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: D2414 − 21

Standard Test Method for

Carbon Black—Oil Absorption Number (OAN)1
This standard is issued under the fixed designation D2414; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.

1. Scope Gravity of Liquids by Digital Density Meter

1.1 This test method covers the determination of the oil D4483 Practice for Evaluating Precision for Test Method
absorption number of carbon black. Standards in the Rubber and Carbon Black Manufacturing
Industries
1.2 The values stated in SI units are to be regarded as the D4821 Guide for Carbon Black—Validation of Test Method
standard. The values given in parentheses are for information Precision and Bias
only. D5554 Test Method for Determination of the Iodine Value of
1.3 This standard does not purport to address all of the Fats and Oils
safety concerns, if any, associated with its use. It is the 2.2 DIN Standards:3
responsibility of the user of this standard to establish appro- DIN 16945 Testing of resins, hardeners and accelerators, and
priate safety, health, and environmental practices and deter- catalyzed resins
mine the applicability of regulatory limitations prior to use. DIN EN ISO 660 Animal and vegetable fats and oils -
1.4 This international standard was developed in accor- Determination of acid value and acidity
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the 3. Summary of Test Method
Development of International Standards, Guides and Recom- 3.1 In this test method, oil is added by means of a
mendations issued by the World Trade Organization Technical constant-rate buret to a sample of carbon black in the mixer
Barriers to Trade (TBT) Committee. chamber of an absorptometer. As the sample absorbs the oil,
the mixture changes from a free-flowing state to one of a
2. Referenced Documents semiplastic agglomeration, with an accompanying increase in
2.1 ASTM Standards:2 viscosity. This increased viscosity is transmitted to the torque-
D445 Test Method for Kinematic Viscosity of Transparent sensing system of the absorptometer. When the viscosity of the
and Opaque Liquids (and Calculation of Dynamic Viscos- mixture reaches a predetermined torque level, the absorptom-
ity) eter and buret will shut off simultaneously. The volume of oil
D1218 Test Method for Refractive Index and Refractive added is read from the direct-reading buret. The volume of oil
Dispersion of Hydrocarbon Liquids per unit mass of carbon black is the oil absorption number.
D1765 Classification System for Carbon Blacks Used in 3.2 Either DBP, paraffin or Epoxidized Fatty Acid Ester
Rubber Products (EFA) oils are acceptable for use with most standard pelleted
D1799 Practice for Carbon Black—Sampling Packaged grades of carbon black including N-series carbon blacks found
Shipments in Classification D1765. OAN testing using paraffin or EFA
D1900 Practice for Carbon Black—Sampling Bulk Ship- oils on some standard blacks and specialty blacks including
ments powder products may result in unacceptable differences as
D4052 Test Method for Density, Relative Density, and API compared to OAN testing with DBP oil. Paraffin and EFA oils
are considered non-hazardous; some paraffin oils are FDA
1
This test method is under the jurisdiction of ASTM Committee D24 on Carbon
approved. For any of the oils, Sections 8 – 12 (Calibration,
Black and is the direct responsibility of Subcommittee D24.11 on Carbon Black Procedure, Calculation, and Report) are to be consistent with
Structure. the oil selected for use. Referee testing between suppliers and
Current edition approved June 1, 2021. Published July 2021. Originally approved users should use DBP oil until such time that precision data are
in 1965. Last previous edition approved in 2019 as D2414 – 19. DOI: 10.1520/
D2414-21. available for alternate oils.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
3
Standards volume information, refer to the standard’s Document Summary page on Available from Deutsches Institut fur Normung e.V.(DIN), Burggrafenstrasse 6,
the ASTM website. 10787 Berlin, Germany, http://www.din.de.

