Standard Practice for Carbon Black—Evaluation of an Industry Reference Black

SIGNIFICANCE AND USE
3.1 These guidelines are intended to ensure that IRBs are evaluated by a standard procedure.  
3.2 These guidelines are to be used to establish the average physicochemical and physical rubber properties of a lot of carbon black to be used as an IRB.
SCOPE
1.1 This practice covers guidelines for the production and testing for uniformity of a lot of carbon black to be used as an Industry Reference Black (IRB).  
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
1.3 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 and health practices and determine the applicability of regulatory limitations prior to use.

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Historical
Publication Date
31-Dec-2014
Current Stage
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D4122 − 10a (Reapproved 2015)
Standard Practice for
Carbon Black—Evaluation of an Industry Reference Black
This standard is issued under the fixed designation D4122; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope D3191Test Methods for Carbon Black in SBR (Styrene-
Butadiene Rubber)—Recipe and Evaluation Procedures
1.1 This practice covers guidelines for the production and
D3192Test Methods for Carbon Black Evaluation in NR
testing for uniformity of a lot of carbon black to be used as an
(Natural Rubber)
Industry Reference Black (IRB).
D3265Test Method for Carbon Black—Tint Strength
1.2 The values stated in SI units are to be regarded as the
D3493Test Method for Carbon Black—Oil Absorption
standard. The values given in parentheses are for information
Number of Compressed Sample (COAN)
only.
D5230Test Method for Carbon Black—Automated Indi-
1.3 This standard does not purport to address all of the
vidual Pellet Hardness
safety concerns, if any, associated with its use. It is the D6556Test Method for Carbon Black—Total and External
responsibility of the user of this standard to establish appro-
Surface Area by Nitrogen Adsorption
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
3. Significance and Use
3.1 These guidelines are intended to ensure that IRBs are
2. Referenced Documents
evaluated by a standard procedure.
2.1 ASTM Standards:
3.2 These guidelines are to be used to establish the average
D412TestMethodsforVulcanizedRubberandThermoplas-
physicochemical and physical rubber properties of a lot of
tic Elastomers—Tension
carbon black to be used as an IRB.
D1506Test Methods for Carbon Black—Ash Content
D1508Test Method for Carbon Black, Pelleted Fines and
4. Production, Quality Control, and Quality Assurance
Attrition
4.1 It is assumed that the manufacturer of the IRB will use
D1509Test Methods for Carbon Black—Heating Loss
D1510Test Method for Carbon Black—Iodine Adsorption state-of-the-art techniques to ensure maximum uniformity
throughouttheentireproductionrun.Theproductionshouldbe
Number
made in one continuous production lot run. The testing called
D1513Test Method for Carbon Black, Pelleted—Pour Den-
for in this practice is not intended to be a substitute for
sity
in-process quality control. This interlaboratory study is only
D1514Test Method for Carbon Black—Sieve Residue
adequate to verify the quality of a homogeneous lot.
D1618 Test Method for Carbon Black Extractables—
Transmittance of Toluene Extract
4.2 Thesizeofthelotisdeterminedbyhistoricalrecordson
D2414Test Method for Carbon Black—Oil Absorption
the rate of use. The lot should have an expected life of 8 to 10
Number (OAN)
years at the most recent rate of use.
D3182PracticeforRubber—Materials,Equipment,andPro-
4.3 The black should be bagged in 50-lb polyethylene bags
cedures for Mixing Standard Compounds and Preparing
to reduce moisture incursion. Each pallet of bagged black
Standard Vulcanized Sheets
should be wrapped in plastic to reduce environmental expo-
sure. The bagged black will be segregated into at least twelve
equal sized sublots for uniformity testing.
This practice is under the jurisdiction of ASTM Committee D24 on Carbon
Black and is the direct responsibility of Subcommittee D24.61 on Carbon Black
Sampling and Statistical Analysis.
5. Sampling
Current edition approved Jan. 1, 2015. Published February 2015. Originally
5.1 Afterasuitabletimetoallowtheblacktostabilize,abag
approved in 1982. Last previous edition approved in 2010 as D4122–10a. DOI:
10.1520/D4122-10AR15.
will be selected from the approximate middle of each of the
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
sublots; the bags selected will be numbered from one through
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
n, where n is the total number of sublots, in order to represent
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. the corresponding production lot.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4122 − 10a (2015)
5.2 n4-dm (1-gal)samples,numberedfromonethrough n, 6.4.1.1 Iodine Adsorption Number (Test Method D1510)—
and taken from the corresponding bags, will be sent to each Report the result obtained from an individual determination in
participant in the interlaboratory study to evaluate the new grams of iodine per kilogram to the nearest 0.1 unit.
