Determination of Strength of Colorants and Bases For Architectural, Marine, Maintenance, Commercial, and Industrial Coatings

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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: D8163 − 18

Standard Test Method for


Determination of Strength of Colorants and Bases for
Architectural, Marine, Maintenance, Commercial, and
Industrial Coatings1
This standard is issued under the fixed designation D8163; 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 ization established in the Decision on Principles for the


1.1 This test method covers the determination of strength of Development of International Standards, Guides and Recom-
colorant dispersions, colored and white bases, for architectural, mendations issued by the World Trade Organization Technical
marine, maintenance, commercial, and industrial coatings. Barriers to Trade (TBT) Committee.
1.2 This test method applies to colorant dispersions and 2. Referenced Documents
colored and white bases regardless of the methods used to
disperse these materials. 2.1 ASTM Standards:2
1.3 The resultant test value is in terms of percent strength in D823 Practices for Producing Films of Uniform Thickness
which a material stronger than standard is implied by values of Paint, Coatings and Related Products on Test Panels
larger than 100 % and weaker than standard is implied by D1475 Test Method for Density of Liquid Coatings, Inks,
values less than 100 %. The value of 100 % implies exact and Related Products
strength conformance to the test method. D3964 Practice for Selection of Coating Specimens for
Appearance Measurements
1.4 This test method is suitable for the determination of E284 Terminology of Appearance
strength when tolerances are set about standards that are E308 Practice for Computing the Colors of Objects by Using
prepared either by weight concentration or volume concentra- the CIE System
tion. E1164 Practice for Obtaining Spectrometric Data for Object-
1.5 The test result is empirically determined. The user Color Evaluation
determines and supplies the standard for strength of the product E1331 Test Method for Reflectance Factor and Color by
under test and the test result is relative to that supplied Spectrophotometry Using Hemispherical Geometry
standard. E1349 Test Method for Reflectance Factor and Color by
1.6 The values stated in either SI units or inch-pound units Spectrophotometry Using Bidirectional (45°:0° or 0°:45°)
are to be regarded separately as standard. The values stated in Geometry
each system may not be exact equivalents; therefore, each
system shall be used independently of the other. Combining 3. Terminology
values from the two systems may result in non-conformance 3.1 Definitions: Terms and definitions in Terminology E284
with the standard. are applicable to this test method.
1.7 This standard does not purport to address all of the 3.1.1 reflection factor, n—in strength of colorant or base, a
safety concerns, if any, associated with its use. It is the value representative of the fraction of incident radiant energy
responsibility of the user of this standard to establish appro- that is reflected from a surface under conditions specified.
priate safety, health, and environmental practices and deter-
3.1.2 strength, n—of a colorant or base, a value that is
mine the applicability of regulatory limitations prior to use.
quantitatively related to the effective concentration of a test
1.8 This international standard was developed in accor-
colorant or test base relative to the effective concentration of
dance with internationally recognized principles on standard-
the standard or reference for that colorant or base.
1
This test method is under the jurisdiction of ASTM Committee D01 on Paint
and Related Coatings, Materials, and Applications and is the direct responsibility of
2
Subcommittee D01.26 on Optical Properties. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved June 1, 2018. Published June 2018. Originally contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
approved in 2017. Last previous edition approved in 2017 as D8163 – 17. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D8163-18. the ASTM website.

