ASTM D2007-19(2024)e1
(Test Method)Standard Test Method for Characteristic Groups in Rubber Extender and Processing Oils and Other Petroleum-Derived Oils by the Clay-Gel Absorption Chromatographic Method
Standard Test Method for Characteristic Groups in Rubber Extender and Processing Oils and Other Petroleum-Derived Oils by the Clay-Gel Absorption Chromatographic Method
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.
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, health, and environmental practices and determine the 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 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.
General Information
Relations
Standards Content (Sample)
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.
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Designation: D2007 − 19 (Reapproved 2024)
Standard Test Method for
Characteristic Groups in Rubber Extender and Processing
Oils and Other Petroleum-Derived Oils by the Clay-Gel
Absorption Chromatographic Method
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.
ε NOTE—Editorially updated Terminology Section 3 in March 2024.
1. Scope 2. Referenced Documents
1.1 This test method covers a procedure for classifying oil 2.1 ASTM Standards:
samples of initial boiling point of at least 260 °C (500 °F) into D2226 Classification for Various Types of Petroleum Oils
the hydrocarbon types of polar compounds, aromatics and for Rubber Compounding Use
saturates, and recovery of representative fractions of these D4175 Terminology Relating to Petroleum Products, Liquid
types. This classification is used for specification purposes in Fuels, and Lubricants
rubber extender and processing oils. D5309 Specification for Cyclohexane 999
E691 Practice for Conducting an Interlaboratory Study to
NOTE 1—See Test Method D2226.
Determine the Precision of a Test Method
1.2 This test method is not directly applicable to oils of
greater than 0.1 % by mass pentane insolubles. Such oils can 3. Terminology
be analyzed after removal of these materials, but precision is
3.1 Definitions:
degraded (see Appendix X1).
3.1.1 For definitions of terms used in this test method, refer
1.3 The values stated in SI units are to be regarded as the to Terminology D4175.
standard. The values given in parentheses are for information 3.2 Definitions of Terms Specific to This Standard:
only. 3.2.1 The following terms refer to the hydrocarbon types
and structural groups as measured by this test method:
1.4 This standard does not purport to address all of the
3.2.2 aromatics, n—material that, on percolation, passes
safety concerns, if any, associated with its use. It is the
through a column of adsorbent clay in a n-pentane eluent but
responsibility of the user of this standard to establish appro-
adsorbs on silica gel under the conditions specified.
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use. 3.2.3 asphaltenes, or n-pentane insolubles, n—insoluble
Specific warning statements are given in 6.1, Section 7, A1.4.1, matter that precipitates from a solution of oil in n-pentane
and A1.5.5. under the specified conditions.
1.5 This international standard was developed in accor-
3.2.4 polar aromatics, n—synonym for polar compounds.
dance with internationally recognized principles on standard-
3.2.5 polar compounds, n—material retained on adsorbent
ization established in the Decision on Principles for the
clay after percolation of the sample in n-pentane eluent under
Development of International Standards, Guides and Recom-
the conditions specified.
mendations issued by the World Trade Organization Technical
3.2.6 saturates, n—material that, on percolation in a
Barriers to Trade (TBT) Committee.
n-pentane eluent, is not adsorbed on either the clay or silica gel
under the conditions specified.
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. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved March 1, 2024. Published April 2024. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1968. Last previous edition approved in 2019 as D2007 – 19. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D2007-19R24E01. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D2007 − 19 (2024)
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 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
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.
FIG. 1 Anticreep Beaker
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.
6.8 Round Bottom Flask, 3-necked, borosilicate, 500 mL
capacity (Fig. 3).
5. Significance and Use
6.9 Condenser, borosilicate (Fig. 3).
5.1 The composition of the oil included in rubber com-
3,4
6.10 Adapter Tube with Vigreux column (Fig. 3).
pounds has a large effect on the characteristics and uses of the
compounds. The determination of the saturates, aromatics, and 6.11 Flexible Joint, TFE-fluorocarbon and borosilicate,
4,5
24/40 T ground glass joints on each end.
polar compounds is a key analysis of this composition.
S
5.2 The determination of the saturates, aromatics, and polar
7. Reagents and Materials
compounds and further analysis of the fractions produced is
7.1 Purity of Reagents, Reagent grade chemicals shall be
often used as a research method to aid understanding of oil
used in all tests. Unless otherwise indicated, it is intended that
effects in rubber and other uses.
all reagents shall conform to the specifications of the commit-
tee on Analytical Reagents of the American Chemical Society,
6. Apparatus
where such specifications are available. Other grades may be
6.1 Beakers, Anticreep, 150 mL capacity, as illustrated in
used, provided it is first ascertained that the reagent is of
Fig. 1. (Warning—Beakers should be examined for sharp
sufficiently high purity to permit its use without lessening the
edges and fire polished, if necessary.)
accuracy of the determination.
