ASTM D3265-23
(Test Method)Standard Test Method for Carbon Black-Tint Strength
Standard Test Method for Carbon Black-Tint Strength
SIGNIFICANCE AND USE
4.1 For the broad range of commercial rubber grade carbon blacks, tint strength is highly dependent upon particle size. Tint strength can be used as an indication of particle size; however, tint strength is also dependent on structure and aggregate size distribution. Therefore, differences in tint strength within grades of carbon black may reflect differences other than particle size.
Note 1: This test method was developed primarily for the characterization of N100, N200, and N300 series carbon blacks.
4.2 Tint strength values within the carbon black industry have been developed using a Automatic Muller apparatus which is used to prepare carbon black-zinc oxide pastes. An alternative mixing apparatus, Hauschild SpeedMixer3,4 (DAC 150 FVZ), and a corresponding procedure have been extensively studied within D24 and shown to provide equivalent tint strength for all carcass or soft blacks and most tread blacks with the exception of higher surface area N100 types and specialty blacks. Therefore, it is the responsibility of the user of this alternate apparatus to ensure their products will adequately disperse. Disputes arising between a user and producer should be resolved using the Automatic Muller apparatus until ASTM develops adequate precision statements.
4.3 The term ITRB is used in the entire text for both, the original ITRB, used as the first reference material for tint testing, but which is now used up, and the successor reference material, ITRB2.
SCOPE
1.1 This test method covers the determination of the tint strength of carbon black relative to an industry tint reference black (ITRB).
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
Frequently Asked Questions
ASTM D3265-23 is a standard published by ASTM International. Its full title is "Standard Test Method for Carbon Black-Tint Strength". This standard covers: SIGNIFICANCE AND USE 4.1 For the broad range of commercial rubber grade carbon blacks, tint strength is highly dependent upon particle size. Tint strength can be used as an indication of particle size; however, tint strength is also dependent on structure and aggregate size distribution. Therefore, differences in tint strength within grades of carbon black may reflect differences other than particle size. Note 1: This test method was developed primarily for the characterization of N100, N200, and N300 series carbon blacks. 4.2 Tint strength values within the carbon black industry have been developed using a Automatic Muller apparatus which is used to prepare carbon black-zinc oxide pastes. An alternative mixing apparatus, Hauschild SpeedMixer3,4 (DAC 150 FVZ), and a corresponding procedure have been extensively studied within D24 and shown to provide equivalent tint strength for all carcass or soft blacks and most tread blacks with the exception of higher surface area N100 types and specialty blacks. Therefore, it is the responsibility of the user of this alternate apparatus to ensure their products will adequately disperse. Disputes arising between a user and producer should be resolved using the Automatic Muller apparatus until ASTM develops adequate precision statements. 4.3 The term ITRB is used in the entire text for both, the original ITRB, used as the first reference material for tint testing, but which is now used up, and the successor reference material, ITRB2. SCOPE 1.1 This test method covers the determination of the tint strength of carbon black relative to an industry tint reference black (ITRB). 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.
SIGNIFICANCE AND USE 4.1 For the broad range of commercial rubber grade carbon blacks, tint strength is highly dependent upon particle size. Tint strength can be used as an indication of particle size; however, tint strength is also dependent on structure and aggregate size distribution. Therefore, differences in tint strength within grades of carbon black may reflect differences other than particle size. Note 1: This test method was developed primarily for the characterization of N100, N200, and N300 series carbon blacks. 4.2 Tint strength values within the carbon black industry have been developed using a Automatic Muller apparatus which is used to prepare carbon black-zinc oxide pastes. An alternative mixing apparatus, Hauschild SpeedMixer3,4 (DAC 150 FVZ), and a corresponding procedure have been extensively studied within D24 and shown to provide equivalent tint strength for all carcass or soft blacks and most tread blacks with the exception of higher surface area N100 types and specialty blacks. Therefore, it is the responsibility of the user of this alternate apparatus to ensure their products will adequately disperse. Disputes arising between a user and producer should be resolved using the Automatic Muller apparatus until ASTM develops adequate precision statements. 4.3 The term ITRB is used in the entire text for both, the original ITRB, used as the first reference material for tint testing, but which is now used up, and the successor reference material, ITRB2. SCOPE 1.1 This test method covers the determination of the tint strength of carbon black relative to an industry tint reference black (ITRB). 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.
ASTM D3265-23 is classified under the following ICS (International Classification for Standards) categories: 83.040.20 - Rubber compounding ingredients. The ICS classification helps identify the subject area and facilitates finding related standards.
ASTM D3265-23 has the following relationships with other standards: It is inter standard links to ASTM D3265-23a, ASTM D1900-06(2015), ASTM D4821-15, ASTM D4821-14, ASTM D1799-03a(2014), ASTM D1900-06(2011), ASTM D1799-03a(2008), ASTM D4821-07e1, ASTM D4821-07, ASTM D1900-06, ASTM D4821-06, ASTM D4821-05, ASTM D4821-04, ASTM D4821-03a, ASTM D1799-03a. Understanding these relationships helps ensure you are using the most current and applicable version of the standard.