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

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 D2414 − 21
4. Significance and Use 8. Oil Absorptometers, Instrument Calibration, and End-
4.1 The oil absorption number of a carbon black is related to Point Procedures
the processing and vulcanizate properties of rubber compounds 8.1 Absorptometer:
containing the carbon black. 8.1.1 Model—Three different types of absorptometers are in
use: (1) early models based on springs and mechanical indica-
5. Apparatus4 tion of torque (Type A and B), (2) second generation absorp-
5.1 Balance, analytical, with an 0.01-g sensitivity. tometers equipped with load cells and digital torque display
(Type E7), and (3) current model absorptometers which are
5.2 Oven, gravity-convection type, capable of maintaining designed with a torque measuring system that includes a
125° 6 5°C. micro-computer and software to continuously record torque
5.3 Spatula, rubber, 100-mm. and oil volume with time (Types H and C and modified Type
E7). Types A, B, and E7 are designed to stop mixing at a
5.4 Absorptometer, equipped with a constant-rate buret that
predetermined, fixed torque level, which is the recommended
delivers 4 6 0.024 cm3/min.
procedure for measuring hard or tread blacks (calibration
5.5 Desiccator. Procedure A). The computer controlled models (Types H and C
and modified Type E7) absorptometers can provide an end-
6. Reagent and Standards point at a fixed or predetermined torque level such that these
6.1 Purity of Reagents—Reagent grade chemicals shall be types of absorptometers are well-suited for measuring OAN of
used in all tests. Unless otherwise indicated, it is intended that all types of carbon blacks.
all reagents shall conform to the specifications of the Commit- 8.1.2 Mixing Bowl—Typically the absorptometer is deliv-
tee on Analytical Reagents of the American Chemical Society, ered with either a surface-treated stainless steel or anodized
where such specifications are available.5 Other grades may be aluminum mixing bowl. These bowls are considered accept-
used, provided it is first ascertained that the reagent is of able provided they give the correct reading for the appropriate
sufficiently high purity to permit its use without lessening the SRB reference standards. The surface finish of the mixer
accuracy of the determination. chamber is critical for maintaining proper calibration, and the
bowl should not be modified to achieve calibration.
6.2 n-Dibutyl Phthalate, having a density of 1.042 to 1.047
Mg/m3 at 25°C and a relative density of 1.045 to 1.050 at 25°C. NOTE 2—Stainless steel chambers have been found satisfactory for the
test when they are manufactured to a roughness value (Ra) of 2.5 6
6.3 Paraffın Oil, having a kinematic viscosity of 10 to 0.4 µm (100 6 15 µin.) based upon 8 measurements. No single measure-
34 mm2/s (cSt) at 40°C. ment should be greater than 3.6 µm (140 µin.) or less than 1.5 µm (60
µin.). Stainless steel bowls purchased with an absorptometer have been
NOTE 1—Three paraffin oils have been found suitable including Marcol pre-polished for 16 h to minimize bowl surface changes affecting
82 from Exxon, 80/90 White Oil from Conoco-Phillips, and LC1 oil from calibration during their initial use. It is recommended that new replace-
Lab Chemicals, Germany. All three oils are pharmaceutical or food grade ment stainless steel bowls should also be pre-polished in the same manner
oil, or both, based on available data. (see Annex A3).
6.4 Epoxidized Fatty Acid Ester (EFA), meeting the speci- 8.2 Instrument Calibration—Several components influence
fications listed in Annex A4. It is recommended to store the the calibration: the dynamometer torque spring or the load cell,
product at temperatures between 7 and 30°C. If stored in sealed the torque limit switch or the indicator set point, the damper
original containers, the product is stable for at least 12 months. (oil damper or electronic damping), and the mixing head
For handling and safety, please refer to safety data sheet. consisting of two counter rotating blades and a mixing bowl. It
6.5 ASTM D24 Standard Reference Blacks, SRB.6 is necessary that all of these components are in good condition
and are properly adjusted to achieve acceptable calibration.
7. Sampling 8.2.1 Rotor Blades—The speed of the motor driving the
rotor blades is either fixed (Type A and B) or has to be set
7.1 Samples shall be taken in accordance with Practices (Type E, C, and H) to 125 r/min. Due to a gear, one blade spins
D1799 and D1900. at 125 r/min, the other blade at 250 r/min.
8.2.2 Constant-Rate Buret—The delivery rate of the buret is
to be 4 cm3/min. See Annex A1 for detailed instructions on the
4
All apparatus are to be operated and maintained in accordance with the procedure for calibration check of the constant-rate buret.
manufacturers’ directions for optimum performance. 8.2.3 Spring Tension (Type A and B)—It is recommended
5
Reagent Chemicals, American Chemical Society Specifications , American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
that the torque spring is adjusted so that the SRB F standard
listed by the American Chemical Society, see Analar Standards for Laboratory will develop a maximum torque between 70 % and full-scale
Chemicals, BDH Ltd., Poole, Dorset, U.K. and the United States Pharmacopeia and deflection. This is achieved by selecting the appropriate spring
National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD. strength and adjusting the spring tension in accordance with the
6
The sole source of supply of ASTM Standard Reference Blacks known to the instructions of the manufacturer.
committee at this time is Laboratory Standards and Technologies, 227 Somerset,
Borger, TX 79007, http://carbonstandard.com/. If you are aware of alternative
suppliers, please provide this information to ASTM International Headquarters.
7
Your comments will receive careful consideration at a meeting of the responsible Type E absorptometers can be modified with additional hardware and micro-
technical committee,1 which you may attend. computer system.

