This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what

changes have been made to the previous version. Because

it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.

Designation: D2007 − 11 (Reapproved 2016) D2007 − 19

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 D2007; 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 Scope*
1.1 This test method covers a procedure for classifying oil samples of initial boiling point of at least 260 °C (500 °F) into the
hydrocarbon types of polar compounds, aromatics and saturates, and recovery of representative fractions of these types. This
classification is used for specification purposes in rubber extender and processing oils.
NOTE 1—See Test Method D2226.
1.2 This test method is not directly applicable to oils of greater than 0.1 % by mass pentane insolubles. Such oils can be
analyzed after removal of these materials, but precision is degraded (see Appendix X1).
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
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
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applicability of regulatory limitations prior to use. Specific warning statements are given in 6.1, Section 7, A1.4.1, and A1.5.5.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization

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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:2
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D2226 Classification for Various Types of Petroleum Oils for Rubber Compounding Use
D5309 Specification for Cyclohexane 999 ASTM D2007-19
https://standards.iteh.ai/catalog/standards/sist/51359c4c-1ba8-43de-abb8-03a03ce6eec1/astm-d2007-19
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method

3. Terminology
3.1 Definitions of Terms Specific to This Standard:
3.1.1 The following terms refer to the hydrocarbon types and structural groups as measured by this test method:
3.1.2 aromatics—aromatics, n—material that, on percolation, passes through a column of adsorbent clay in a n-pentane eluent
but adsorbs on silica gel under the conditions specified.
3.1.3 asphaltenes, or n-pentane insolubles—insolubles, n—insoluble matter that precipitates from a solution of oil in n-pentane
under the specified conditions.
3.1.4 polar aromatics—aromatics, n—synonym for polar compounds.
3.1.5 polar compounds—compounds, n—material retained on adsorbent clay after percolation of the sample in n-pentane eluent
under the conditions specified.
3.1.6 saturates—saturates, n—material that, on percolation in a n-pentane eluent, is not adsorbed on either the clay or silica gel
under the conditions specified.

1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcommittee
D02.04.0C on Liquid Chromatography.
Current edition approved Oct. 1, 2016Dec. 15, 2019. Published November 2016January 2020. Originally approved in 1968. Last previous edition approved in 20112016
as D2007 – 11.D2007 – 11 (2016). DOI: 10.1520/D2007-11R16.10.1520/D2007-19.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.

*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

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 D2007 − 19
4. Summary of Test Method
4.1 The sample is diluted with solvent and charged to a glass percolation column containing clay in the upper section and silica
gel plus clay in the lower section. n-pentane is then charged to the double column until a definite quantity of effluent has been
collected. The upper (clay) section is removed from the lower section and washed further with n-pentane. A toluene-acetone
mixture 50 to 50 by volume is then charged to the clay section for desorption and a specified volume of effluent collected. The
lower (gel) column may be desorbed by recirculation of toluene.
4.2 The solvents are completely removed from the recovered 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 difference, or measured
following evaporation of the toluene used for desorption of the gel column.
4.3 When the sample contains more than 0.1 % by mass of n-pentane insolubles, this test method cannot be used directly. The
insoluble matter must be removed from the sample prior to charging to the column. A method for this removal is given as an
appendix.
4.4 Alternative methods are provided (1) for recovery of aromatics from the gel column, and (2) for analysis of oil with
high-polar content.
5. Significance and Use
5.1 The composition of the oil included in rubber compounds has a large effect on the characteristics and uses of the compounds.
The determination of the saturates, aromatics, and polar compounds is a key analysis of this composition.
5.2 The determination of the saturates, aromatics, and polar compounds and further analysis of the fractions produced is often
used as a research method to aid understanding of oil effects in rubber and other uses.
6. Apparatus
6.1 Beakers, Anticreep, 150-mL150 mL capacity, as illustrated in Fig. 1. (Warning—Beakers should be examined for sharp
edges and fire polished, if necessary.) iTeh Standards
6.2 Clay-Gel Column, constructed as illustrated in Fig. 2.
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6.3 Conical Flasks, (Erlenmeyer), 250 mL capacity.

graduated, 500 mL capacity Erlenmeyer Document Preview

6.4 Solvent Receiver, capable of collecting solvent, without splashing or loss of material during the analysis. A wide-mouth,
flask is one such example that has been found suitable to use.
6.5 Filter Funnel, long stem, 125 mm diameter; stem; for use with 185 mm ready folded, fine-texture, rapid filter paper.
6.6 Separatory Funnel, 500 mL. ASTM D2007-19
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FIG. 1 Anticreep Beaker