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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: D3265 − 23
Standard Test Method for
Carbon Black—Tint Strength
This standard is issued under the fixed designation D3265; 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 to produce a black or gray paste. This paste is then spread to
produce a surface suitable for measuring the reflectance of the
1.1 This test method covers the determination of the tint
mixture by means of a photo-electric reflectance meter. The
strength of carbon black relative to an industry tint reference
reflectance of the tested sample is then compared to the
black (ITRB).
reflectance of the ITRB prepared in the same manner. The tint
1.2 The values stated in SI units are to be regarded as the
strength of the tested sample is expressed as units of the
standard. The values given in parentheses are for information
reflectance of the ITRB divided by the reflectance of the
only.
sample and multiplied by 100. The test value is therefore
1.3 This standard does not purport to address all of the
expressed in %.
safety concerns, if any, associated with its use. It is the
3.2 Correction Factor:
responsibility of the user of this standard to establish appro-
3.2.1 A correction factor in Eq 3 is needed when raw
priate safety, health, and environmental practices and deter-
materials Paraplex G-62 and ZnO Lot#8 or earlier produced
mine the applicability of regulatory limitations prior to use.
before 2012, in combination with ITRB2, are used. For
1.4 This international standard was developed in accor-
additional details refer to ASTM D3265-17a.
dance with internationally recognized principles on standard-
3.2.2 There should be no correction applied when ITRB is
ization established in the Decision on Principles for the
used with Paraplex G-62 and ZnO Lot#8 or earlier.
Development of International Standards, Guides and Recom-
3.2.3 There should be no correction applied when using the
mendations issued by the World Trade Organization Technical
currently available tint raw materials (see Section 6) for pastes
Barriers to Trade (TBT) Committee.
prepared with either ITRB or ITRB2.
2. Referenced Documents
4. Significance and Use
2.1 ASTM Standards:
4.1 For the broad range of commercial rubber grade carbon
D1799 Practice for Carbon Black—Sampling Packaged
blacks, tint strength is highly dependent upon particle size. Tint
Shipments
strength can be used as an indication of particle size; however,
D1900 Practice for Carbon Black—Sampling Bulk Ship-
tint strength is also dependent on structure and aggregate size
ments
distribution. Therefore, differences in tint strength within
D4483 Practice for Evaluating Precision for Test Method
grades of carbon black may reflect differences other than
Standards in the Rubber and Carbon Black Manufacturing
particle size.
Industries
NOTE 1—This test method was developed primarily for the character-
D4821 Guide for Carbon Black—Validation of Test Method
ization of N100, N200, and N300 series carbon blacks.
Precision and Bias
4.2 Tint strength values within the carbon black industry
3. Summary of Test Method
have been developed using a Automatic Muller apparatus
which is used to prepare carbon black-zinc oxide pastes. An
3.1 A carbon black sample is mixed with a white powder
3,4
(zinc oxide) and a liquid vehicle (epoxidized soybean oil, ESO) alternative mixing apparatus, Hauschild SpeedMixer (DAC
150 FVZ), and a corresponding procedure have been exten-
sively studied within D24 and shown to provide equivalent tint
This test method is under the jurisdiction of ASTM Committee D24 on Carbon
strength for all carcass or soft blacks and most tread blacks
Black and is the direct responsibility of Subcommittee D24.21 on Carbon Black
Surface Area and Related Properties.
Current edition approved Feb. 1, 2023. Published February 2023. Originally
approved in 1973. Last previous edition approved in 2021 as D3265 – 21. DOI: The sole source of supply of the apparatus – Hauschild SpeedMixer®, which
10.1520/D3265-23. has been qualified for this method, including the DAC150 FVZ – known to the
For referenced ASTM standards, visit the ASTM website, www.astm.org, or committee at this time is Hauschild, www.hauschild-speedmixer.com.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM If you are aware of alternative suppliers, please provide this information to
Standards volume information, refer to the standard’s Document Summary page on ASTM International Headquarters. Your comments will receive careful consider-
the ASTM website. ation at a meeting of the responsible technical committee, which you may attend.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3265 − 23
3,4
with the exception of higher surface area N100 types and 5.11 SpeedMixer (DAC 150 FVZ), PP15 cups and holder.
specialty blacks. Therefore, it is the responsibility of the user of
5.12 IKA A-10 Analytical Mill, A-14 SS cutter, A-18 cham-
this alternate apparatus to ensure their products will adequately
9,4
ber reducer.
disperse. Disputes arising between a user and producer should
10,4
be resolved using the Automatic Muller apparatus until ASTM
5.13 5 mm Glass Grinding Beads.
develops adequate precision statements.
6. Reagents and Materials
4.3 The term ITRB is used in the entire text for both, the
original ITRB, used as the first reference material for tint
6.1 Purity of Reagents—Reagent grade chemicals shall be
testing, but which is now used up, and the successor reference
used in all tests. Unless otherwise indicated, it is intended all
material, ITRB2.
reagents shall conform to the specifications of the Committee
on Analytical Reagents of the American Chemical Society,
5. Apparatus
where such specifications are available. Other grades may be
used, provided it is first ascertained that the reagent is of
5.1 Analytical Balance, with a sensitivity of 60.1 mg.
sufficiently high purity to permit its use without lessening the
5,4
5.2 Automatic Muller.
accuracy of the determination.
5.3 Photometric Instrument, capable of detecting differ-
6.2 Industry Tint Reference Black.
ences in the amount of light reflectance between shades of
6,4
13,14
gray. The instrument is to be operated following the manu-
6.3 Plasticizer, soybean oil epoxide.
facturer’s instructions for optimum performance.
6.4 Denatured Alcohol, for cleaning purposes.
5.4 Oven, Gravity-Convection Type, capable of temperature
regulation within 61°C at 125°C (62°F at 257°F) and 6.5 Zinc Oxide, Industry Tint Zinc Oxide.
temperature uniformity within 65°C (69°F).
6.6 ASTM D24 Standard Reference Blacks.
5.5 Reflectance Standards, as required for each reflectance
instrument for checking calibration.