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 D2414 − 21
NOTE 3—The absorptometers Type E, C, and H are calibrated by the 9.4 For a tread or carcass-type normalization curve, because
manufacturer to give a direct reading of torque in mNm; this calibration of the differing grades in SRB series and material ages, all
should not be modified in order to achieve a desired level of torque. If
calibration is necessary, refer to the instrument manufacturer’s recommen-
three SRBs should normally be from the same series (example:
dations. The instrument torque calibration should not be confused with the series-9). However, when the normalization range provided by
torque limit switch described in 8.3.1. a given SRB set does not cover the normalization range
8.2.4 Damper—For the Type A absorptometer, it is recom- needed, follow Guide D4821 Subsection 8.2 to choose the
mended to keep the valve of the oil damper fully closed. The proper alternative SRB material to be used in the normalization
Type B absorptometer shall provide a full-scale recovery of 3 curve.
6 0.5 s; the valve has to be adjusted accordingly. The Type E NOTE 4—When only tread- or carcass-type carbon blacks are to be
absorptometer has an electronic damping option and Types C tested, the normalization can be limited to either the three tread SRBs
and H have appropriate software damping. Make sure that (example: 9A, 9B, 9C for typical OAN levels or 9A, 9C, 9H for high OAN
these damping options are activated. levels > 125 10–5 m3/kg (cm3/100 g)) or the three carcass-type SRBs
(example: 9D, 9E, 9F).
8.2.5 Stainless Mixing Bowls—When replacing an old mix-
ing bowl with a new one, further pre-polish may be needed 9.5 Perform a regression analysis using the standard value
after installation even if those mixing bowls are typically of the standard (y value) and the rolling average measured
already pre-polished by the manufacturer. The surface finish of value (x value). Separate carcass and tread normalization
the mixer chamber is critical for maintaining proper curves should be maintained.
calibration, and the bowl shall not be modified to achieve 9.6 Normalize the values of all subsequent samples using
calibration other than described in Annex A3. the regression equation as follows:
8.3 End-Point Procedures: Normalized value 5 ~ measured value*slope! 1intercept (1)
8.3.1 Torque Limit Switch (TLS) or the Indicator Set
9.7 For normalized values of the SRBs that are consistently
Point—If the end-point of the test is determined by a fixed
outside the x-chart limits listed in Guide D4821, the instrument
torque limit, the setting of the TLS, also called indicator
calibration and end-point procedures in Section 8 should be
set-point, has to be selected using one of the following three
reviewed.
procedures:
8.3.1.1 Procedure A: End-Point at Fixed Torque Level— 9.8 When any absorptometer or calibration changes occur, a
This “classical” method is well suited for most hard or tread new normalization curve must be initiated as described in
blacks but may lead to problems when low-torque carcass Section 9.
blacks are to be tested; proceed to Procedure B for low-torque 9.9 In most instances, if normalized values of the SRB’s are
carbon blacks. For Type A, B, and E absorptometers, adjust the not within x-chart limits provided in Guide D4821, and the
TLS or the indicator set point in such way that the current SRB normalizations are current, it will be necessary to replace the
F standard gives the correct target value within the limits as mixer chamber with one of proper surface finish. Review
defined in Guide D4821. For Type E, C, and H absorptometers Appendix X1.
dedicated to testing tread blacks only, there is no advantage to
setting the TLS based on the SRB F standard; for these 10. Procedure
absorptometers, set the TLS to 3500 mNm for DBP oil, or 4000
10.1 Dry an adequate sample for 1 h in the specified oven
mNm for paraffin oil.
set at 125°C. Prior to testing, cool the sample in a desiccator for
8.3.1.2 Procedure B: End-Point at 70 % of the Maximum
a minimum of 30 min.
Torque—Certain carcass blacks and thermal blacks may fail to
give an end-point due to insufficient torque level. Therefore, 10.2 Weigh the sample to the nearest 0.01 g. The recom-
the preferred method for testing soft blacks is to record the mended masses are as follows:
torque curve using a chart-recorder or a data acquisition system Carbon Black Mass, g
and to read the end-point at 70 % of the maximum of the torque N630, N642, and N700 series, except N765 25
N800 and N900 series, SRB-9D 40
achieved. Set the TLS or the indicator set point to full scale in All others 20
order to disable the automatic shut-off of the absorptometer.
10.3 It is recommended that a testing temperature of 23 6
9. Normalization using Standard Reference Blacks (SRB) 5°C be maintained, as measured by a thermocouple in the
9.1 Physically calibrate the test apparatus including TLS mixing bowl. If a temperature controllable mixing bowl is not
adjustment using the instructions in 8.3. available, keep the bowl temperature below 30°C and comply
with Note 5 and Note 6 while running the samples.
9.2 Test the six ASTM Standard Reference Blacks (SRBs)
in duplicate to establish the average measured value. Addi- NOTE 5—If the absorptometer has remained idle for more than 15 min
tional values are added periodically, typically on a weekly and a temperature controllable bowl is not being used, a 10-min warm-up
sample must be run before beginning a test. It is important that the mixer
basis. An alternative to periodic normalizations are daily chamber temperature be kept uniform. Preferably, allow 5 min between
additions of SRB normalization tests such that the normaliza- the end of one test and the start of another.
tion curve is continuously maintained. The rolling average of NOTE 6—It is important that the temperature of the bowl be the same for
the measured values is computed from the latest four values. machine calibration as for oil absorption testing. ASTM task group work
has shown that an increase in bowl temperature can cause higher values
9.3 For a tread or carcass-type normalization curve, all three that increased variability in bowl temperatures cause increased test
SRBs should be included. variability.