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 D2007 − 19

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NOTE 1—Check to ascertain ID is 44 mm. ASTM D2007-19
FIG. 2 Clay-Gel Percolating Column
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6.7 Hot Plate, explosion proof, controlled to a surface temperature of 100 °C to 105 °C.
NOTE 2—Temperatures should be uniform on the top of the hot plate. Some laboratory hot plates benefit by the inclusion of an aluminum plate,
approximately 6 mm thick, included under or on top of regular plate top.
6.8 Round Bottom Flask, 3-necked, borosilicate, 500 mL capacity (Fig. 3).
6.9 Condenser, borosilicate (Fig. 3).
6.10 Adapter Tube with Vigreux column (Fig. 3).3,4
6.11 Flexible Joint, TFE-fluorocarbon and borosilicate, 24/40 TS ground glass joints on each end.4,5
7. Reagents and Materials
7.1 Purity of Reagents, Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents shall conform to the specifications of the committee on Analytical Reagents of the American Chemical Society, where
such specifications are available.6 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high
purity to permit its use without lessening the accuracy of the determination.

3
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.
4
If you are aware of alternative suppliers, please provide this information to ASTM International Headquarters. Your comments will receive careful consideration at a
meeting of the responsible technical committee,1 which you may attend.
5
Cole Parmer No. 6675-40 has been found suitable for this purpose.
6
Reagent Chemicals, American Chemical Society Specifications,ACS Reagent Chemicals, Specifications and Procedures for Reagents and Standard-Grade Reference
Materials, American Chemical Society, Washington, DC. For Suggestionssuggestions on the testing of reagents not listed by the American Chemical Society, see
AnnualAnalar 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.

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ASTM D2007-19
FIG. 3 Extraction Apparatus
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7.2 Acetone, reagent grade, minimum purity. (Warning—Acetone is extremely flammable.)
7.3 Calcium Chloride, anhydrous granules.
7.4 Clay Adsorbent, 500 µm to 250 µm (30 mesh to 60 mesh) 60 mesh) Attapulgus.4,7 Clay quality may be determined using
the azobenzene equivalence test shown in Annex A1. The azobenzene activity test measures the adsorptive characteristics of the
clay. Azobenzene equivalence value should be 30 to 35. Clay outside of these limits should be discarded.
7.5 Cyclohexane, conforming to Specification D5309. (Optional, see 8.1.9.) (Warning—Cyclohexane is extremely flammable.
Harmful if inhaled.)
7.6 Pentane, ,reagent grade 99.0 % minimum purity. (Warning—
n-Pentane is extremely flammable. Harmful if inhaled.)
7.7 Silica Gel, activated, conforming to the following inspections:4,8
Sieve analysis >30 sieve size, 5 % (mass) maximum;
>50 sieve size, 45 % (mass) min
>100 sieve size, 80 % (mass) min
>200 sieve size, 94 % (mass) min
7.7.1 Gel should be activated for 4 h in an air oven at 190 °C in a shallow pan.

7
The sole source of supply of clay adsorbent known to the committee at this time is Forcoven Products, 22010 East Martin Dr., Porter, TX 77365. Packaged in moisture
resistant twinned packets of 50 and 100 g (sufficient for one determination). These packets are packed 50 sets per case. It is important that extremes of temperature be avoided
on stored clay samples.
8
The sole source of supply of pentane known to the committee at this time is Special Products Div., Phillips Petroleum Co., Bartlesville, OK.
8
The sole source of supply of silica gel meeting these specifications known to the committee at this time is Forcoven Products, 22010 East Martin Dr., Porter, TX 77365,
packaged in 200 g moisture resistant packets. Sieve analysis should be checked on other sources of gel.

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7.8 Toluene, reagent grade minimum purity. (Warning—Toluene is flammable. Vapor harmful.)
7.9 Toluene-Acetone Mixture (50 to 50 by volume), mix equal volumes of toluene and acetone.
7.10 In order to obtain results that are consistent with those obtained elsewhere, it is very important that only the reagents and
materials described in this section be used.