IRB.
6.4.1.2 Oil Absorption Number (Test Method D2414)—
Report the result obtained from an individual determination in
5.3 Additionally, a 4-dm (1-gal) sample of the previous
–5 3 3
10 m kg (cm /100 g) to the nearest 0.1 unit.
IRB taken from a common blended source will also be sent to
6.4.2 Record data on Table 2 (or in a form that captures the
each participant.
same information as in Table 2).
6. Procedure
7. Statistical Analysis
6.1 Test, in order, one of the n samples on each of the one
to n days. These days shall be as near to consecutive as
7.1 For each test in Table 1, enter the results from each
possible.
laboratory for each sample into the form shown in Table 3.
Then calculate the statistics defined in Table 3.
6.2 Each day a sample is tested, subject it to all of the test
methods described in 6.3 and 6.4.
NOTE1—Rubberphysicaltestdataaretobeenteredasdifferencesfrom
the previous IRB. For example:
6.3 Rubber Physical Tests:
6.3.1 Perform the following physical tests in rubber on both
Difference 5 X 2 X (1)
1 2
the new and previous IRB. Test samples mixed in accordance
where:
withTestMethodsD3191andcurefor50minat145°Caswell
X = measured value for new IRB, and
as samples mixed in accordance with Test Methods D3192,
X = measured value for previous IRB.
Test Method A, and cure for 30 min at 145°C.
7.2 If any row average test result falls outside the interval
6.3.1.1 InaccordancewithTestMethodsD412,TestMethod
definedbytheupperandlowercontrollimitsshowninTable3,
A,testfivedumbbellsfromeachcuredsheetanddeterminethe
thiswillindicatethatthesublotofIRBrepresentedbythatrow
median values of tensile stress at 300% elongation, tensile
average may be rejected by Committee D24 as being a
strength, and ultimate elongation.
nonhomogeneous portion of the production lot.
6.3.1.2 Record data in absolute numbers (not as differences
from IRB) on Table 1, reporting tensile stress and tensile
7.3 If any laboratory average test result (column average)
strength to the nearest 0.1 MPa and ultimate elongation to the
falls outside the upper and lower control limits shown in Table
nearest 5%.
3,thenthatlaboratory’sdataforthattestshouldbedeletedand
6.4 Informational Physicochemical Tests: Table 3 should be recalculated excluding that laboratory. Such
6.4.1 Perform the following physicochemical tests on the data indicates that the laboratory has a significant reproduc-
new IRB: ibility problem, which needs corrective action.
TABLE 1 Industry Reference Black Test Data
Laboratory Number __
Tensile
300 %
Stress at Elonga- Tensile Strength, Elonga-
Day of Mix- Sample Tensile Strength, Modulus,
300 %, tion, % MPa tion, %
ing and Date No. MPa D3191 MPa
MPa D3191 D3192 D3192
D3192
D3191
Day No.__ 50' 30'
Date ____ Prev. IRB 50' 30'
Day No.__ 50' 30'
Date ____ Prev. IRB 50' 30'
Day No.__ 50' 30'
Date ____ Prev. IRB 50' 30'
Day No.__ 50' 30'
Date ____ Prev. IRB 50' 30'
Day No.__ 50' 30'
Date ____ Prev. IRB 50' 30'
Day No.__ 50' 30'
Date ____ Prev. IRB 50' 30'
Day No.__ 50' 30'
Date ____ Prev. IRB 50' 30'
Day No.__ 50' 30'
Date ____ Prev. IRB 50' 30'
Day No.__ 50' 30'
Date ____ Prev. IRB 50' 30'
Day No.__ 50' 30'
Date ____ Prev. IRB 50' 30'
Day No.__ 50' 30'
Date ____ Prev. IRB 50' 30'
Day No.__ 50' 30'
Date ____ Prev. IRB 50' 30'
D4122 − 10a (2015)
TABLE 2 Industry Reference Black Informational Test Data
Laboratory Number__
Oil Absorption
Iodine No., No.,
Day of Mixing
–5 3 3
Sample No. g/kg 10 mg /kg (cm /
and Date
D1510 100 g)
D2414
Day No.____ ___
Date ____
Day No.____ ___
Date ____
Day No.____ ___
Date ____
Day No.____ ___
Date ____
Day No.____ ___
Date ____
Day No.____ ___
Date ____
Day No.____ ___
Date ____
Day No.____ ___
Date ____
Day No.____ ___
Date ____
Day No.____ ___
Date ____
Day No.____ ___
Date ____
Day No.____ ___
Date ____
TABLE 3 Statistical Analysis Form
NOTE 1—Experience so far has shown that neither a laboratory’s test values nor a sample’s test values are random values about the grand average,
but tend to reflect a persistent bias typified by the average value for the laboratory or the sample. Consequently, it is not appropriate to divide the
reproducibility by the square root of L or N as might otherwise be the case when comparing averages of L or N values to the grand average of L× N
values.