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 D2414 − 21
10.4 Transfer the sample to the absorptometer mixer cham- disassembly, and the use of the preset cleanup cycle for Types
ber and replace the chamber cover. For Type H, close the safety E, C, and H (use of water to aid cleanup is not recommended).
door surrounding the mixing chamber. NOTE 8—It is not necessary to clean and polish the mixing blades and
10.5 Position the buret delivery tube over the hole in the chamber with a solvent, but it is recommended to remove all visible
mixer chamber cover, and for Types A, B, or E set the buret residues by wiping the chamber and mixing blade surfaces.
digital counter to zero (Types C and H have automatic reset). 11. Calculation
Insure the buret delivery tubes have no air bubbles.
11.1 Calculate the oil absorption number of the sample, to
10.6 Activate the “start” button. On the Type E the nearest 0.1 10–5m3/kg (cm3/100 g) as follows:
absorptometer, activate both “start” buttons simultaneously.
The apparatus will operate until one of the following condi-
tions are met: 1) sufficient torque has developed to activate the
Oil absorption number, 1025 m 3 /kg 5 H A
B J
3 100 3 C 1D (2)

torque-limit switch, which will halt the absorptometer and where:

buret; 2) the sample torque has reached a maximum and then A = volume of oil used, cm3,
dropped below maximum torque for a preset period of time B = mass of tested sample, g,
(using Procedure B). C = slope of normalization curve (see Section 9), and
NOTE 7—In the event that an endpoint is not obtained (maximum torque D = y-intercept of normalization curve (see Section 9).
< TLS) when using an absorptometer with a fixed TLS such as Type B or
E, it is acceptable to mill pelleted carbon blacks using a coarse grinder 12. Report
such as a coffee mill. The carbon black should be milled for only a few
seconds to allow sufficient grind time to change the pellets to powder
12.1 Report the following information:
form. High-speed micronizing mills and air-jet mills are not acceptable, as 12.1.1 Proper identification of the sample,
they can reduce the carbon black structure. 12.1.2 Oil (DBP, paraffin, or EFA),
10.7 For Type B and E oil absorptometers, record the 12.1.3 Method for end-point determination (Procedure A, B
volume of oil used as indicated by the buret digital counter. For or C in 8.2),
Type C and H oil absorptometers, the normalized OAN test 12.1.4 Sample mass, if different than shown in 10.2, and
results are obtained directly from the instrument software. A 12.1.5 The result obtained from the individual determina-
summary of recommended end-point type is shown below for tion is reported to the nearest 0.1 10−5m3/kg (cm3/100 g).
the two general types of carbon black:
13. Precision and Bias
Recommended End-Point Procedure and Results
End-Point 13.1 These precision statements have been prepared in
CB Type Result*
Procedure accordance with Practice D4483-99. Refer to this practice for
Hard/Tread A Normalized
Soft/Carcass B Normalized
terminology and other statistical details.
*OAN test results should always be normalized to standard reference blacks 13.2 Interlaboratory precision program (ITP) information
(SRB) when reported.
was conducted as detailed in Table 1. Both repeatability and
10.8 Dismantle the mixer chamber and clean the mixing reproducibility represent short-term (daily) testing conditions.
blades and chamber with a rubber spatula and reassemble. The testing was performed using two operators in each
10.9 Mixing chamber cleanup can be aided by the addition laboratory performing the test once on each of two days (total
of dry carbon black to the mixing chamber prior to of four tests). A test result is the value obtained from a single