8. Procedure
8.1 Fractionation:
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 g
of silica gel plus 50 g of clay on top of the gel in the lower section (Note 5). Place a piece of glass wool (of about 25 mm loose
thickness) over the top surface of the clay in the upper column to prevent agitation of the clay while charging the eluent solvents.
Join the columns (clay over gel) after lubricating the joint with hydrocarbon-insoluble grease. It is important that the adsorbents
in each column be packed to a constant level. A minimum of ten taps with a soft rubber hammer at different points up and down
and 25 taps on top of each column should be employed to achieve constant level. A suitable rubber hammer may be assembled
by fastening two No. 7 or 8 rubber stoppers on one end of a small rod about 200 mm long. Use fresh adsorbents for each
determination.
8.1.2 If n-pentane insolubles were not determined, select the appropriate sample size in accordance with the following polar
content ranges, if the proper range can be anticipated; otherwise, use a 10 g 6 0.5 g sample.
Polar Content Range,
mass percent Sample Size, g
0–20 10 ± 0.5
Above 20 5 ± 0.2
8.1.3 Dilute with 25 mL of n-pentane solvent and mix well to ensure a uniform solution of the sample. The sample should not
display precipitate or flocculate at this point. If a precipitate is present asphaltenes may be removed by the procedure of Appendix
X1, however, the precision statement no longer applies. It is important that the polar content result obtained be not greater than
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that for the sample size as specified above, since the capacity of the clay for retaining polar constituents becomes limited at these
concentrations. If results exceed this specification, repeat the test using a smaller sample. Partitioning between aromatics and polar

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compounds is affected by sample size. Results using different sample size may not be equivalent.
NOTE 3—For viscous oils, dilutions of the sample with 25 mL of cyclohexane is more convenient and does not affect the results. Cyclohexane used

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in this manner will not detect small quantities of asphaltenes, however.
8.1.4 Add 25 mL of n-pentane to the top of the clay portion of the assembled column and allow to percolate into the clay. As
soon as nearly all of the n -pentane has entered the clay, charge to the column the diluted sample of 8.1.3. Wash the sample beaker
(or flask) with n-pentane and add the washings to the column. After nearly all of this material has entered the clay, wash the walls
ASTMThe
of the column above the clay free of sample with n-pentane. D2007-19
sample and eluent solvent can be added to the column through
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a 65 mm diameter, wide-stem funnel (the funnel can be left on top of the column). At no time during the run should air be allowed
to enter the clay bed.
8.1.5 When nearly all of the washings have entered the clay, charge n-pentane to the column and maintain a head level well
above the clay beds (Note 4) to wash the saturate portion of the sample from the adsorbents. Recover 280 mL 6 10 mL 300 mL
of the first n-pentane effluent from the column in a graduated, 500 mL wide-mouth conical flask.the solvent receiver.
NOTE 4—Columns may be briefly separated, if necessary, to give a solvent head 5 mm to 10 mm deep in the second (lower) column. Loss of the head
will give channeling in the lower column, with inaccurate results.
NOTE 5—With long use, the frits in the absorption columns become progressively less porous. If the time for percolation doubles over that for a new
column, the slow columns are to be discarded.
NOTE 6—If only saturates are to be determined, proceed to 8.3 and subsequent calculation of saturates.
8.1.6 Disconnect the two sections. Allow the lower section to drain into a receiver. Continue washing the upper clay section with
n-pentane. Maintain a moderate liquid head level above the clay during this wash and adjust n-pentane additions so that the level
is about 25 mm when 150 mL have been collected in the receiver. Discontinue additions at this point and allow the liquid to
essentially drain from the column. The quantity in the receiver should then be about 200 mL. The n-pentane from this step and
from the draining of the lower column should be discarded if aromatics are to be determined by difference. This n-pentane should
be added to the aromatics solution from the gel column during solvent evaporation (8.3) if aromatics are to be recovered.
NOTE 7—This extra n-pentane washing of the clay section is necessary in order to ensure complete removal of aromatics from the clay.
8.1.7 After n-pentane effluent has essentially drained from the column, charge a 50 to 50 volume mixture of toluene–acetone.
Collect the effluent in a 500 mL separatory funnel. Collect 250 mL of the toluene-acetone (plus n-pentane) effluent or until the
effluent is practically colorless (only in exceptional cases will more than 300 mL of effluent be required).
8.1.8 Stopper the separatory funnel containing the toluene-acetone fraction and swirl it a few times to aid in settling the water.
Then let it stand for about 5 min. Drain off and discard the lower (aqueous) layer. Add approximately 10 g of anhydrous calcium
chloride granules to the fraction remaining in the separatory funnel and shake for about 30 s; vent frequently during the shaking
period. Allow the mixture to settle for at least 10 min.

