ASTM D3265-00

Standard Test Method for Carbon Black—Tint Strength

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 and health practices and determine the applicability of regulatory limitations prior to use.

General Information

• Status: Historical
• Publication Date: 09-Dec-2001
• ICS: 83.040.20 - Rubber compounding ingredients
• Technical Committee: D24 - Carbon Black
• Drafting Committee: D24.11 - Carbon Black Structure

Relations

• Replaced By: ASTM D3265-01 - Standard Test Method for Carbon Black—Tint Strength
• Effective Date: 10-Dec-2001
• Referred By: ASTM D4122-17(2023) - Standard Practice for Carbon Black—Evaluation of an Industry Reference Black
• Effective Date: 10-Dec-2001
• Referred By: ASTM D4821-20 - Standard Guide for Carbon Black—Validation of Test Method Precision and Bias
• Effective Date: 10-Dec-2001
• Referred By: ASTM D7849-23 - Standard Classification for Nomenclature of Reference Materials of Committee D24
• Effective Date: 10-Dec-2001
• Referred By: ASTM D5817-20 - Standard Practice for Carbon Black, Pelleted—Reduction, Blending, and Drying of Gross Samples for Testing
• Effective Date: 10-Dec-2001
• Referred By: ASTM D1765-23a - Standard Classification System for Carbon Blacks Used in Rubber Products
• Effective Date: 10-Dec-2001
• Referred By: ASTM D3053-23 - Standard Terminology Relating to Carbon Black
• Effective Date: 10-Dec-2001
• Referred By: ASTM D6915-23 - Standard Practice for Carbon Black—Evaluation of Standard Reference Blacks
• Effective Date: 10-Dec-2001

