n-pentane effluent has essentially drained from the beakers at 10 min intervals. Solvents are considered
the column, charge a 50 to 50 volume mixture of toluene–ac- removed when the weight loss between weighings is less than
etone. Collect the effluent in a 500-mL separatory funnel. 10 mg.
Collect 250 mL of the toluene-acetone (plus n-pentane) effluent
or until the effluent is practically colorless (only in exceptional 9. Calculation
cases will more than 300 mL of effluent be required). 9.1 Calculate the amount of n-pentane insolubles, saturates,
8.1.8 Stopper the separatory funnel containing the toluene- aromatics, and polar compounds in the sample as follows:
acetone fraction and swirl it a few times to aid in settling the Saturates, mass % 5 ~B/A! 3 100 (1)
water. Then let it stand for about 5 min. Drain off and discard
the lower (aqueous) layer. Add approximately 10 g of anhy- Aromatics, mass % 5 ~C/A! 3 100 (2)
drous calcium chloride granules to the fraction remaining in the
separatory funnel and shake for about 30 s; vent frequently
Polar compounds ~Note 11!, for 10 g sample 5 ~D/A! 3 100 (3)
during the shaking period. Allow the mixture to settle for at
least 10 min.
Polar compounds, mass % for 5 g sample 5 @~0.88 3 D/A!# 3 100
8.1.9 Filter the fraction through a rapid folded filter paper
(4)
catching the filtrate in a 500-mL conical flask. Rinse the
separatory funnel with approximately 25 mL of n-pentane, where:
filter and collect with the mixed solvent fraction. Wash the A = grams of original sample used,
filter paper with an additional 10 to 15 mL of n-pentane and B = grams of residue from n-pentane effluent from the clay
collect with the mixed solvent fraction. IMPORTANT—Make gel column (8.1.4),
all transfers of organic solvents from the separatory funnels C = grams of residue from the toluene desorption of the
through the top and avoid transferring any water that may have lower column and from the last n-pentane rinse of the
accumulated around the calcium chloride. columns (8.1.6 and 8.2.3), and
8.2 Desorption of Aromatics: D = grams of residue from toluene-acetone effluent (8.1.8).
8.2.1 If it is desired to determine the aromatics by isolation
rather than by difference, the gel column (lower column of the NOTE 9—The factor included in the calculation for the 5 g sample is
clay gel adsorption column of 8.1, see Fig. 2), after the 280 6 established experimentally to maintain continuity of results over a wide
10 mL of n-pentane have been collected, is placed in the range of polar compounds in rubber extender oils.
extraction assembly of Fig. 3. 9.2 If saturates, aromatics, and polars are all determined, the
8.2.2 Toluene (200 6 10 mL) is placed in the 500-mL flask total mass of all the recovered fractions must equal at least
and refluxed at such a rate of 10 6 2 mL/min for 2 h. 97 % of the sample charged. If this recovery is not obtained,
NOTE 8—Toluene reflux can be measured by collection for a 1 min repeat the test.
period using a graduated cylinder through valve A, Fig. 3. 9.3 If aromatics were not desorbed, use the n-pentane
insolubles, saturates content, and polar compounds as deter-
8.2.3 At the end of this time, the valve (A) is opened and the
mined in 9, calculate the amount of aromatics as follows:
toluene removed into a waste solvent receiver to a volume of
approximately 50-mL in the flask. The solution remaining is Aromatics, mass % 5 100 2 ~E 1 F! (5)
then combined with the n-pentane from 8.1.6 for recovery of where:
aromatics. Do not go further by distillation, as oil will be lost, E = mass % saturates, and
giving inaccurate results. F = mass % polar compounds.
8.3 Solvent Removal:
8.3.1 Label and weigh for tare the anti-creep beakers that 10. Report
are to be used for the evaporation of solvent (one each for polar 10.1 Report the following information:
compounds, saturates, and aromatics desorbed). Fill the anti- 10.1.1 Sample identification.
creep beakers approximately half full with the respective 10.1.2 Saturate content, aromatic content, and polar content,
solutions, (saturates from 8.1.4, aromatics from 8.1.6 and 8.2.3, as appropriate, in mass %.
polars from 8.1.8), then place them on the controlled hot plate 10.1.3 Method of determination of aromatic content: des-
at surface temperature of 100 to 105°C, refilling as this volume orption (8.2) or difference (9.3).
is reduced to one-quarter full. A gentle sweep may be used over 10.1.4 If aromatics were desorbed, the percent recovery
the surface of the liquid. It should not ruffle the surface nor (9.2).
should this nitrogen jet be placed below the surface. The flasks 10.1.5 Asphaltene content if the method of Appendix X1
which contained the fractions should be rinsed with n-pentane, was used.