7. Sampling
5.6 Spatulas, 100 to 150 mm (4 to 6 in.), two, flexible,
7.1 Samples of shipments shall be taken in accordance with
tapered.
Practices D1799 and D1900.
5.7 Syringe, 5-cm , automatic refilling, reproducible to
60.02 cm .
8. Calibration and Standardization
5.8 Wiping Tissue, absorbent and lint free.
8.1 Standard Pastes—Prepare pastes of the ITRB, following
9.2 – 9.3.2 for the following masses, prepare the 0.1000-g
5.9 Paste Application Apparatus—Any one of the following
Automatic Muller paste or the 0.1200-g SpeedMixer paste in
groups of equipment may be used:
duplicate:
5.9.1 Apparatus for Film Drawdown Method:
7,4
5.9.1.1 Film Applicator, 0.076 mm (0.003 in.) in depth.
5.9.1.2 Polished Glass Plate, approximately 760 by 500 by
10 mm (30 by 20 by 0.375 in.). 9
The sole source of supply of the apparatus (Part #EW-04301-00) known to the
5.9.2 Apparatus for Roller Spreader Method:
committee at this time is Cole-Parmer Instrument Company, 625 East Bunker Court,
8,4
Vernon Hills, IL 60061. http://www.coleparmer.com
5.9.2.1 Tint Roller Spreader.
The sole source of supply of glass grinding beads known to the committee at
5.10 Desiccator.
this time is Quackenbush Co., Inc., 6711 Sands Rd., Crystal Lake, IL 60014.
http://www.quackco.com
Reagent Chemicals, American Chemical Society Specifications , American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
The following instruments have been found satisfactory for this test method: listed by the American Chemical Society, see Analar Standards for Laboratory
Hoover Automatic Muller, Model M5, Hoover Color Corp., P.O. Box 218, State Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Highway 693, Hiwassee, VA 24347. Automatic Pigment Muller JEL 25/53-II, J. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Engelsmann AG, Frankenthaler Str. 137 – 141, 67059 Ludwigshafen, Germany, MD.
www.engelsmann.de. The original ITRB is depleted and therefore no longer commercially available.
The following instruments have been found satisfactory for this test method: However, any available stocks of original ITRB may still be used. The successor of
Erichsen Tint Tester 527, available from T. J. Bell, Inc., 1340 Home Ave., Akron, the original ITRB is ITRB2. ITRB2 was commercialized in 2012.
OH 44310, and Hunter MiniScan EZ, available from Hunter Associates Laboratory, The sole source of supply of the epoxidized soybean oil (Greenflex 7170)
Inc., 11491 Sunset Hills Road, Reston, Virginia 20190-5280. known to the committee at this time is Balentine Enterprises, Inc., dba Laboratory
The Hunter MiniScan XE or XE Plus may still be used for the test, but are no Standards and Technologies, 227 Somerset St., Borger, TX 79007, www.carbon-
longer commercially available. Instructions are the same for all Hunter Miniscan standard.com.
types. Supporting data (on the shelf life of this material) have been filed at ASTM
The Densicron reflectometer, though no longer commercially available, may be International Headquarters and may be obtained by requesting Research Report
used for the test. For instructions, see Test Method D3265 – 01. RR:D24-1004.
7 15
The sole source of supply of the Film Applicator, Catalog No. 5553, known to The sole source of supply of Industry Tint Zinc Oxide known to the committee
the committee at this time is Byk-Gardner, 9104 Guilford Rd., Columbia, MD at this time is Balentine Enterprises, Inc., dba Laboratory Standards and
21046, http://www.byk.com. Technologies, 227 Somerset St., Borger, TX 79007, www.carbonstandard.com.
8 16
The sole source of supply of the Tint Roller Spreader, Model 1A, known to the The sole source of supply of ASTM D24 Standard Reference Blacks known to
committee at this time is Titan Specialties, Inc., P.O. Box 2316, Pampa, TX the committee at this time is Laboratory Standards and Technologies, 227 Somerset
79066-2316. St., Borger, TX 79007.
D3265 − 23
on a periodic basis using ASTM D24 Standard Reference
Calibration Tint
Industry Tint Reference Black
Units [%]
Blacks. The standard tint strength values and the acceptable
Automatic SpeedMixer
test limit of the standard reference blacks may be found in
Muller Pastes Pastes
0.0900 g 0.1080 g 90.0 Guide D4821.
0.1000 g 0.1200 g 100.0
8.3 Hunter MiniScan:
0.1100 g 0.1320 g 110.0
0.1200 g 0.1440 g 120.0
8.3.1 Calibrate the instrument using the black and white
0.1300 g 0.1560 g 130.0
tiles.
NOTE 2—Optionally, 0.1400 and 0.1500 g of Automatic Muller paste or
8.3.2 Place the instrument in Setup Mode. Set up instrument
0.1680 and 0.1800 g of SpeedMixer paste may be added in the standard-
with XYZ color scale, D65 illuminant, 10° observer, average a
ization step when samples with tint results above 130 tint units are tested.
minimum of three readings. (Note that Y corresponds to the
The modified standardization should only be used for samples exceeding
130 tint units. lightness/darkness function, and thus represents the informa-
tion of interest).
8.2 Erichsen Tint Tester 527:
8.3.3 Read each of the ITRB pastes at least three times and
8.2.1 Turn on the power switch and allow for 30 min
record only the average Y value of the three readings. The Y
warm-up.
value for the 0.1000-g Automatic Muller or 0.1200-g Speed-
8.2.2 Place the reflectance head on the black calibration
Mixer paste should read approximately 2.60. Calculate the tint
panel and adjust the digital readout to 0.00 using the “zero”
strength of the ITRB pastes as follows:
control potentiometer.