Test Method: ASTM D _ _ _
Sample
¯
No. Laboratory No.→ 1 2 . i . LX
R

...
j
...
N
¯ %
X
X5
C
¯
Row average X = ∑ X/L
R i
% ¯
Grand average test value X5 X /N
( j R
%
Upper and lower control limits for row averages 5X6reproducibilityofthetestmethod.
¯
Column aver
...


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: D4122 − 10a D4122 − 10a (Reapproved 2015)
Standard Practice for
Carbon Black—Evaluation of an Industry Reference Black
This standard is issued under the fixed designation D4122; 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
1.1 This practice covers guidelines for the production and testing for uniformity of a lot of carbon black to be used as an Industry
Reference Black (IRB).
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.3 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 and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2.1 ASTM Standards:
D412 Test Methods for Vulcanized Rubber and Thermoplastic Elastomers—Tension
D1506 Test Methods for Carbon Black—Ash Content
D1508 Test Method for Carbon Black, Pelleted Fines and Attrition
D1509 Test Methods for Carbon Black—Heating Loss
D1510 Test Method for Carbon Black—Iodine Adsorption Number
D1513 Test Method for Carbon Black, Pelleted—Pour Density
D1514 Test Method for Carbon Black—Sieve Residue
D1618 Test Method for Carbon Black Extractables—Transmittance of Toluene Extract
D2414 Test Method for Carbon Black—Oil Absorption Number (OAN)
D3182 Practice for Rubber—Materials, Equipment, and Procedures for Mixing Standard Compounds and Preparing Standard
Vulcanized Sheets
D3191 Test Methods for Carbon Black in SBR (Styrene-Butadiene Rubber)—Recipe and Evaluation Procedures
D3192 Test Methods for Carbon Black Evaluation in NR (Natural Rubber)
D3265 Test Method for Carbon Black—Tint Strength
D3493 Test Method for Carbon Black—Oil Absorption Number of Compressed Sample (COAN)
D5230 Test Method for Carbon Black—Automated Individual Pellet Hardness
D6556 Test Method for Carbon Black—Total and External Surface Area by Nitrogen Adsorption
3. Significance and Use
3.1 These guidelines are intended to ensure that IRBs are evaluated by a standard procedure.
3.2 These guidelines are to be used to establish the average physicochemical and physical rubber properties of a lot of carbon
black to be used as an IRB.
4. Production, Quality Control, and Quality Assurance
4.1 It is assumed that the manufacturer of the IRB will use state-of-the-art techniques to ensure maximum uniformity throughout
the entire production run. The production should be made in one continuous production lot run. The testing called for in this
practice is not intended to be a substitute for in-process quality control. This interlaboratory study is only adequate to verify the
quality of a homogeneous lot.
This practice is under the jurisdiction of ASTM Committee D24 on Carbon Black and is the direct responsibility of Subcommittee D24.61 on Carbon Black Sampling
and Statistical Analysis.
Current edition approved Feb. 15, 2010Jan. 1, 2015. Published March 2010February 2015. Originally approved in 1982. Last previous edition approved in 2010 as
D4122 – 10.D4122 – 10a. DOI: 10.1520/D4122-10A.10.1520/D4122-10AR15.
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4122 − 10a (2015)
4.2 The size of the lot is determined by historical records on the rate of use. The lot should have an expected life of 8 to 10
years at the most recent rate of use.
4.3 The black should be bagged in 50-lb polyethylene bags to reduce moisture incursion. Each pallet of bagged black should
be wrapped in plastic to reduce environmental exposure. The bagged black will be segregated into at least twelve equal sized
sublots for uniformity testing.
5. Sampling
5.1 After a suitable time to allow the black to stabilize, a bag will be selected from the approximate middle of each of the
sublots; the bags selected will be numbered from one through n, where n is the total number of sublots, in order to represent the
corresponding production lot.
5.2 n 4-dm (1-gal) samples, numbered from one through n, and taken from the corresponding bags, will be sent to each
participant in the interlaboratory study to evaluate the new IRB.
5.3 Additionally, a 4-dm (1-gal) sample of the previous IRB taken from a common blended source will also be sent to each
participant.
6. Procedure
6.1 Test, in order, one of the n samples on each of the one to n days. These days shall be as near to consecutive as possible.