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

1
D8163 − 18
4. Summary of Test Method marked with values that are half these dimensions and so
4.1 The user supplies a standard base and a standard would be marked 100 and 150 µm [4 and 6 mils], respectively.
colorant. A standard sample is prepared from these ingredients Under some circumstances, drawdown bars with other clear-
by a predetermined formula that will achieve a target reflec- ances may be appropriately used.
tance. A test sample is made using the same formula by mixing 7.5 Apparatus to hold the drawdown chart in place while the
the material being tested with the appropriate standard material drawdown is made and this may consist of a glass plate or a
depending upon whether the material under test is a colorant or vacuum plate to hold the drawdown flat on a smooth and level
a base. surface.
4.2 The standard sample and the test sample are drawn 7.6 Color Measuring Instrument: a colorimetric spectropho-
down side by side on a black-and-white test chart. tometer meeting the requirements of Practice E1164 having a
4.3 The drawdown is dried by appropriate means, and the spectral range of at least 400 to 700 nm at 10 nm intervals and
spectral reflectance factor of each standard and sample are having a measuring port ideally 25 mm in size, and measuring
measured on a spectrophotometer. Total:Normal (di:0), sometimes called SPIN or SIN.
Alternatively, but less desirably, one may utilize a smaller
4.4 A value is selected, or calculated, from among the measuring aperture and measuring geometry Diffuse:Normal
spectrophotometric reflection functions to represent the relative (de:0), 45°:Normal (45:0) or (0:45).
reflection factors of each of the two specimens.
4.5 These two values are converted by calculation to optical 8. Reagents and Materials
parameters, K-over-S, where K is the Kubelka-Munk absorp- 8.1 Users are responsible for providing standard strength
tion coefficient and S the Kubelka-Munk scattering coefficient. white base and standard strength colorants for each colorant or
These values are appropriately put in ratio with each other and base put under test. These materials will have to be replaced
multiplied by 100 to achieve the test value, relative strength in when they are depleted, and special care shall be taken that the
percent of the standard value. The ratio assumes that the optical replacement materials have exact continuity of strength with
parameters are directly, linearly proportional to the relative the materials they are replacing.
concentration of the dispersed media in the range of concen-
tration used in the test. 9. Calibration and Standardization
9.1 Verify the calibration of the weight per gallon cup at
5. Significance and Use
least once each month in accordance with the instructions for
5.1 The test method results are suitable for use by manu- doing so in accordance with Test Method D1475.
facturers of colorants and bases for quality control purposes on
9.2 Verify the calibration of the spectrophotometer at least
manufactured product.
once each month in accordance with Practice E1164 in which
5.2 The test method results are suitable for use by purchas- this process is called standardization and verification.
ers of colorants and bases for incoming quality control or the
determination of money value of colorants and bases. 10. Conditioning
6. Interferences 10.1 Assure that all materials have been shaken on a paint
shaker for at least 2 min on the day on which they will be used.
6.1 Differences between the standard and the test materials
in the following properties may be interpreted by the test 10.2 The viscosity ranges of most materials within the scope
method as a strength difference and thus comprise an interfer- of this test method are such that the vigorous shaking necessary
ence with the test: color difference between the standard to homogenization of the materials causes air to be entrapped
specimen and the test specimen in the hue or chroma in the liquid. As part of the sample conditioning, users shall
directions, gloss difference, metamerism, measurement geom- employ at least one of the three methods given in Test Method
etry differences, hiding differences, and flocculation differ- D1475 for the removal of air from the sample. The methods are
ences. centrifugation, vacuum deaeration, and reduction of viscosity
with solvent, including water if applicable. Only the sample
6.2 The presence of any one or more of these interferences under current consideration need be deaerated, not the entire
could invalidate the test results. stored standard material.
7. Apparatus 11. Procedure
7.1 Electronic Scale, with readability of at least 0.001 g and
resolution of at least 0.01 g. METHOD A
7.2 Weight per gallon cup if strength is assessed by volume. 11.1 Colorant Test Method:
11.1.1 Prepare a wet standard by blending an amount of
7.3 Black-and-white sealed drawdown charts. standard white base and standard colorant to achieve a reflec-
7.4 Drawdown Bars, capable of applying a coating typically tance at the wavelength of maximum absorption of between 35
15.25 cm [6 in.] wide. The applicators shall be capable of and 50 % reflectance with 40 % reflectance considered ideal.
applying 200 and 300 µm [8 and 12 mils] wet film or other wet Prepare this sample by weight even though the strength value
film thickness as appropriate. Bird type bars are usually sought may be by volume.