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 3265 – 00
Standard Test Method for
Carbon Black—Tint Strength
This standard is issued under the fixed designation D 3265; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope strength can be used as an indication of particle size; however,
tint strength is also dependent on structure and aggregate size
1.1 This test method covers the determination of the tint
distribution. Therefore, differences in tint strength within
strength of carbon black relative to an industry tint reference
grades of carbon black may reflect differences other than
black (ITRB).
particle size.
1.2 The values stated in SI units are to be regarded as the
standard. The values given in parentheses are for information
NOTE 1—This test method was developed primarily for the character-
only.
ization of N100, N200, and N300 series carbon blacks.
1.3 This standard does not purport to address all of the
5. Apparatus
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 5.1 Analytical Balance, with a sensitivity of 60.1 mg.
5.2 Automatic Muller.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. 5.3 Photometric Instrument, capable of detecting differ-
ences in the amount of light reflectance between shades of
2. Referenced Documents
gray. The instrument is to be operated following the manu-
2.1 ASTM Standards: facturer’s instructions for optimum performance.
D 1799 Practice for Carbon Black—Sampling Packaged 5.4 Oven, Gravity-Convection Type, capable of temperature
Shipments regulation within 61°C at 125°C (62°F at 257°F) and
D 1900 Practice for Carbon Black—Sampling Bulk Ship- temperature uniformity within6 5°C (69°F).
ments 5.5 Reflectance Standards, as required for each reflectance
D 3324 Practice for Carbon Black—Improving Test Repro- instrument for checking calibration.
ducibility Using ASTM Reference Blacks 5.6 Spatulas, 100 to 150 mm (4 to 6 in.), two, flexible,
D 4483 Practice for Determining Precision for Test Method tapered.
2 3
Standards in the Rubber and Carbon Black Industries 5.7 Syringe, 5-cm , automatic refilling, reproducible to 6
0.02 cm .
3. Summary of Test Method
5.8 Wiping Tissue, absorbent and lint free.
3.1 A carbon black sample is mixed with a white powder
5.9 Paste Application Apparatus—Any one of the following
(zinc oxide) and a liquid vehicle (soybean oil epoxide) to groups of equipment may be used:
produce a black or gray paste. This paste is then spread to
5.9.1 Apparatus for Film Drawdown Method:
produce a surface suitable for measuring the reflectance of the 5.9.1.1 Film Applicator, 0.076 mm (0.003 in.) in depth.
mixture by means of a photo-electric reflectance meter. The 5.9.1.2 Polished Glass Plate, approximately 760 by 500 by
reflectance of the tested sample is then compared to the
10 mm (30 by 20 by 0.375 in.).
reflectance of the ITRB prepared in the same manner. The tint 5.9.2 Apparatus for Roller Spreader Method:
strength of the tested sample is expressed as units of the
reflectance of the ITRB divided by the reflectance of the
Hoover Automatic Muller, Model M5, available from Hoover Color Corp., P.O.
sample and multiplied by 100.
Box 218, State Highway 693, Hiwassee, VA 24347, has been found satisfactory for
this test method.
4. Significance and Use
The following instruments have been found satisfactory for this test method:
Erichsen Tint Tester 527, available from T. G. Bell, Inc., 1340 Home Ave.,
4.1 For the broad range of commercial rubber grade carbon
Akron, OH 44310; Densichron Reflectometer, Catalog No. 3837, composed of the
blacks, tint strength is highly dependent upon particle size. Tint
following parts: Model 1 Photometer-Linear Scale, Catalog No. 3830D; Reflection
Head, Catalog No. 3832A; Regulated 6-V Transformer, Catalog No. 3834M;
Reflection Tile Set (Standard), Catalog No. 3827T, available from Sargent-Welch
This test method is under the jurisdiction of ASTM Committee D24 on Carbon Scientific Co., Densichron Div., 7300 N. Lander Ave., Skokie, IL 60076. This model
Black and is the direct responsibility of Subcommittee D24.11 on Absorptive is no longer available and the suggested replacement model 3867 B has not been
Properties of Carbon Black. found to be satisfactory. Hunter MiniScan XE or XE Plus, available from Hunter
Current edition approved May 10, 2000. Published June 2000. Originally Associates Laboratory, Inc., 11491 Sunset Hills Road, Reston, Virginia 22090-5280.
published as D 3265 – 73. Last previous edition D 3265 – 99a. Film Applicator, Catalog No. AR-3800F, available from Pacific Scientific Co.,
Annual Book of ASTM Standards, Vol 09.01. 2431 Linden Ln., Silver Spring, MD 20910.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 3265
5.9.2.1 Tint Roller Spreader. 8.2.4 If the duplicate pastes are unacceptable, prepare an-