8.2.3 Following Section 9, prepare the paste drawdown for Tint @%# 5 I/Y × 100 (2)
reflectance measurement.
where:
8.2.4 Use one of the 0.1000-g Automatic Muller or 0.1200-g
I = reflectance of 0.1000-g Automatic Muller or 0.1200-g
SpeedMixer ITRB pastes of 8.1 to set the instrument to read
SpeedMixer ITRB paste.
3.00 using the calibration control potentiometer.
Y = reflectance value of sample.
8.2.5 Determine the reflectivity on the remaining 0.1000-g
Automatic Muller or 0.1200-g SpeedMixer ITRB paste. This
8.3.4 Follow 8.2.10 – 8.2.13 to complete the calibration of
reflectance reading must be from 2.99 through 3.01 for the the Hunter MiniScan.
duplicate pastes to be considered acceptable.
8.2.6 If the duplicate 0.1000-g Automatic Muller or 9. Procedure
0.1200-g SpeedMixer pastes are acceptable, the two duplicate
9.1 Paste Preparation:
pastes are blended together using a spatula, and the instrument
9.1.1 Automatic Muller Paste Preparation:
is set to read 3.00 using the calibration control potentiometer.
9.1.1.1 Dry the zinc oxide, ITRB, and the carbon black
8.2.7 If the duplicate pastes are unacceptable, prepare an-
sample(s) for 1 h in the specified oven set at 125 6 1°C (257
other 0.1000-g Automatic Muller or 0.1200-g SpeedMixer
6 2°F). Remove to a desiccator and allow to cool to room
paste following 9.2 – 9.3.2, and follow 8.2.5.
temperature.
8.2.8 Determine the reflectance value for all of the remain-
ing ITRB pastes of 8.1.
NOTE 4—The ITRB must be dried each day a test is performed,
preferably at the same time as the tested sample. Dry only the required
8.2.9 Calculate the tint strength of the standard pastes as
amoun
...
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: D3265 − 21 D3265 − 23
Standard Test Method for
Carbon Black—Tint Strength
This standard is issued under the fixed designation D3265; 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 test method covers the determination of the tint strength of carbon black relative to an industry tint reference black
(ITRB).
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.
2. Referenced Documents
2.1 ASTM Standards:
D1799 Practice for Carbon Black—Sampling Packaged Shipments
D1900 Practice for Carbon Black—Sampling Bulk Shipments
D4483 Practice for Evaluating Precision for Test Method Standards in the Rubber and Carbon Black Manufacturing Industries
D4821 Guide for Carbon Black—Validation of Test Method Precision and Bias
3. Summary of Test Method
3.1 A carbon black sample is mixed with a white powder (zinc oxide) and a liquid vehicle (epoxidized soybean oil, ESO) to
produce a black or gray paste. This paste is then spread to produce a surface suitable for measuring the reflectance of the mixture
by means of a photo-electric reflectance meter. The reflectance of the tested sample is then compared to the reflectance of the ITRB
prepared in the same manner. The tint strength of the tested sample is expressed as units of the reflectance of the ITRB divided
by the reflectance of the sample and multiplied by 100. The test value is therefore expressed in %.
3.2 Correction Factor:
3.2.1 A correction factor in Eq 3 is needed when raw materials Paraplex G-62 and ZnO Lot#8 or earlier produced before 2012,
in combination with ITRB2, are used. For additional details refer to ASTM D3265-17a.
This test method is under the jurisdiction of ASTM Committee D24 on Carbon Black and is the direct responsibility of Subcommittee D24.21 on Carbon Black Surface
Area and Related Properties.
Current edition approved May 1, 2021Feb. 1, 2023. Published June 2021February 2023. Originally approved in 1973. Last previous edition approved in 20192021 as
D3265 – 19b.D3265 – 21. DOI: 10.1520/D3265-21.10.1520/D3265-23.
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
D3265 − 23
3.2.2 There should be no correction applied when ITRB is used with Paraplex G-62 and ZnO Lot#8 or earlier.
3.2.3 There should be no correction applied when using the currently available tint raw materials (see Section 6) for pastes
prepared with either ITRB or ITRB2.
4. Significance and Use
4.1 For the broad range of commercial rubber grade carbon blacks, tint strength is highly dependent upon particle size. Tint
strength can be used as an indication of particle size; however, tint strength is also dependent on structure and aggregate size
distribution. Therefore, differences in tint strength within grades of carbon black may reflect differences other than particle size.
NOTE 1—This test method was developed primarily for the characterization of N100, N200, and N300 series carbon blacks.
4.2 Tint strength values within the carbon black industry have been developed using a Automatic Muller apparatus which is used
3,4
to prepare carbon black-zinc oxide pastes. A newAn alternative mixing apparatus, Hauschild SpeedMixer (DAC 150 FVZ), and
a corresponding procedure have been extensively studied within D24 and shown to provide equivalent tint strength for all carcass
or soft blacks and most tread blacks with the exception of higher surface area N100 types and specialty blacks. Therefore, it is the
responsibility of the user of this alternate apparatus to ensure their products will adequately disperse. Disputes arising between a
user and producer should be resolved using the Automatic Muller apparatus until ASTM develops adequate precision statements.
4.3 The term ITRB is used in the entire text for both, the original ITRB, used as the first reference material for tint testing, but
which is now used up, and the successor reference material, ITRB2.
5. Apparatus
5.1 Analytical Balance, with a sensitivity of 60.1 mg.
5,4
5.2 Automatic Muller.
6,4
5.3 Photometric Instrument, capable of detecting differences in the amount of light reflectance between shades of gray. The
instrument is to be operated following the manufacturer’s instructions for optimum performance.