TABLE 1 Precision Parameters for Test Method D2414, Method N/A (Type 1 Precision)A
Units 10−5 m3/kg (cm3/100 g)
Number of
Laborato-
ries
Mean
Material Period (M/H/L)B Sr r (r) SR R (R)
Level
SRB-9A Mar 2013 77(0/1/1) 71.5 0.47 1.33 1.9 1.55 4.38 6.1
SRB-9B Mar 2016 87(0/2/0) 98.9 0.40 1.14 1.1 1.11 3.14 3.2
SRB-9D Mar 2018 75(2/2/1) 34.5 0.25 0.72 2.1 0.72 2.03 5.9
SRB-9E Aug 2016 81(1/3/0) 89.2 0.44 1.24 1.4 0.89 2.53 2.8
SRB-9F Mar 2015 74(1/0/0) 134.5 0.53 1.51 1.1 1.59 4.51 3.3
SRB-9G Aug 2017 74(0/2/1) 38.6 0.23 0.64 1.7 1.76 4.98 12.9
SRB-9C Aug 2019 79(1/2/0) 124.4 0.44 1.24 1.0 1.23 3.49 2.8
SRB-9A2 Aug 2018 76(0/2/0) 71.4 0.34 0.97 1.4 1.18 3.34 4.7
Mar/Apr
SRB-9H 74(1/1/0) 178.3 0.57 1.63 0.9 1.92 5.43 3.0
2020
Average 94.0
Pooled Values 0.42 1.19 1.3 1.38 3.90 4.1
A
Preferred precision shown in bold text.
B
M = number of outliers for Mean; H = number of outliers for High variation; L = number of outliers for Low variation.

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 D2414 − 21
determination. Acceptable difference values were not mea- significant difference in the two materials, samples, and so forth, which
sured. The between operator component of variation is in- generated the two test results.
cluded in the calculated values for r and R. 13.5 Reproducibility—The pooled reproducibility, R, of
this test method has been established as 3.90 10–5 m3/kg
13.3 The precision results in this precision and bias section
(cm3/100 g). Any other value in Table 1 may be used as an
give an estimate of the precision of this test method with the
estimate of reproducibility, as appropriate. The difference
materials used in the particular interlaboratory programs de-
between two single and independent test results found by two
scribed in 13.2. The precision parameters should not be used
operators working under the prescribed reproducibility condi-
for acceptance or rejection testing of any group of materials
tions in different laboratories on identical test material will
without documentation that they are applicable to those par-
exceed the reproducibility on an average of not more than once
ticular materials and the specific testing protocols of the test
in 20 cases in the normal and correct operation of the method.
method. Any appropriate value may be used from Table 1.
Two single test results produced in different laboratories that
13.4 Repeatability—The pooled repeatability, r, of this test differ by more than the appropriate value from Table 1 must be
has been established as 1.19 10–5 m3/kg (cm3/100 g). Any other suspected of being from different populations and some appro-
value in Table 1 may be used as an estimate of repeatability, as priate investigative or technical/commercial action taken.
appropriate. The difference between two single test results (or 13.6 Bias—In test method terminology, bias is the difference
determinations) found on identical test material under the between an average test value and the reference (true) test
repeatability conditions prescribed for this test will exceed the property value. Reference values do not exist for this test
repeatability on an average of not more than once in 20 cases method since the value or level of the test property is
in the normal and correct operation of the method. Two single exclusively defined by the test method. Bias, therefore, cannot
test results that differ by more than the appropriate value from be determined.
Table 1 must be suspected of being from different populations
and some appropriate action taken. 14. Keywords
NOTE 9—Appropriate action may be an investigation of the test method 14.1 carbon black; epoxidized fatty-acid ester (EFA);
procedure or apparatus for faulty operation or the declaration of a n–dibutyl phthalate; oil absorption number; paraffin oil

ANNEXES

(Mandatory Information)

A1. CALIBRATION CHECK OF CONSTANT-RATE BURET

A1.1 Scope A1.3.3 With the buret completely full, set the stopcock to
A1.1.1 The constant-rate buret is an integral part of the the delivery position. Run the buret on “deliver” until a
absorption-measuring system. Failure of the buret to deliver constant flow is obtained from the delivery tube.
the specified amount of reagent to the carbon black will result A1.3.4 Stop the buret and set the digital counter to zero.
in erroneous absorption readings. This annex provides a A1.3.5 Position a tared 150-cm3 beaker under the delivery
method for checking the delivery rate of the constant-rate tube.
buret. One of the reasons for the incorrect absorption values
(caused by incorrect reagent delivery by the automatic buret) is A1.3.6 Simultaneously start the buret and stop watch.
entrapped air in the plastic tubing or the delivery tube, A1.3.7 After 2 min, stop the buret and record the digital
especially above the nozzle. This trouble source should be counter reading.
checked first.
A1.3.8 Weigh and record the amount of reagent delivered.
A1.2 Apparatus A1.3.9 Refill the buret.
A1.2.1 Stop Watch. A1.3.10 Repeat A1.3.3 – A1.3.9, changing the delivery time
A1.2.2 Beaker, 150-cm3. in A1.3.7 to 4 and 8 min.