5
 D 2007 – 03
11. Precision and Bias 13 the long run, in the normal and correct operation of this test
11.1 The precision of this test method as determined by method, exceed the following values only in one case in
statistical examination of interlaboratory results is as follows: twenty:
11.1.1 Repeatability—The difference between two test re- Saturate content, mass % 4.0
Aromatic content, mass % 3.3
sults, obtained by the same operator with the same apparatus Polar content, mass %
under constant operating conditions on identical test material, at polar contents of less than 1 % 0.4
would in the long run, in the normal and correct operation of at polar contents of 1 % to 5 % 1.3
at polar contents of greater than 5 % 1.8
the test method, exceed the following values only in one case
in twenty: 11.1.3 The above precision statements do not include
Saturate content, mass % 2.1 samples that have been prepared by removal of asphaltenes
Aromatic content, mass % 2.3 (Appendix X1). The precision on such samples is poorer than
Polar content, mass %
at polar contents of less than 1 % 0.24 the statements above.
at polar contents of 1 to 5 % 0.81 11.2 Bias—The procedure for measuring saturates, aro-
at polar contents of greater than 5 % 1.2
matic, and polar contents has no bias because the values are
11.1.2 Reproducibility—The difference between two single defined only in terms of this test method.
and independent results obtained by different operators work-
ing in different laboratories on identical test material would, in 12. Keywords
12.1 clay-gel absorption; elution chromatography; hydro-
13
Supporting data have been filed at ASTM International Headquarters and may carbon type; liquid chromatography; petroleum derived oils;
be obtained by requesting Research Report RR: D02-1193. rubber extender oils; rubber processing oils

ANNEX

(Mandatory Information)

A1. AZOBENZENE ACTIVITY TEST FOR CLAY

A1.1 Scope A1.3.5 Spectrophotometer, capable of operation at 446-mm

wavelength,7,14 equipped with a 1-mm (or 0.5-mm) thickness
A1.1.1 This test method describes a procedure for measur-
cell.
ing the adsorption activity of percolation type clays.
A1.4 Reagents
A1.2 Summary of Test Method
A1.4.1 Azobenzene Solution (1 %), prepared by dissolving
A1.2.1 A solution of 1 mass % azobenzene in isooctane is 10 6 0.001 g of c.p. azobenzene in 990 g of isooctane.
percolated through a weighed amount of clay contained in a (Warning—Azobenzene is a suspect carcinogen. Isooctane is
specified column. The amount of liquid recovered as percolate flammable.)
at the point where the concentration of azobenzene is 0.5
mass % (50 mass % of the original concentration) is a measure A1.5 Procedure
of the adsorption activity of the clay. A1.5.1 Insert a small piece of glass wool into the bottom of
the glass column (6.0-mm outside diameter tubing) and move
A1.3 Apparatus it up the tubing until top surface is 25 mm (1 in.) from the joint
A1.3.1 Azobenzene Percolation Column, glass constructed of the two glass sections (see Fig. A1.1).
from 12.0-mm outside diameter and 6.0-mm outside diameter NOTE A1.1—Insert a sufficient amount of glass wool to hold in place.
standard glass tubing with a reservoir of approximately 125 mL Fold the glass wool to produce a smooth surface for the top of the plug.
near the top. The top of the column shall be a female spherical A1.5.2 Weigh 20 6 0.001 g of clay sample and pour it into
ground-glass joint. The bottom of the column has a stopcock the column.
with internal metering valve attached by means of a standard A1.5.3 Pack the clay in the column to a constant level by
taper joint. The entire percolation assembly is illustrated in Fig. using an electric vibrator.
A1.1.
NOTE A1.2—A satisfactorily packed column will be achieved by lightly
A1.3.2 Graduated Cylinders, 5 or 10-mL capacity, 0.1-mL holding the vibrator next to the column and moving it up and down over
graduation. the clay height. Perform the “up and down” vibrations at 4 points
A1.3.3 Gas or Air Pressure System, regulated. approximately 90° spacings around the column.
A1.3.4 Vibrator, electric. The type of tungsten carbide
tipped vibrating pencil used for marking glass is satisfactory if
a rubber stopper is slipped over the tip. 14
A Bausch and Lomb Spectronic 20 has been found suitable for this purpose.