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D8163 − 18
11.1.2 Prepare a wet sample by blending the identical METHOD B
weight of standard white base as is contained in the wet 11.2 Base Test Method:
standard and an identical weight of test colorant as is contained 11.2.1 Prepare a wet standard by blending an amount of
in the wet standard if the test colorant is to be assessed by standard white base and standard colorant to achieve a reflec-
weight, otherwise an identical volume as contained in the wet tance of between 35 and 50 % reflectance factor with 40 %
standard. reflectance factor considered ideal. Prepare this sample by
11.1.3 The standard white base used in both samples shall weight even though the strength value sought is by volume.
be of the same lot and from the same deaerated subsample of 11.2.2 The standard colorant used in both samples shall be
standard white base. of the same lot and from the same deaerated subsample of
11.1.4 Drawdown the two wet samples side by side on a standard colorant.
black-and-white sealed drawdown card in accordance with 11.2.3 Prepare a wet sample by blending the identical
Practices D823 Method C for motor-driven blade or Method E weight of test white base, if the test result is to be assessed by
for hand-held blade. Use a drawdown bar that will achieve a weight; otherwise, an identical volume, as is contained in the
film thick enough to be opaque when dry. This is usually wet standard and an identical weight; otherwise, an identical
considered to be met by a contrast ratio of 0.98 or more. Place volume of standard colorant as is contained in the wet standard.
the test sample on the left half of the card and the standard The standard colorant used in both samples shall be taken from
sample on the right. the same lot and the same deaerated subsample of standard
11.1.5 Rub up both samples immediately after the draw- colorant.
down by rubbing a small circle in the wet paint several times 11.2.4 Follow the procedure of 11.1.4 – 11.1.10 as the
with light pressure from a finger to assess for differences in balance of the test method procedure is identical for test base
flocculation. Perform this rub up over the black portion of the to that of the test colorant.
card. Inspect the drawdown for differences in color as a result
of flocculation in either sample. Any visual differences in these METHOD C
properties shall cause a termination of the test at this juncture 11.3 White Colorant Method:
in the test process. 11.3.1 Prepare a wet standard by blending an amount of
11.1.6 Dry the specimen card by air dry overnight, force standard white colorant and standard black colorant to achieve
drying in a low (approximately 25°C (77°F) oven with moving a reflectance in neutral base of between 35 and 50 %
air), or in a microwave oven. reflectance factor with 40 % reflectance factor considered
11.1.7 Inspect the drawdown for differences in color in the ideal. Prepare this sample at an appropriate level of total
hue difference direction, metamerism, or gloss. Any visual colorant concentration to achieve hiding in the neutral base.
differences in these properties shall cause a termination of the Prepare this sample by weight even though the strength value
test at this juncture in the test process. sought is by volume.
11.1.8 Select a representative area of the standard specimen 11.3.2 Prepare a wet sample by blending the identical
over the white portion of the card and the test specimen over weight of neutral base, test white colorant, and standard black
the white portion of the card to be measured. Such selection colorant, if the test result is to be assessed by weight,
shall be in accordance with Practice D3964. otherwise, an identical volume as is contained in the wet
11.1.9 Measure the reflectance factor of both the standard standard. The standard colorant and neutral base used in both
and the test specimens in accordance with Test Method E1331 samples shall be of the same lot and from the same deaerated
if hemispherical illumination is used or Test Method E1349 if subsample of standard colorant and neutral base.
bidirectional instrumentation (0:45) is used. 11.3.3 Follow the procedure of 11.1.3 – 11.1.10 as the
11.1.10 Select a value to be used as the reflection factor in balance of the test method procedure is identical for test white
the calculations from the list of possibilities in Table 1. If a colorant to that of the test colorant.
tristimulus value is chosen, it shall be the minimum value from
among X, Y, and Z. Further, if a tristimulus value is chosen, 12. Calculation
select an illuminant-observer weight set for tristimulus inte-
gration from Practice E308. Perform the tristimulus integration 12.1 Using the selected or calculated value of the reflection
in accordance with Practice E308. Scale the reflection factor to factors of the standard sample and the test sample, calculate the
be in the range zero to unity. Perform the strength calculations following values for each specimen:
in accordance with Section 12. ~1 2 p !2
P5 (1)
2p
TABLE 1 List of Allowable Values to be Chosen for Reflection where:
Factor
Ρ = reflection factor of the standard or test specimen in the
Value of Reflection Factor Priority
numeric range of zero to unity.
CIE tristimulus value X 1
CIE tristimulus value Y 1 12.2 Then, for colorant strength, ratio the results as follows:
CIE tristimulus value Z 1
Reflection factor at wavelength of maximum absorption 4 100P test
Sc 5 (2)
Reflection factor at commonly agreed wavelength 5 P std
Area under the K-over-S curve 6
and, for base strength:

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D8163 − 18
100P std in a white base, three samples were prepared and one specimen
Sb 5 (3)
P test drawdown was prepared from each sample. After the spectro-
photometric measurements, the analysis was carried out using
13. Report
a minimum of four different analyses allowed by the choice, in
13.1 Report the following values: the standard, of reflection function. The standard deviation of
13.1.1 Description of the material under test, including the all results was 0.35 % strength. That places the 95 %
product identification and the lot number; confidence limit at 0.7 % strength and means that two results,
13.1.2 The date of the test; obtained by identical procedures under reproducibility
13.1.3 The name of the appraiser of the test; conditions, are to be held suspect if they should differ by more
13.1.4 The calculated strength value obtained by the test than 1 % strength.
and the parameter used for assessing the strength test;
13.1.5 The make, model, and serial number of the spectro- 14.2 A complete interlaboratory study of this test method is
photometric instrument used in the test as well as the instru- being conducted and a complete precision statement is ex-
ment setup conditions, including the specular port setting and pected to be available on or before January 2019.
the aperture size; and 14.3 Bias—There can be no bias in the test result because
13.1.6 The wet film thickness designation of the drawdown the test method is empirical.
bar used to make the drawdown.
14. Precision and Bias 15. Keywords
14.1 Precision—A robustness test has been carried out by 15.1 strength of base; strength of color; strength of colorant;
Subcommittee D01.26. In this test of the strength of a colorant tint strength