6.2 Clay-Gel Column, constructed as illustrated in Fig. 2.
7.2 Acetone, reagent grade, minimum purity. (Warning—
6.3 Conical Flasks, (Erlenmeyer), 250 mL capacity. Acetone is extremely flammable.)
6.4 Solvent Receiver, capable of collecting solvent, without
7.3 Calcium Chloride, anhydrous granules.
splashing or loss of material during the analysis. A wide-
mouth, graduated, 500 mL capacity Erlenmeyer flask is one
The sole source of supply of the adapter tube known to the committee at this
such example that has been found suitable to use.
time is Owens Glass Apparatus, Inc., 128 River Road, Channelview, TX 77530. This
6.5 Filter Funnel, long stem; for use with 185 mm ready item can be fabricated at any scientific glassblowing shop.
If you are aware of alternative suppliers, please provide this information to
folded, fine-texture, rapid filter paper.
ASTM International Headquarters. Your comments will receive careful consider-
6.6 Separatory Funnel, 500 mL. ation at a meeting of the responsible technical committee, which you may attend.
Cole Parmer No. 6675-40 has been found suitable for this purpose.
6.7 Hot Plate, explosion proof, controlled to a surface
ACS Reagent Chemicals, Specifications and Procedures for Reagents and
temperature of 100 °C to 105 °C. Standard-Grade Reference Materials, American Chemical Society, Washington,
DC. For suggestions on the testing of reagents not listed by the American Chemical
NOTE 2—Temperatures should be uniform on the top of the hot plate.
Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,
Some laboratory hot plates benefit by the inclusion of an aluminum plate, U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma-
approximately 6 mm thick, included under or on top of regular plate top. copeial Convention, Inc. (USPC), Rockville, MD.
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D2007 − 19 (2024)
NOTE 1—Check to ascertain ID is 44 mm.
FIG. 2 Clay-Gel Percolating Column
7.4 Clay Adsorbent, 500 μm to 250 μm (30 mesh to
Sieve analysis >30 sieve size, 5 % (mass) maximum;
4,7
>50 sieve size, 45 % (mass) min
60 mesh) Attapulgus. Clay quality may be determined using
>100 sieve size, 80 % (mass) min
the azobenzene equivalence test shown in Annex A1. The
>200 sieve size, 94 % (mass) min
azobenzene activity test measures the adsorptive characteristics
7.7.1 Gel should be activated for 4 h in an air oven at
of the clay. Azobenzene equivalence value should be 30 to 35.
190 °C in a shallow pan.
Clay outside of these limits should be discarded.
7.8 Toluene, reagent grade minimum purity. (Warning—
7.5 Cyclohexane, conforming to Specification D5309.
Toluene is flammable. Vapor harmful.)
(Optional, see 8.1.9.) (Warning—Cyclohexane is extremely
7.9 Toluene-Acetone Mixture (50 to 50 by volume), mix
flammable. Harmful if inhaled.)
equal volumes of toluene and acetone.
7.6 Pentane, 99.0 % minimum purity. (Warning—
7.10 In order to obtain results that are consistent with those
n-Pentane is extremely flammable. Harmful if inhaled.)
obtained elsewhere, it is very important that only the reagents
7.7 Silica Gel, activated, conforming to the following
and materials described in this section be used.
4,8
inspections:
8. Procedure
The sole source of supply of clay adsorbent known to the committee at this time
8.1 Fractionation:
is Forcoven Products, 22010 East Martin Dr., Porter, TX 77365. Packaged in
8.1.1 Prepare the adsorption column (Fig. 2) by placing
moisture resistant twinned packets of 50 and 100 g (sufficient for one determina-
100 g of clay adsorbent in the upper section of the column and
tion). These packets are packed 50 sets per case. It is important that extremes of
temperature be avoided on stored clay samples.
200 g of silica gel plus 50 g of clay on top of the gel in the
The sole source of supply of silica gel meeting these specifications known to
lower section (Note 5). Place a piece of glass wool (of about
the committee at this time is Forcoven Products, 22010 East Martin Dr., Porter, TX
25 mm loose thickness) over the top surface of the clay in the
77365, packaged in 200 g moisture resistant packets. Sieve analysis should be
checked on other sources of gel. upper column to prevent agitation of the clay while charging
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D2007 − 19 (2024)
not greater than 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. Partition-
ing between aromatics and polar 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. Cyclo-
hexane used 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 of the column above the clay free of
sample with n-pentane. The sample and eluent solvent can be
added to the column through 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 300 mL of the first
n-pentane effluent from the column in 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
FIG. 3 Extraction Apparatus
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
the eluent solvents. Join the columns (clay over gel) after
section with n-pentane. Maintain a moderate liquid head level
lubricating the joint with hydrocarbon-insoluble grease. It is
above the clay during this wash and adjust n-pentane additions
important that the adsorbents in each column be packed to a
so that the level is about 25 mm when 150 mL have been
constant level. A minimum of ten taps with a soft rubber
collected in the receiver. Discontinue additions at this point and
hammer at different points up and down and 25 taps on top of
allow the liquid to essentially drain from the column. The
each column should be employed to achieve constant level. A
quantity in the receiver should then be about 200 mL. The
suitable rubber hammer may be assembled by fastening two
n-pentane from this step and from the draining of the lower
No. 7 or 8 rubber stoppers on one end of a small rod about
column should be discarded if aromatics are to be determined
200 mm long. Use fresh adsorbents for each determination.
by difference. This n-pentane should be added to the aromatics
8.1.2 If n-pentane insolubles were not determined, select the
soluti
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