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 D 2007 – 03

FIG. A1.1 Azobenzene Percolation Assembly

A1.5.4 Add 100–115 mL of azobenzene solution to the A1.5.7 Plot the effluent azobenzene concentration versus
column. the effluent volume, and graphically determine the effluent
A1.5.5 Collect percolate in graduated 5 or 10-mL cylinders. volume at 0.5 mass % azobenzene concentration (50 % of the
Maintain the percolation rate at 1 mL/min. The rate control starting solution concentration). This is the azobenzene equiva-
shall be approximately established after 3 mL have been lence of the clay.
collected and well established by the time 5 mL of eluent have A1.6 Interpretation of Results
been collected. Determine additional rate checks periodically
A1.6.1 The average of duplicate determinations of azoben-
throughout the test. If the rate is too fast, adjust the needle
zene equivalence is used to determine the suitability of a clay
value as necessary to maintain the specified rate. If the rate is
for use in this test method. If the duplicate azobenzene
found to be below the prescribed limit, connect the pressure
equivalence values differ by more than 1 mL, make a third
line to the top of the column and apply pressure to adjust to the
determination and use the average of all three.
specified rate. (Warning—Normally only light pressure will
A1.6.2 A Clay with an average azobenzene equivalence
be required; that is 5 to 15 mm Hg. At test termination, the
between 30 and 35 meets the activity criterion (see 7.3). Clay
number of minutes required to collect the eluent should not
with azobenzene equivalence values outside this range is not
differ from the millilitres of eluent collected by more than two.)
suitable for use in this test method.
A1.5.6 After 25 mL of effluent has been collected, collect at
least 6 samples sequentially of 2 mL each. Measure the A1.7 Precision and Bias
azobenzene concentration of these samples using the spectrom- A1.7.1 No statement is made about either the precision or
eter which has been previously calibrated with known concen- the bias of this procedure for determining the azobenzene
trations of azobenzene in isooctane, using a wavelength of 446 equivalence of clay since the result merely states whether there
mm. is conformance to the criteria specified in this test method.

7
 D 2007 – 03

APPENDIX

(Nonmandatory Information)

X1. PROCEDURE FOR SAMPLES WITH PRECIPITATES OR FLOCCULATE

X1.1 Removal of Asphaltenes X1.1.1.4 Transfer the solution to an anti-creep beaker in

X1.1.1 If the diluted sample of 8.1.9 is not free from portions and evaporate the n-pentane on a hot plate at a
precipitates or flocculate, an approximation of the characteris- temperature of 100–105°C. Rinse the flask with small portions
tic groups can be obtained by the following procedure: of n-pentane, adding these rinsings to the anti-creep beaker.
X1.1.1.1 Weigh 10 6 0.5 g of the sample to the nearest 0.5 n-Pentane shall be considered removed when the change in
mg in a preweighed 250-mL conical flask, add 100 mL of weight is less than 10 mg in 10 min at this temperature. Slow
n-pentane and mix well. Warm the mixture in a warm water nitrogen flows over the beaker can be used to assist the
bath for a few seconds with intermittent swirling to hasten evaporation, but rapid stirring by the gas should be avoided.
solution. Allow the mixture to stand about 30 min at or near X1.1.1.5 Weigh the recovered oil. The weight of sample
room temperature. Samples containing a high content of (7.1) less the weight of the oil is the asphaltenes content. This
insolubles may require more agitation to dissolve the oil can then be diluted for charge to the clay-gel column (6.2).
n-pentane-soluble portion. In such cases, use a stirring rod,
together with intermittent warming and swirling to hasten X1.2 Precision and Bias
solution of the sample. Solution should be cooled to room
temperature before filtering. X1.2.1 The precision of this test method was determined by
X1.1.1.2 Set up a filtering assembly, using a 500-mL flask, a round robin of too few samples to meet the requirements of
a 125-mm borosilicate filtering funnel equipped with a folded Practice E 691. However, it can be approximated as:
rapid 15-cm filter paper, and filter the sample. Rinse the conical Repeatability: 1.3 %
flask and stirring rod with 60-mL n-pentane, and pour the rinse Reproducibility: 7.8 %
through the paper filter. X1.2.2 Bias—There is insufficient interlaboratory test data
X1.1.1.3 Rinse the filter paper and contents with 60 mL of to establish a statistical statement of bias for the procedure in
n-pentane in small portions from a dispensing bottle, taking Appendix X1.
care to rinse down the sides of the filter paper.

SUMMARY OF CHANGES

Committee D02.04 has identified the location of selected changes to this standard since the last issue
(D 2007–02) that may impact the use of this standard.

(1) Added new Note 5. (3) Corrected 10.1.2.

(2) Corrected 9.2.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
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