5.4 Oven, Gravity-Convection Type, capable of temperature regulation within 61°C at 125°C (62°F at 257°F) and temperature
uniformity within 65°C (69°F).
5.5 Reflectance Standards, as required for each reflectance instrument for checking calibration.
5.6 Spatulas, 100 to 150 mm (4 to 6 in.), two, flexible, tapered.
3 3
5.7 Syringe, 5-cm , automatic refilling, reproducible to 60.02 cm .
5.8 Wiping Tissue, absorbent and lint free.
5.9 Paste Application Apparatus—Any one of the following groups of equipment may be used:
SpeedMixer is a registered trademark of FlackTek Inc., 1708 Highway 11, Bldg. G, Landrum, SC 29356. http://www.speedmixer.comThe sole source of supply of the
apparatus – Hauschild SpeedMixer®, which has been qualified for this method, including the DAC150 FVZ – known to the committee at this time is Hauschild,
www.hauschild-speedmixer.com.
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, which you may attend.
The following instruments have been found satisfactory for this test method: Hoover Automatic Muller, Model M5, Hoover Color Corp., P.O. Box 218, State Highway
693, Hiwassee, VA 24347. Automatic Pigment Muller JEL 25/53-II, J. Engelsmann AG, Frankenthaler Str. 137 – 141, 67059 Ludwigshafen, Germany, www.engelsmann.de.
The following instruments have been found satisfactory for this test method: Erichsen Tint Tester 527, available from T. J. Bell, Inc., 1340 Home Ave., Akron, OH 44310,
and Hunter MiniScan EZ, available from Hunter Associates Laboratory, Inc., 11491 Sunset Hills Road, Reston, Virginia 20190-5280.
The Hunter MiniScan XE or XE Plus may still be used for the test, but are no longer commercially available. Instructions are the same for all Hunter Miniscan types.
The Densicron reflectometer, though no longer commercially available, may be used for the test. For instructions, see Test Method D3265 – 01.
D3265 − 23
5.9.1 Apparatus for Film Drawdown Method:
7,4
5.9.1.1 Film Applicator, 0.076 mm (0.003 in.) in depth.
5.9.1.2 Polished Glass Plate, approximately 760 by 500 by 10 mm (30 by 20 by 0.375 in.).
5.9.2 Apparatus for Roller Spreader Method:
8,4
5.9.2.1 Tint Roller Spreader.
5.10 Desiccator.
3,4
5.11 SpeedMixer (DAC 150 FVZ), PP15 cups and holder.
9,4
5.12 IKA A-10 Analytical Mill, A-14 SS cutter, A-18 chamber reducer.
10,4
5.13 5 mm Glass Grinding Beads.
6. Reagents and Materials
6.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended all reagents
shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where such
specifications are available. 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.
6.2 Industry Tint Reference Black.
13,14
6.3 Plasticizer, soybean oil epoxide.
6.4 Denatured Alcohol, for cleaning purposes.
6.5 Zinc Oxide, Industry Tint Zinc Oxide.
6.6 ASTM D24 Standard Reference Blacks.
7. Sampling
7.1 Samples of shipments shall be taken in accordance with Practices D1799 and D1900.
The sole source of supply of the Film Applicator, Catalog No. 5553, known to the committee at this time is Byk-Gardner, 9104 Guilford Rd., Columbia, MD 21046,
http://www.byk.com.
The sole source of supply of the Tint Roller Spreader, Model 1A, known to the committee at this time is Titan Specialties, Inc., P.O. Box 2316, Pampa, TX 79066-2316.
The sole source of supply of the apparatus (Part #EW-04301-00) known to the committee at this time is Cole-Parmer Instrument Company, 625 East Bunker Court, Vernon
Hills, IL 60061. http://www.coleparmer.com
The sole source of supply of glass grinding beads known to the committee at this time is Quackenbush Co., Inc., 6711 Sands Rd., Crystal Lake, IL 60014.
http://www.quackco.com
Reagent Chemicals, American Chemical Society Specifications , American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed by
the American Chemical Society, see Analar 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.
The original ITRB is depleted and therefore no longer commercially available. However, any available stocks of original ITRB may still be used. The successor of the
original ITRB is ITRB2. ITRB2 was commercialized in 2012.
The sole source of supply of the epoxidized soybean oil (Greenflex 7170) known to the committee at this time is Balentine Enterprises, Inc., dba Laboratory Standards
and Technologies, 227 Somerset St., Borger, TX 79007, www.carbonstandard.com.
Supporting data (on the shelf life of this material) have been filed at ASTM International Headquarters and may be obtained by requesting Research Report
RR:D24-1004.
The sole source of supply of Industry Tint Zinc Oxide known to the committee at this time is Balentine Enterprises, Inc., dba Laboratory Standards and Technologies,
227 Somerset St., Borger, TX 79007, www.carbonstandard.com.
The sole source of supply of ASTM D24 Standard Reference Blacks known to the committee at this time is Laboratory Standards and Technologies, 227 Somerset St.,
Borger, TX 79007.
D3265 − 23
8. Calibration and Standardization
8.1 Standard Pastes—Prepare pastes of the ITRB, following 9.2 – 9.3.2 for the following masses, prepare the 0.1000-g Automatic
Muller paste or the 0.1200-g SpeedMixer paste in duplicate:
Calibration Tint
Industry Tint Reference Black
Units [%]
Automatic SpeedMixer
Muller Pastes Pastes
0.0900 g 0.1080 g 90.0
0.1000 g 0.1200 g 100.0
0.1100 g 0.1320 g 110.0
0.1200 g 0.1440 g 120.0
0.1300 g 0.1560 g 130.0
NOTE 2—Optionally, 0.1400 and 0.1500 g of Automatic Muller paste or 0.1680 and 0.1800 g of SpeedMixer paste may be added in the standardization
step when samples with tint results above 130 tint units are tested. The modified standardization should only be used for samples exceeding 130 tint units.