A1.3 Procedure A1.4 Calculation

A1.3.1 Ensure that all seals and tubing are in good condi- A1.4.1 Calculate the volume of oil from the delivered mass
tion. and density (A1.3.8) as follows:
A1.3.2 Fill the buret and delivery tubes with oil. Ensure that mass delivered
Delivery, cm3 5 (A1.1)
all air is removed from the system. oil density

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A1.5 Acceptable Results A1.6.2 Variation in oil density has been observed between
different labs and lots of oil. typical DBP density at 23°C was
A1.5.1 The calculated delivery should be within the follow-
observed to vary from 1.044 to 1.050 g/cm3, and typical
ing limits of the digital counter reading:
Marcol 82 density at 23°C was observed to vary from 0.843 to
Time, min Volume, cm3 Tolerance, cm3
2 8 ±0.05
0.846 g/cm3. Until further guidelines are made available by
4 16 ±0.10 D24, it is an acceptable practice to utilize an average density
8 32 ±0.20 value from Table A1.1, or either lot data at a specified
A1.6 Oil Density temperature.
A1.6.3 Selection of the appropriate oil density from Table
A1.6.1 Oil density is necessary to calculate the volume of
A1.1 is dependent on the temperature of the oil in use. It is
oil delivered from a buret as described in A1.4. Oil densities
suggested that a temperature measurement be made on the oil
may be analyzed using calibrated hydrometers or density
in the buret reservoir, and the appropriate density used in A1.4.
meters at specified temperatures. Typical densities for both
DBP and paraffin oil have been obtained from different A1.6.4 Conoco-Phillips 80/90 White Oil density is reported
laboratories measuring different lots of oils as shown in Table at 15.6°C (60°F) as 0.855 g/cm3; LC1 oil density is reported at
A1.1. EFA oil densities were obtained from the vendors 15°C (59°F) as 850 kg/m3 (0.85 g/cm3).
technical data and other laboratory measurements. A1.6.5 Epoxidized sunflower oil density is reported at 20°C
NOTE A1.1—New oil densities will be added to Table A1.1 as as 0.900 to 0.910 g/cm3. Additional density data at three
alternative oils are identified and demonstrated as suitable for OAN temperatures was reported as follows: 20.0°C as 0.9033 g/cm3,
testing, and as density data are made available to D24. 25.0°C as 0.8998 g/cm3, and 30.0°C as 0.8933 g/cm3.

TABLE A1.1 Oil Density

Typical DBP Oil Density Typical Marcol 82 Paraffin Oil Density
Temp °C Lab 1 g/cm3 Lab 2 g/cm3 Average g/cm3 Lab 1 g/cm3 Lab 2 g/cm3 Average g/cm3
20.0 1.052 1.047 1.049 0.845 0.848 0.846
21.0 1.051 1.046 1.049 0.844 0.847 0.846
22.0 1.050 1.045 1.048 0.844 0.846 0.845
23.0 1.050 1.044 1.047 0.843 0.846 0.844
24.0 1.049 1.043 1.046 0.842 0.845 0.844
25.0 1.048 1.043 1.045 0.841 0.844 0.843
26.0 1.047 1.042 1.044 0.841 0.844 0.842
27.0 1.046 1.041 1.044 0.840 0.843 0.842
28.0 1.046 1.040 1.043 0.839 0.842 0.841
29.0 1.045 1.039 1.042 0.839 0.842 0.840
30.0 1.044 1.038 1.041 0.838 0.841 0.840

A2. DETERMINATION OF MAXIMUM TORQUE

A2.1 Scope A2.2 Procedure

A2.1.1 On some instruments the SRB F (N683) will not A2.2.1 Set the torque pointer to 10 on the Set Scale. For
develop sufficient torque to produce acceptable test precision. Type E absorptometers, move the shut-off alarm set point to
This is an indication that other similar type carbon blacks may maximum scale. This makes 100 % of the torque range
also test with poor precision. available.
A2.1.2 In order to obtain acceptable test precision in these
situations, it is necessary that the absorptometer be adjusted NOTE A2.1—Torque limit switch settings should always be made with
the instrument stopped and the mixing chamber empty.
mechanically or electronically for Type E absorptometers so
that the SRB F will develop a maximum torque of at least 70 % A2.2.2 Start the apparatus having followed 10.1 – 10.6 for
of full scale. This procedure gives the needed instructions to testing SRB F.
determine the maximum torque developed by a carbon black
sample.

