ASTM D4122-17(2023)
(Practice)Standard Practice for Carbon Black—Evaluation of an Industry Reference Black
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.4 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.
Designation: D4122 − 17 (Reapproved 2023)
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 Transmittance of Toluene Extract
D2414 Test Method for Carbon Black—Oil Absorption
1.1 This practice covers guidelines for the production and
Number (OAN)
testing for uniformity of a lot of carbon black to be used as an
D3182 Practice for Rubber—Materials, Equipment, and Pro-
Industry Reference Black (IRB).
cedures for Mixing Standard Compounds and Preparing
1.2 The values stated in SI units are to be regarded as the
Standard Vulcanized Sheets
standard. The values given in parentheses are for information
D3191 Test Methods for Carbon Black in SBR (Styrene-
only.
Butadiene Rubber)—Recipe and Evaluation Procedures
1.3 This standard does not purport to address all of the
D3192 Test Methods for Carbon Black Evaluation in NR
safety concerns, if any, associated with its use. It is the (Natural Rubber)
responsibility of the user of this standard to establish appro-
D3265 Test Method for Carbon Black—Tint Strength
priate safety, health, and environmental practices and deter- D3493 Test Method for Carbon Black—Oil Absorption
mine the applicability of regulatory limitations prior to use.
Number of Compressed Sample (COAN)
1.4 This international standard was developed in accor- D5230 Test Method for Carbon Black—Automated Indi-
dance with internationally recognized principles on standard-
vidual Pellet Hardness
ization established in the Decision on Principles for the D6556 Test Method for Carbon Black—Total and External
Development of International Standards, Guides and Recom-
Surface Area by Nitrogen Adsorption
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
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
D412 Test Methods for Vulcanized Rubber and Thermoplas-
physicochemical and physical rubber properties of a lot of
tic Elastomers—Tension
carbon black to be used as an IRB.
D1506 Test Methods for Carbon Black—Ash Content
D1508 Test Method for Carbon Black, Pelleted Fines and
4. Production, Quality Control, and Quality Assurance
Attrition
D1509 Test Methods for Carbon Black—Heating Loss
4.1 It is assumed that the manufacturer of the IRB will use
D1510 Test Method for Carbon Black—Iodine Adsorption
state-of-the-art techniques to ensure maximum uniformity
Number
throughout the entire production run. The production should be
D1513 Test Method for Carbon Black, Pelleted—Pour Den-
made in one continuous production lot run. The testing called
sity
for in this practice is not intended to be a substitute for
D1514 Test Method for Carbon Black—Sieve Residue
in-process quality control. This interlaboratory study is only
D1618 Test Method for Carbon Black Extractables—
adequate to verify the quality of a homogeneous lot.
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 eight to
This practice is under the jurisdiction of ASTM Committee D24 on Carbon
ten years at the most recent rate of use.
Black and is the direct responsibility of Subcommittee D24.61 on Carbon Black
Sampling and Statistical Analysis.
4.3 The black should be bagged in 50 lb polyethylene bags
Current edition approved May 1, 2023. Published June 2023. Originally
ɛ1
to reduce moisture incursion. Each pallet of bagged black
approved in 1982. Last previous edition approved in 2017 as D4122 – 17 . DOI:
10.1520/D4122-17R23.
should be wrapped in plastic to reduce environmental expo-
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
sure. Depending on the size of the lot, the bagged black will be
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
segregated into equal sized sublots, typically ten to twenty,
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. representing some logical subdivision, such as a truck load.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4122 − 17 (2023)
5. Sampling 6.2 Rubber Physical Tests:
6.2.1 Perform the following physical tests in rubber on both
5.1 To avoid having to break down stacked and wrapped
the new and previous IRB. Test samples mixed in accordance
bags on a pallet, the bags to be used as samples for uniformity
with Test Methods D3191, Test Method A, Test Method B, or
and property determination testing are typically removed at
Test Method C and cure for 50 min at 145 °C as well as
appropriate times from the bagging stream. At least one sample
samples mixed in accordance with Test Methods D3192, Test
per sublot will be collected for uniformity testing. If more than
Method A, Test Method B, or Test Method C and cure for
one sample point is identified for each sublot, they should be
30 min at 145 °C. It is preferred that participating laboratories
spaced to represent approximately equal quantities. Typically,
be found so that data from all test methods can be included for
two bags are taken at each sampling point. One is retained by
evaluation.
the producer for in-house uniformity testing and one is used for
6.2.1.1 In accordance with Test Methods D412, Test Method
samples to be distributed to participants in the rubber testing
A, test five dumbbells from each cured sheet and determine the
and uniformity ITP. The bags selected will be numbered from
mean values of tensile stress at 300 % elongation, tensile
one through n, where n is the total number of sublots, in order
strength, and ultimate elongation.
to represent the corresponding production lot or labeled to
6.2.1.2 Record data in absolute numbers (not as differences
identify the sublot and its position relative to the whole of the
corresponding production lot. from IRB) on Table 1, reporting tensile stress and tensile
strength to the nearest 0.1 MPa and ultimate elongation to the
5.2 n 4-dm (1 gal) samples, numbered from one through n,
nearest 5 %.
or marked with the labels from 5.1 as taken from the corre-
sponding bags, will be sent to each participant in the interla-
6.3 Informational Physicochemical Tests:
boratory study to evaluate the new IRB.
6.3.1 Perform the following physicochemical tests on the
new IRB:
5.3 Additionally, a 4-dm (1 gal) sample of the previous
6.3.1.1 Iodine Adsorption Number (Test Method D1510)—
IRB taken from a common blended source will also be sent to
Report the result obtained from an individual determination in
each participant.
grams of iodine per kilogram to the nearest 0.1 unit.
6. Procedure
6.3.1.2 Oil Absorption Number (Test Method D2414)—
Report the result obtained from an individual determination in
6.1 It is preferred that all of the samples be tested on the
–5 3 3
10 m kg (cm /100 g) to the nearest 0.1 unit.
same day for any of the test methods described in 6.2 and 6.3.
If the testing cannot be completed in the same day, it should be 6.3.2 Record data on Table 2 (or in a form that captures the
completed in consecutive days. same information as in Table 2).
TABLE 1 Industry Reference Black Test Data
Laboratory Number __ Test Method _____
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 − 17 (2023)
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 ____
where:
7. Statistical Analysis
X = measured value for new IRB, and
7.1 For each test in Table 1, enter the results from each
X = measured value for previous IRB.
laboratory for each sample into the form shown in Table 3.
Then calculate the statistics defined in Table 3. 7.2 If any row average test result falls outside the interval
defined by the upper and lower control limits shown in Table 3,
NOTE 1—Rubber physical test data are to be entered as differences from
this will indicate that the sublot of IRB represented by that row
the previous IRB. For example:
Difference 5 X 2 X (1)
1 2
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 Met
...
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