8.2 Erichsen Tint Tester 527:
8.2.1 Turn on the power switch and allow for 30 min warm-up.
8.2.2 Place the reflectance head on the black calibration panel and adjust the digital readout to 0.00 using the “zero” control
potentiometer.
8.2.3 Following Section 9, prepare the paste drawdown for reflectance measurement.
8.2.4 Use one of the 0.1000-g Automatic Muller or 0.1200-g SpeedMixer ITRB pastes of 8.1 to set the instrument to read 3.00
using the calibration control potentiometer.
8.2.5 Determine the reflectivity on the remaining 0.1000-g Automatic Muller or 0.1200-g SpeedMixer ITRB paste. This
reflectance reading must be from 2.99 through 3.01 for the duplicate pastes to be considered acceptable.
8.2.6 If the duplicate 0.1000-g Automatic Muller or 0.1200-g SpeedMixer pastes are acceptable, the two duplicate pastes are
blended together using a spatula, and the instrument is set to read 3.00 using the calibration control potentiometer.
8.2.7 If the duplicate pastes are unacceptable, prepare another 0.1000-g Automatic Muller or 0.1200-g SpeedMixer paste following
9.2 – 9.3.2, and follow 8.2.5.
8.2.8 Determine the reflectance value for all of the remaining ITRB pastes of 8.1.
8.2.9 Calculate the tint strength of the standard pastes as follows:
Tint % 5 3.00/S ×100 (1)
@ #
where:
S = reflectance value of sample.
8.2.10 Calculate a regression of the standard values (y value) on the measured values (x value) by using the least squares method.
8.2.11 The measured tint strength of all subsequent samples is corrected by substituting each measured value into this linear
equation and calculating the corrected value for the tint strength.
8.2.12 New regression coefficients are determined periodically, typically on a monthly basis.
NOTE 3—Proper paste preparation and regression may be validated by analyzing at least one SRB tread grade (SRB A-C). After applying the normalization
to the tint pastes and calculation as described in Section 10 the tested SRB samples should be within the accuracy limits given in Guide D4821.
8.2.13 Proper calibration and standardization of the equipment, reagents, materials, and method shall be checked on a periodic
D3265 − 23
basis using ASTM D24 Standard Reference Blacks. The standard tint strength values and the acceptable test limit of the standard
reference blacks may be found in Guide D4821.
8.3 Hunter MiniScan:
8.3.1 Calibrate the instrument using the black and white tiles.
8.3.2 Place the instrument in Setup Mode. Set up instrument with XYZ color scale, D65 illuminant, 10° observer, average a
minimum of three readings. (Note that Y corresponds to the lightness/darkness function, and thus represents the information of
interest).
8.3.3 Read each of
...
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: D3265 − 23
Standard Test Method for
Carbon Black—Tint Strength
This standard is issued under the fixed designation D3265; 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 to produce a black or gray paste. This paste is then spread to
produce a surface suitable for measuring the reflectance of the
1.1 This test method covers the determination of the tint
mixture by means of a photo-electric reflectance meter. The
strength of carbon black relative to an industry tint reference
reflectance of the tested sample is then compared to the
black (ITRB).
reflectance of the ITRB prepared in the same manner. The tint
1.2 The values stated in SI units are to be regarded as the
strength of the tested sample is expressed as units of the
standard. The values given in parentheses are for information
reflectance of the ITRB divided by the reflectance of the
only.
sample and multiplied by 100. The test value is therefore
1.3 This standard does not purport to address all of the expressed in %.
safety concerns, if any, associated with its use. It is the
3.2 Correction Factor:
responsibility of the user of this standard to establish appro-
3.2.1 A correction factor in Eq 3 is needed when raw
priate safety, health, and environmental practices and deter-
materials Paraplex G-62 and ZnO Lot#8 or earlier produced
mine the applicability of regulatory limitations prior to use.
before 2012, in combination with ITRB2, are used. For
1.4 This international standard was developed in accor-
additional details refer to ASTM D3265-17a.
dance with internationally recognized principles on standard-
3.2.2 There should be no correction applied when ITRB is
ization established in the Decision on Principles for the
used with Paraplex G-62 and ZnO Lot#8 or earlier.
Development of International Standards, Guides and Recom-
3.2.3 There should be no correction applied when using the
mendations issued by the World Trade Organization Technical
currently available tint raw materials (see Section 6) for pastes
Barriers to Trade (TBT) Committee.
prepared with either ITRB or ITRB2.
2. Referenced Documents
4. Significance and Use
2.1 ASTM Standards:
4.1 For the broad range of commercial rubber grade carbon
D1799 Practice for Carbon Black—Sampling Packaged
blacks, tint strength is highly dependent upon particle size. Tint
Shipments
strength can be used as an indication of particle size; however,
D1900 Practice for Carbon Black—Sampling Bulk Ship-
tint strength is also dependent on structure and aggregate size
ments
distribution. Therefore, differences in tint strength within
D4483 Practice for Evaluating Precision for Test Method
grades of carbon black may reflect differences other than
Standards in the Rubber and Carbon Black Manufacturing
particle size.
Industries
NOTE 1—This test method was developed primarily for the character-
D4821 Guide for Carbon Black—Validation of Test Method
ization of N100, N200, and N300 series carbon blacks.