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A2.2.3 As the sample begins to develop viscosity and the T max 5 ~ 10 2 N min! 3 10 (A2.1)
torque increases, the pointer will move down the scale towards where:
zero. The maximum % torque, Tmax, developed by the sample
is as follows: Nmin = the lowest pointer reading.

A3. PRE-POLISHING PROCEDURE FOR NEW REPLACEMENT STAINLESS STEEL BOWLS

A3.1 Scope A3.3 Procedure

A3.1.1 New stainless steel absorptometer mixing bowls are A3.3.1 Weigh 25 g of SRB F carbon black and transfer this
typically pre-polished by the manufacturer such that they will sample into the absorptometer mixing chamber.
meet the required tolerances of the SRB’s once a normalization A3.3.2 Turn on the absorptometer and add 35 cc of oil.
curve has been prepared. When normalized OAN results do not
NOTE A3.1—Depending on the instrument model, it may be necessary
meet the tolerances stated in Guide D4821, and the non- to relieve the torque limit switch to prevent automatic shutoff; and it may
normalized SRB F (N683) is more than 3 to 4 cm3/100 g less be necessary to increase the spring tension.
than the target value, it is recommended to pre-polish the bowl.
A3.3.3 Allow the absorptometer to run continuously for the
Pre-polishing will increase the non-normalized OAN of the
desired time period. It is recommended to check the SRB F
SRB F.
non-normalized OAN value every 3 to 4 h of pre-polishing.
A3.1.2 The length of the pre-polish procedure depends on The mixing bowl must be cooled to room temperature prior to
how much change is required. For only 1 to 2 units of increase checks with the SRB F.
in OAN, pre-polishing of 4 h should be followed by a
NOTE A3.2—The absorptometer bowl must be securely covered during
measurement of the SRB F to determine the non-normalized this time to prevent the loss of sample to be able to achieve adequate
OAN. If the value has not sufficiently changed, continue pre-polishing action.
pre-polishing until the desired change is achieved. A non- A3.3.4 After pre-polishing, stop the absorptometer, empty
normalized value for the SRB F that is 3 to 4 units less than the sample, and clean the mixing chamber and blades. Allow
target is desirable for a new bowl. Non-normalized OAN value the chamber to cool to room temperature. If the SRB F check
increases of more than 1 to 2 units may require as much as 8 is within the expected range proceed to A3.3.5; if not, resume
to 16 h of pre-polishing. pre-polish described in A3.3.1.
A3.2 Reagents A3.3.5 Check and adjust the torque-switch setting and,
depending on instrument type, the spring tension before
A3.2.1 Carbon Black (SRB F - N683 type).
proceeding with normalization following the standard testing
A3.2.2 n-Dibutyl Phthalate, Paraffın Oil, or EFA Oil. procedure.

A4. EPOXIDIZED FATTY ACID ESTER (EFA) OIL SPECIFICATION

A4.1 See Table A4.1.

TABLE A4.1 Specifications of EFA Oil For Use in OAN/COAN Test

Test Method Units Min. Max.
Refractive index (20°C) ASTM D1218 nD20 1.4530 1.4590
Acid number DIN EN ISO 660 mg KOH/g 0.0 3.0
Iodine number ASTM D5554-95 gI2/100g 0.0 5.0
Epoxy oxygen content DIN 16945 wt. % 3.5 4.5
Density (20°C) ASTM D4052 g/cm3 0.900 0.920
Viscosity, kinematic (40°C) ASTM D445 mm2/s 10.0 30.0

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APPENDIX

(Nonmandatory Information)