5.10 Desiccator. other 0.1000-g paste following 9.1-9.9. Repeat 8.2.1 and 8.2.2
with the new paste, and blend it with whichever of the previous
6. Reagents and Materials
0.1000-g pastes which will satisfy the limits of 8.2.2. Repeat
6.1 Purity of Reagents—Reagent grade chemicals shall be 8.2.1 using this blend.
used in all tests. Unless otherwise indicated, it is intended all
8.2.5 Following 9.10 and 9.12, determine the reflectance
reagents shall conform to the specifications of the Committee
value for all of the remaining ITRB pastes of 8.1.
on Analytical Reagents of the American Chemical Society,
8.2.6 Calculate the tint strength for the standard pastes as
where such specifications are available. Other grades may be
follows:
used, provided it is first ascertained that the reagent is of
Tint Units 5 80/S 3 100 (1)
sufficiently high purity to permit its use without lessening the
accuracy of the determination. where:
S 5 reflectance value of sample.
6.2 Industry Tint Reference Black.
6.3 Plasticizer, soybean oil epoxide. 8.2.7 If the measured tint values are not within the guide-
lines (60.8 % relative of the target tint strength values) given
6.4 Solvent, cleaning, low toxicity, and nonflammable.
6.5 Zinc Oxide, Industry Tint Zinc Oxide. in 8.1, then a regression of the standard values (y value) on the
measured values (x value) must be calculated using the least
6.6 ASTM D-24 Standard Reference Blacks.
squares method.
7. Sampling
NOTE 2—It is almost always necessary to develop a statistical equation
7.1 Samples of shipments shall be taken in accordance with
to measure tint strength values.
Practices D 1799 and D 1900.
8.2.8 The measured tint strength of all subsequent samples
8. Calibration and Standardization shall then be corrected by substituting each measured value
into this linear equation and calculating the corrected value for
8.1 Standard Pastes— Prepare pastes of the ITRB, follow-
the tint strength.
ing 9.1-9.9 for the following masses, prepare the 0.1000-g
8.2.9 New registration coefficients are determined periodi-
paste in duplicate:
cally, typically on a monthly basis.
Industry Tint Reference Black
(g in 10.2 mixture) Calibration Tint Units Acceptable Range 8.2.10 Proper calibration and standardization of the equip-
ment, reagents, materials, and method shall be checked on a
0.0900 90.0 89.3 – 90.7
periodic basis using the ASTM D-24 Standard Reference
0.1000 100.0 99.2 – 100.8
0.1100 110.0 109.1 – 110.9 Blacks. The standard tint strength values and the acceptable
0.1200 120.0 119.0 – 121.0
test limit of the standard reference blacks may be found in
0.1300 130.0 129.0 – 131.0
Practice D 3324.
8.2 Densichron Reflectometer
8.3 Erichsen Tint Tester 527:
8.2.1 Following 9.10 and 9.11, use one of the 0.1000-g (100
8.3.1 Turn on the power switch and allow for 30 min
tint units) ITRB pastes to set the instrument to an 80 reflectance
warm-up.
value.
8.3.2 Place the reflectance head on the black calibration
8.2.2 Following 9.10 and 9.12, determine the reflectivity of
panel and adjust the digital readout to 0.00 using the “zero”
the remaining 0.1000-g paste. The reflectance reading must be
control potentiometer.
from 79.5 to 80.5 for the duplicate pastes to be considered
8.3.3 Following 9.10, prepare the paste drawdown for
acceptable.
reflectance measurement.
8.2.3 If the duplicate 0.1000-g pastes are acceptable, the two
8.3.4 Use one of the 0.1000-g ITRB pastes of 8.1 to set the
are blended together using a spatula, and repeat 8.2.1 using this
instrument to read 3.00 using the calibration control potenti-
blend.
ometer.
8.3.5 Determine the reflectivity on the remaining 0.1000-g
ITRB paste. This reflectance reading must be from 2.99
Tint Roller Spreader, Model 1A, available from Titan Specialties, Inc., P.O Box
through 3.01 for the duplicate pastes to be considered accept-
2316, Pampa, TX 79066-2316 has been found satisfactory for this test method.
able.
“Reagent Chemicals, American Chemical Society Specifications,” Am. Chemi-
cal Soc., Washington, DC. For suggestions on the testing of reagents not listed by
8.3.6 Follow 8.2.3 and 8.2.4.
the American Chemical Society, see “Analar Standards for Laboratory U.K.
8.3.7 Determine the reflectance value for all of the remain-
Chemicals,” BDH Ltd., Poole, Dorset, and the “United States Pharmacopeia.”
ing ITRB pastes of 8.1.
Industry Tint Reference Black, an N-330 carbon black, is available from Titan
Specialties, Inc., P.O. Box 2316, Pampa, TX 79066-2316.
8.3.8 Calculate the tint strength of the standard pastes as
Chemical Abstracts Registry Number 12768-71-7,“ Paraplex G-62,” available
follows:
from C. P. Hall Co., Technical Center, Customer Service Department, 5851 West
73rd St., Chicago, IL, 60638 (312/767-4600). Minimum order is 5 gals and order