Precision and Bias
4.2 Tint strength values within the carbon black industry
3. Summary of Test Method
have been developed using a Automatic Muller apparatus
3.1 A carbon black sample is mixed with a white powder which is used to prepare carbon black-zinc oxide pastes. An
3,4
alternative mixing apparatus, Hauschild SpeedMixer (DAC
(zinc oxide) and a liquid vehicle (epoxidized soybean oil, ESO)
150 FVZ), and a corresponding procedure have been exten-
sively studied within D24 and shown to provide equivalent tint
This test method is under the jurisdiction of ASTM Committee D24 on Carbon
strength for all carcass or soft blacks and most tread blacks
Black and is the direct responsibility of Subcommittee D24.21 on Carbon Black
Surface Area and Related Properties.
Current edition approved Feb. 1, 2023. Published February 2023. Originally
approved in 1973. Last previous edition approved in 2021 as D3265 – 21. DOI: The sole source of supply of the apparatus – Hauschild SpeedMixer®, which
10.1520/D3265-23. has been qualified for this method, including the DAC150 FVZ – known to the
For referenced ASTM standards, visit the ASTM website, www.astm.org, or committee at this time is Hauschild, www.hauschild-speedmixer.com.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM If you are aware of alternative suppliers, please provide this information to
Standards volume information, refer to the standard’s Document Summary page on ASTM International Headquarters. Your comments will receive careful consider-
the ASTM website. ation at a meeting of the responsible technical committee, which you may attend.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3265 − 23
3,4
with the exception of higher surface area N100 types and 5.11 SpeedMixer (DAC 150 FVZ), PP15 cups and holder.
specialty blacks. Therefore, it is the responsibility of the user of
5.12 IKA A-10 Analytical Mill, A-14 SS cutter, A-18 cham-
this alternate apparatus to ensure their products will adequately
9,4
ber reducer.
disperse. Disputes arising between a user and producer should
10,4
be resolved using the Automatic Muller apparatus until ASTM 5.13 5 mm Glass Grinding Beads.
develops adequate precision statements.
6. Reagents and Materials
4.3 The term ITRB is used in the entire text for both, the
original ITRB, used as the first reference material for tint
6.1 Purity of Reagents—Reagent grade chemicals shall be
testing, but which is now used up, and the successor reference
used in all tests. Unless otherwise indicated, it is intended all
material, ITRB2.
reagents shall conform to the specifications of the Committee
on Analytical Reagents of the American Chemical Society,
5. Apparatus
where such specifications are available. Other grades may be
used, provided it is first ascertained that the reagent is of
5.1 Analytical Balance, with a sensitivity of 60.1 mg.
5,4 sufficiently high purity to permit its use without lessening the
5.2 Automatic Muller.
accuracy of the determination.
5.3 Photometric Instrument, capable of detecting differ-
6.2 Industry Tint Reference Black.
ences in the amount of light reflectance between shades of
6,4
13,14
gray. The instrument is to be operated following the manu-
6.3 Plasticizer, soybean oil epoxide.
facturer’s instructions for optimum performance.
6.4 Denatured Alcohol, for cleaning purposes.
5.4 Oven, Gravity-Convection Type, capable of temperature
regulation within 61°C at 125°C (62°F at 257°F) and 6.5 Zinc Oxide, Industry Tint Zinc Oxide.
temperature uniformity within 65°C (69°F).
6.6 ASTM D24 Standard Reference Blacks.
5.5 Reflectance Standards, as required for each reflectance
instrument for checking calibration.
7. Sampling
5.6 Spatulas, 100 to 150 mm (4 to 6 in.), two, flexible,
7.1 Samples of shipments shall be taken in accordance with
tapered.
Practices D1799 and D1900.
5.7 Syringe, 5-cm , automatic refilling, reproducible to
60.02 cm . 8. Calibration and Standardization
5.8 Wiping Tissue, absorbent and lint free.
8.1 Standard Pastes—Prepare pastes of the ITRB, following
9.2 – 9.3.2 for the following masses, prepare the 0.1000-g
5.9 Paste Application Apparatus—Any one of the following
Automatic Muller paste or the 0.1200-g SpeedMixer paste in
groups of equipment may be used:
duplicate:
5.9.1 Apparatus for Film Drawdown Method:
7,4
5.9.1.1 Film Applicator, 0.076 mm (0.003 in.) in depth.
5.9.1.2 Polished Glass Plate, approximately 760 by 500 by
10 mm (30 by 20 by 0.375 in.). 9
The sole source of supply of the apparatus (Part #EW-04301-00) known to the
5.9.2 Apparatus for Roller Spreader Method: committee at this time is Cole-Parmer Instrument Company, 625 East Bunker Court,
8,4
Vernon Hills, IL 60061. http://www.coleparmer.com
5.9.2.1 Tint Roller Spreader.
The sole source of supply of glass grinding beads known to the committee at
5.10 Desiccator. this time is Quackenbush Co., Inc., 6711 Sands Rd., Crystal Lake, IL 60014.
http://www.quackco.com
Reagent Chemicals, American Chemical Society Specifications , American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
The following instruments have been found satisfactory for this test method: listed by the American Chemical Society, see Analar Standards for Laboratory
Hoover Automatic Muller, Model M5, Hoover Color Corp., P.O. Box 218, State Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Highway 693, Hiwassee, VA 24347. Automatic Pigment Muller JEL 25/53-II, J. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Engelsmann AG, Frankenthaler Str. 137 – 141, 67059 Ludwigshafen, Germany, MD.
www.engelsmann.de. The original ITRB is depleted and therefore no longer commercially available.