X1. DIAGNOSTIC PROCEDURES FOR MONITORING OAN MIXING CHAMBERS

X1.1 Scope X1.3.2 SRB F non-normalized OAN values for a new

X1.1.1 Diagnostic procedures for monitoring the condition mixing bowl which has been prepolished from the manufac-
of a mixing bowl surface when using DBP, paraffin, or EFA oils turer should be approximately 3 to 4 cm3/100 g less than target.
are described in X1.2 and X1.3, and an assessment of the New chambers always give non-normalized OAN measure-
mixing chamber mechanical operation in X1.4. For oil absorp- ments low versus target. If the non-normalized value is outside
tometers used to measure the OAN of carcass or soft grades (or the 3 to 4 cm3/100 g less than target, the chamber should
other non-reinforcing carbon blacks), the mixing bowl surface undergo further pre-polishing.
must be monitored to insure it is capable of producing X1.3.3 As the mixing bowl is used the raw or measured
acceptable OAN data. This criterion does not apply to tread or SRB F OAN will slowly increase. When the SRB F raw or
hard blacks (that is, reinforcing carbon blacks). measured OAN value is 3 to 4 cm3/100 g greater than target the
X1.1.2 Diagnostic procedures for determining the condition mixing chamber should be evaluated for replacement.
of an OAN mixing bowl have been developed based on the
X1.4 Determining the Mechanical Condition of an OAN
characteristics of SRB F (N683). For an oil absorptometer
Mixing Chamber
system in good condition, the typical maximum torque level
for SRB F is approximately 4500 to 5000 mNm. A typical X1.4.1 An OAN mixing chamber consists of two major
torque value at 70 % of maximum torque is 3500 to 4000 components including a mixing bowl and a mixing drive. A
mNm. mixing drive includes a back-plate, two rotors, bushings,
bearings, gear drive, etc. The back-plate and rotors are typi-
NOTE X1.1—An OAN mixing chamber consists of two major compo- cally constructed of either stainless steel or aluminum.
nents including a mixing bowl and a mixing drive. Often a worn mixing
bowl can be replaced with just a replacement mixing bowl. The mixing X1.4.2 Aluminium mixing bowls typically have an anod-
drive should also be evaluated for mechanical condition as described in ized surface treatment or hardcoat finish. Once the finish is
X1.4.
visibly worn off of an aluminum mixing bowl it should be
replaced. Components which are physically damaged should
X1.2 Monitoring Mixing Chamber Surface Conditions
be replaced. The mixing bowl should be removed and the drive
Using Measured TLS
components inspected. Bushings can be inspected by applying
X1.2.1 For absorptometers which are setup for “Measured side-to-side force to the rotors to check for excessive move-
TLS,” monitor the TLS value of SRB F using an x-chart. The ment.
definition of TLS or torque limit switch is the torque at which X1.4.3 A diagnostic measurement used to assess and moni-
the SRB F equals the specified target value in cm3/100g as tor the general condition of the mixing drive bearings and
found in Guide D4821. For modern instruments, the TLS value rotors is to monitor the idle torque. This is accomplished by
can be measured by the instrument software. first ensuring the mixing chamber has been thoroughly cleaned,
X1.2.2 TLS values for “Measured TLS” are typically 1500 then reassemble as if starting a new test. Start the motor and
to 5000 mNm. New mixing bowls which have been pre- after several seconds observe the average torque reading. This
polished should have TLS values of approximately 3500 to is the idle torque.
5000 mNm. As the mixing bowl wears, the TLS value is X1.4.4 The idle torque of typical mixing chambers will vary
reduced. When the TLS value reaches 1800 mNm or less, the from a low level of 20 to 30 mNm up to higher levels of 100
mixing bowl should be evaluated for replacement using ASTM to 150 mNm. Most new mixing chambers will exhibit an idle
SRB’s as described in X1.2.3. torque less than 100 mNm. The idle torque of an absorptometer
X1.2.3 If the following criterion are exceeded, the mixing mixing chamber should be monitored regularly such that when
bowl should be replaced: a problem occurs that causes the idle torque to rise above a
X1.2.3.1 Normalized OAN values are outside ASTM SRB typical level, it is recognized and can be investigated.
tolerances for OAN testing. X1.4.5 Generally when idle torque levels exceed 150 to 200
X1.2.3.2 Average differences in measured and normalized mNm or a significant rise in idle torque is observed, this is an
OAN values are greater than 63 to 4 cm3/100 g. indication of one of several possible problems:
X1.4.5.1 The mixing assembly is not properly cleaned.
X1.3 Monitoring Mixing Chamber Surface Conditions X1.4.5.2 The torque sensor may need calibrated. Refer to
Using Fixed TLS the manufacturer’s procedures.
X1.3.1 For absorptometers which are setup for fixed or X1.4.5.3 There may be carbon black-oil paste between the
pre-set TLS level as described in Test Method D2414, Subsec- rotors and bushings or inside the bearing assembly. Correcting
tion 8.3.1.1, regularly monitor the raw or measured value of the this condition requires disassembly and cleaning the bearing
SRB F standard using an x-chart. assembly and possible replacement of the rotor bushings which

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may have excess wear. It is not recommended the user perform X1.4.5.4 Some mixing chambers have bearings which re-
this maintenance, but to send the unit to the manufacturer or quire proper alignment. Refer to the manufacturers alignment
other shop familiar with the equipment and specifications. In procedures.
some cases the bearings may be damaged and require replace-
ment.

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