6.2 Each day a sample is tested, subject it to all of the test methods described in 6.3 and 6.4.
6.3 Rubber Physical Tests:
6.3.1 Perform the following physical tests in rubber on both the new and previous IRB. Test samples mixed in accordance with
Test Methods D3191 and cure for 50 min at 145°C as well as samples mixed in accordance with Test Methods D3192, Test Method
A, and cure for 30 min at 145°C.
6.3.1.1 In accordance with Test Methods D412, Test Method A, test five dumbbells from each cured sheet and determine the
median values of tensile stress at 300 % elongation, tensile strength, and ultimate elongation.
6.3.1.2 Record data in absolute numbers (not as differences from IRB) on Table 1, reporting tensile stress and tensile strength
to the nearest 0.1 MPa and ultimate elongation to the nearest 5 %.
6.4 Informational Physicochemical Tests:
6.4.1 Perform the following physicochemical tests on the new IRB:
6.4.1.1 Iodine Adsorption Number (Test Method D1510)—Report the result obtained from an individual determination in grams
of iodine per kilogram to the nearest 0.1 unit.
TABLE 1 Industry Reference Black Test Data
Laboratory Number __
Tensile
300 %
Stress at Elonga- Tensile Strength, Elonga-
Day of Mix- Sample Tensile Strength, Modulus,
300 %, tion, % MPa tion, %
ing and Date No. MPa D3191 MPa
MPa D3191 D3192 D3192
D3192
D3191
Day No.__ 50' 30'
Date ____ Prev. IRB 50' 30'
Day No.__ 50' 30'
Date ____ Prev. IRB 50' 30'
Day No.__ 50' 30'
Date ____ Prev. IRB 50' 30'
Day No.__ 50' 30'
Date ____ Prev. IRB 50' 30'
Day No.__ 50' 30'
Date ____ Prev. IRB 50' 30'
Day No.__ 50' 30'
Date ____ Prev. IRB 50' 30'
Day No.__ 50' 30'
Date ____ Prev. IRB 50' 30'
Day No.__ 50' 30'
Date ____ Prev. IRB 50' 30'
Day No.__ 50' 30'
Date ____ Prev. IRB 50' 30'
Day No.__ 50' 30'
Date ____ Prev. IRB 50' 30'
Day No.__ 50' 30'
Date ____ Prev. IRB 50' 30'
Day No.__ 50' 30'
Date ____ Prev. IRB 50' 30'
D4122 − 10a (2015)
–5 3
6.4.1.2 Oil Absorption Number (Test Method D2414)—Report the result obtained from an individual determination in 10 m kg
(cm /100 g) to the nearest 0.1 unit.
6.4.2 Record data on Table 2 (or in a form that captures the same information as in Table 2).
7. Statistical Analysis
7.1 For each test in Table 1, enter the results from each laboratory for each sample into the form shown in Table 3. Then
calculate the statistics defined in Table 3.
NOTE 1—Rubber physical test data are to be entered as differences from the previous IRB. For example:
Difference 5 X 2 X (1)
1 2
where:
X = measured value for new IRB, and
X = measured value for previous IRB.
7.2 If any row average test result falls outside the interval defined by the upper and lower control limits shown in Table 3, this
will indicate that the sublot of IRB represented by that row average may be rejected by Committee D24 as being a
nonhomogeneous portion of the production lot.
7.3 If any laboratory average test result (column average) falls outside the upper and lower control limits shown in Table 3, then
that laboratory’s data for that test should be deleted and Table 3 should be recalculated excluding that laboratory. Such data
indicates that the laboratory has a significant reproducibility problem, which needs corrective action.
7.4 After deleting data, the remaining data for each test can be used to provide average differences between the new IRB and
the previous one.
7.5 For each test in Table 2, enter the results from each laboratory for each sample in the form shown in Table 3. Then calculate
the statistics defined in Table 3. The results are for information only and not to determine the uniformity of the lot.
8. Acceptance
8.1 All sublots tested as homogeneous by this practice will be considered acceptable by Committee D24 for use as the new IRB.
9. Shelf Life
9.1 The shelf life of the Industry Reference Black (IRB) carbon blacks is indefinite when properly stored in a manner that
protects it from exposure to sources of moisture, such as precipitation, other sources of liquid water, or high humidity
environments. Iodine number is the only property known to change over an extended period (years). This is due to a slow increase
TABLE 2 Industry Reference Black Informational Test Data
Laboratory Number__
Oil Absorption
Iodine No., No.,
Day of Mixing
–5 3 3
Sample No. g/kg 10 mg /kg (cm /
and Date
D1510 100 g
...

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