The following instruments have been found satisfactory for this test method: However, any available stocks of original ITRB may still be used. The successor of
Erichsen Tint Tester 527, available from T. J. Bell, Inc., 1340 Home Ave., Akron, the original ITRB is ITRB2. ITRB2 was commercialized in 2012.
OH 44310, and Hunter MiniScan EZ, available from Hunter Associates Laboratory, The sole source of supply of the epoxidized soybean oil (Greenflex 7170)
Inc., 11491 Sunset Hills Road, Reston, Virginia 20190-5280. known to the committee at this time is Balentine Enterprises, Inc., dba Laboratory
The Hunter MiniScan XE or XE Plus may still be used for the test, but are no Standards and Technologies, 227 Somerset St., Borger, TX 79007, www.carbon-
longer commercially available. Instructions are the same for all Hunter Miniscan standard.com.
types. Supporting data (on the shelf life of this material) have been filed at ASTM
The Densicron reflectometer, though no longer commercially available, may be International Headquarters and may be obtained by requesting Research Report
used for the test. For instructions, see Test Method D3265 – 01. RR:D24-1004.
7 15
The sole source of supply of the Film Applicator, Catalog No. 5553, known to The sole source of supply of Industry Tint Zinc Oxide known to the committee
the committee at this time is Byk-Gardner, 9104 Guilford Rd., Columbia, MD at this time is Balentine Enterprises, Inc., dba Laboratory Standards and
21046, http://www.byk.com. Technologies, 227 Somerset St., Borger, TX 79007, www.carbonstandard.com.
8 16
The sole source of supply of the Tint Roller Spreader, Model 1A, known to the The sole source of supply of ASTM D24 Standard Reference Blacks known to
committee at this time is Titan Specialties, Inc., P.O. Box 2316, Pampa, TX the committee at this time is Laboratory Standards and Technologies, 227 Somerset
79066-2316. St., Borger, TX 79007.
D3265 − 23
on a periodic basis using ASTM D24 Standard Reference
Calibration Tint
Industry Tint Reference Black
Units [%]
Blacks. The standard tint strength values and the acceptable
Automatic SpeedMixer
test limit of the standard reference blacks may be found in
Muller Pastes Pastes
Guide D4821.
0.0900 g 0.1080 g 90.0
0.1000 g 0.1200 g 100.0
8.3 Hunter MiniScan:
0.1100 g 0.1320 g 110.0
0.1200 g 0.1440 g 120.0
8.3.1 Calibrate the instrument using the black and white
0.1300 g 0.1560 g 130.0
tiles.
NOTE 2—Optionally, 0.1400 and 0.1500 g of Automatic Muller paste or
8.3.2 Place the instrument in Setup Mode. Set up instrument
0.1680 and 0.1800 g of SpeedMixer paste may be added in the standard-
with XYZ color scale, D65 illuminant, 10° observer, average a
ization step when samples with tint results above 130 tint units are tested.
minimum of three readings. (Note that Y corresponds to the
The modified standardization should only be used for samples exceeding
130 tint units. lightness/darkness function, and thus represents the informa-
tion of interest).
8.2 Erichsen Tint Tester 527:
8.3.3 Read each of the ITRB pastes at least three times and
8.2.1 Turn on the power switch and allow for 30 min
record only the average Y value of the three readings. The Y
warm-up.
value for the 0.1000-g Automatic Muller or 0.1200-g Speed-
8.2.2 Place the reflectance head on the black calibration
Mixer paste should read approximately 2.60. Calculate the tint
panel and adjust the digital readout to 0.00 using the “zero”
strength of the ITRB pastes as follows:
control potentiometer.
8.2.3 Following Section 9, prepare the paste drawdown for Tint % 5 I/Y × 100 (2)
@ #
reflectance measurement.
where:
8.2.4 Use one of the 0.1000-g Automatic Muller or 0.1200-g
I = reflectance of 0.1000-g Automatic Muller or 0.1200-g
SpeedMixer ITRB pastes of 8.1 to set the instrument to read
SpeedMixer ITRB paste.
3.00 using the calibration control potentiometer.
Y = reflectance value of sample.
8.2.5 Determine the reflectivity on the remaining 0.1000-g
Automatic Muller or 0.1200-g SpeedMixer ITRB paste. This 8.3.4 Follow 8.2.10 – 8.2.13 to complete the calibration of
reflectance reading must be from 2.99 through 3.01 for the
the Hunter MiniScan.
duplicate pastes to be considered acceptable.
8.2.6 If the duplicate 0.1000-g Automatic Muller or 9. Procedure
0.1200-g SpeedMixer pastes are acceptable, the two duplicate
9.1 Paste Preparation:
pastes are blended together using a spatula, and the instrument
9.1.1 Automatic Muller Paste Preparation:
is set to read 3.00 using the calibration control potentiometer.
9.1.1.1 Dry the zinc oxide, ITRB, and the carbon black
8.2.7 If the duplicate pastes are unacceptable, prepare an-
sample(s) for 1 h in the specified oven set at 125 6 1°C (257
other 0.1000-g Automatic Muller or 0.1200-g SpeedMixer
6 2°F). Remove to a desiccator and allow to cool to room
paste following 9.2 – 9.3.2, and follow 8.2.5.
temperature.
8.2.8 Determine the reflectance value for all of the remain-
ing ITRB pastes of 8.1.
NOTE 4—The ITRB must be dried each day a test is performed,
8.2.9 Calculate the tint strength of the standard pastes as preferably at the same time as the tested sample. Dry only the required
amount, as the ITRB should not be dried repeatedly.
follows:
NOTE 5—As an optional
...












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