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8.1.9 Filter the fraction through a rapid folded filter paper catching the filtrate in a 500 mL conical flask. Rinse the separatory
funnel with approximately 25 mL of n-pentane, filter and collect with the mixed solvent fraction. Wash the filter paper with an
additional 10 mL to 15 mL of n-pentane and collect with the mixed solvent fraction. IMPORTANT—Make all transfers of organic
solvents from the separatory funnels through the top and avoid transferring any water that may have accumulated around the
calcium chloride.
8.2 Desorption of Aromatics:
8.2.1 If it is desired to determine the aromatics by isolation rather than by difference, the gel column (lower column of the clay
gel adsorption column of 8.1, see Fig. 2), after the 280 mL 6 10 mL of n-pentane have been collected, is placed in the extraction
assembly of Fig. 3.
8.2.2 Toluene (200 mL 6 10 mL) is placed in the 500 mL flask and refluxed at such a rate of 10 mL ⁄min 6 2 mL ⁄min for 2 h.
NOTE 8—Toluene reflux can be measured by collection for a 1 min period using a graduated cylinder through valve A, Fig. 3.
8.2.3 At the end of this time, the valve (A) is opened and the toluene removed into a waste solvent receiver to a volume of
approximately 50 mL in the flask. The solution remaining is then combined with the n-pentane from 8.1.6 for recovery of
aromatics. Do not go further by distillation, as oil will be lost, giving inaccurate results.
8.3 Solvent Removal:
8.3.1 Label and weigh for tare the anti-creep beakers that are to be used for the evaporation of solvent (one each for polar
compounds, saturates, and aromatics desorbed). Fill the anti-creep beakers approximately half full with the respective solutions,
(saturates from 8.1.4, aromatics from 8.1.6 and 8.2.3, polars from 8.1.8), then place them on the controlled hot plate at surface
temperature of 100 °C to 105 °C, refilling as this volume is reduced to one-quarter full. A gentle sweep may be used over the
surface of the liquid. It should not ruffle the surface nor should this nitrogen jet be placed below the surface. The flasks which
contained the fractions should be rinsed with n-pentane, and this n-pentane added to the respective anti-creep beakers. To avoid
a potential safety incident, it is recommended that the anti-creep beakers be temporarily removed from the hot plate when transfers
are made, such as when the n-pentane rinsings are added, before placing the anti-creep beakers back onto the hot plate.

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8.3.2 When essentially all of the solvent is evaporated, cool and weigh the beakers and their contents.
8.3.3 Place the beakers back on the hot plate, and heat for at least 10 min.

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8.3.4 Cool and weigh the beakers and their contents.
8.3.5 Repeat 8.3.3 and 8.3.4 until the weight loss between weighings is less than 10 mg.

9. Calculation
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9.1 Calculate the amount of n-pentane insolubles, saturates, aromatics, and polar compounds in the sample as follows:
Saturates, mass % 5 ~B/A ! 3100 (1)
ASTM
Aromatics, massD2007-19
% 5 ~C/A ! 3100 (2)
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Polar compounds ~Note 9!, for 10 g sample 5 ~D/A ! 3100 (3)
Polar compounds, mass % for 5 g sample 5 @~0.88 3D/A ! # 3100 (4)

where:
A = grams of original sample used,
B = grams of residue from n-pentane effluent from the clay gel column (8.1.4),
C = grams of residue from the toluene desorption of the lower column and from the last n-pentane rinse of the columns (8.1.6
and 8.2.3), and
D = grams of residue from toluene-acetone effluent (8.1.8).
NOTE 9—The factor included in the calculation for the 5 g sample is established experimentally to maintain continuity of results over a wide range
of polar compounds in rubber extender oils.
9.2 If saturates, aromatics, and polars are all determined, the total mass of all the recovered fractions must equal at least 97 %
of the sample charged. If this recovery is not obtained, repeat the test.
9.3 If aromatics were not desorbed, use the n-pentane insolubles, saturates content, and polar compounds as determined in
Section 9, calculate the amount of aromatics as follows:
Aromatics, mass % 5 100 2 ~E1F ! (5)

where:
E = mass % saturates, and
F = mass % polar compounds.

10. Report
10.1 Report the following information:
10.1.1 Sample identification.