Tint Units 5 3.00/S 3 100 (2)
should state “Refer to ASTM D3265.” A report on the shelf life of this material is
filed at ASTM Headquarters. Request RR: D24-1004.
where:
1,1,1-trichloroethane has been found satisfactory for this test method.
S 5 reflectance value of sample
Available from Forcoven Products, Inc., P.O. Box 1556, Humble, TX 77347.
8.3.9 Follow 8.2.7-8.2.10 to complete calibration of the
F-4 will be used until depleted, at which time F-5 will be used. Available from
Titan Specialties, Inc., P.O. Box 2316, Pampa, TX 79066-2316. Erichsen Tint Tester.
D 3265
8.4 Hunter MiniScan: the muller plates, using a solvent and wiping tissue.
8.4.1 Calibrate the instrument using the black and white 9.10 Prepare the paste for reflectance measurement by one
tiles. of the following methods:
8.4.2 Place the instrument in Setup mode. Setup instrument 9.10.1 Film Drawdown Method:
with XYZ color scale, D65 illuminant, 10° observer, average a 9.10.1.1 Clean the glass plate with a wiping tissue to
minimum of 3 readings. (Note that Y corresponds to the remove any dust particles or film.
lightness/darkness function, and thus represents the informa- 9.10.1.2 Use a spatula to place a portion of the paste near
tion of interest). the top edge of the glass plate.
8.4.3 Read each of the ITRB pastes at least three times and 9.10.1.3 Using a film applicator and applying moderate,
record only the average Y value of the three readings. The Y consistent pressure, draw down the paste to the bottom edge in
value for the 0.1000g paste should read approximately 2.60. 2to3s.
Calculate the tint strength of the ITRB pastes as follows: 9.10.1.4 Pick up the applicator without removing the excess
paste adhered to it; return it to the beginning of the drawdown,
Tint 5 2.60/Y X100 (3)
and again draw down the paste to the bottom edge of the glass
where:
plate in 2 to 3 s. The drawdown shall have a uniform surface
Y 5 reflectance value of sample
approximately 65 mm (2.5 in.) wide. If the surface is not
8.4.4 Follow 8.2.7-8.2.10 to complete the calibration of the
uniform, prepare another drawdown.
Hunter MiniScan.
NOTE 5—The wet film thickness of the drawdown has a nominal
thickness of 0.04 mm (0.0015 in.), or approximately one half the actual
9. Procedure
gap clearance of the applicator.
9.1 Dry the zinc oxide, ITRB, and the carbon black
9.10.2 Roller Spreader Method:
sample(s) for1hinthe specified oven set at 125 6 1°C (257
9.10.2.1 No preparation of the paste is required, for it is
6 2°F). Remove to a desiccator and allow to cool to room
placed directly on the turning roller of the tint roller spreader.
temperature.
9.11 Adjust the reflectance instrument as follows:
NOTE 3—The ITRB must be dried each day a test is performed, 9.11.1 Densichron Reflectometer-Film Drawdown Method:
preferably at the same time as the tested sample. Dry only the required
9.11.1.1 Set the range switch on 2 and the reflection head
amount, as the ITRB should not be dried repeatedly.
with no filter.
9.2 Weigh a sample of exactly 0.1000 g of carbon black into
NOTE 6—Use the ⁄16-in. aperture if reflection head No. 3882A with the
a weighing dish and then weigh onto the carbon black 3.7500
variable aperture sizes is used in place of the recommended No. 3832A.
g of zinc oxide. For N500, N600, N700 series carbon blacks,
NOTE 7—When the light source in reflection head No. 3832A is
weigh exactly 0.2000 g of carbon black and 3.7500 g of zinc replaced, refer to the instrument instruction manual for the method of
checking correct alignment of the new bulb.
oxide.
9.3 Using the syringe, place 2.20 6 0.02 cm or, if
9.11.1.2 Disregarding the first 75 mm (3 in.) at the top of the
preferred, 2.20 g of plasticizer in the center of the mulling
drawdown, set the reflection head aperture over the drawdown
plate.
of the ITRB paste.
9.11.1.3 Adjust the Densichron reflectometer to read an
NOTE 4—If the use of 2.20 cm (2.20 g) of plasticizer produces an
3 average value of 80 for at least four readings taken at different
unmanageable fluid paste, then it is acceptable to use 2.00 cm (2.00 g) of
positions. All readings shall be taken after the instrument
plasticizer for both the ITRB standard and the sample.
stabilizes at a new position, usually in 15 to 20 s.
9.4 Place the zinc oxide and carbon black in the center of
the pool of plasticizer. NOTE 8—The black tile working standard, supplied with the Den-
sichron reflectometer, may be used as a secondary standard by reading its
9.5 Mix the three materials with a spatula, confining them as
reflectance value after the Densichron reflectometer has been adjusted to
close to the center as possible; mix until they are well
an 80 average reflectance value on the ITRB paste. The tile reflectance
incorp
...