APPENDIX

(Nonmandatory Information)

X1. INTERPRETATION OF THE TEST METHOD AND RATIONALE USED IN ITS DEVELOPMENT

X1.1 Interpretation of the Test Method where:


X1.1.1 In 8.1, the user is required to supply standard Cc = concentration, on a scale of zero to unity, of the
materials in support of the test method. It is advisable to select colorant in the white, and the white concentration is
1–Cc.
an amount of these standard materials that will support a year’s
worth of anticipated tests, unless this amount is more than is X1.1.4 The K-over-S of the mix is chosen from Table X1.1
reasonable and feasible to store. and Kw and Kc are the Kubelka-Munk absorption constants of
the white and colorant, respectively, and Sw and Sc the
X1.1.2 In 10.2, at least one method of deaeration is required scattering constants of the white and colorant. Table X1.1
to be used on all prepared samples. This source of uncertainty provides those values of K-over-S of the mix at 40 %
is most important to constrain when it becomes necessary to reflectance for the values of K1 and K2 listed in the left-hand
make a weight-per-gallon assessment, as may happen when a columns. K1 and K2 are the first-surface reflectance and the
conversion between volume formula and weight formula is internal reflectance from the underside of the specimen, respec-
necessary. It may be prudent in the interest of accuracy to use tively. These values are used in the Saunderson correction, if
two methods of deaeration in this circumstance. applied.
X1.1.3 In X1.1.1, the user is asked to estimate a concentra-
TABLE X1.1 Selection of K/Smix Value Given Certain Values of
tion of colorant in the standard white base that will achieve a K1 and K2
reflection factor of 40 %. Users of this test method are likely to K1 K2 K/Smix
be engaged in computer color matching of their color catalog No correction applied 0.4500
and are thus likely to have prior knowledge of the Kubelka- 0.00 0.00 0.4500
Munk Ks and Ss of the standard materials being used in this test 0.00 0.40 0.2132
0.00 0.45 0.1865
method. Select a wavelength nearest the largest values of K for 0.00 0.60 0.1125
the colorant. Gather the Ks and Ss of both standard colorant 0.02 0.40 0.2304
0.02 0.45 0.2018
and standard base at this wavelength, and apply the following 0.02 0.60 0.1222
equation: 0.03 0.40 0.2399
0.03 0.45 0.2102

Cc 5
K w2
K
S SD mix
Sw
(X1.1)
0.03
0.04
0.60
0.40
0.1276
0.2500

SD
K
S 2
S mix c
K
S SD mix
S w 1K w 2K c
0.04
0.04
0.45
0.60
0.2190
0.1333

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D8163 − 18
X1.1.5 In X1.1.1, the user is required to estimate the amount X1.1.11 When choosing a single wavelength of maximum
of colorant necessary to achieve about a 40 % reflectance absorption, choosing a commonly agreed wavelength, or cal-
factor. When making samples as small as 250 g in typical culating the area under the K-over-S curve, one should avoid
mid-tone or deep-tone white bases, the amount of required wavelengths 400 to 410 and 690 to 700 nm for several reasons,
colorant may be less than a single gram. In no case should a including poorer signal-to-noise ratios in these ranges in most
test proceed in which any ingredient is less than 10 g on a scale instruments, the rutile absorption band in the short wavelength
with readability of 0.001 g and a measurement uncertainty of region, and absorption losses in the long-wave region.
about 0.02 g. This may be achieved by premixing the colorant
with perhaps up to nine parts by volume of clear, or neutral X1.1.12 In Paragraph 11.1.10, one is allowed to choose any
base, to one part of colorant in an intermediate material that is weight set for tristimulus integration from Practice E308. In the
a large enough preparation that no single ingredient of it is absence of any reason to do otherwise, the use of that set that
under 10 g . Such a procedure complies with the intent of this is most familiar to one’s industry is preferred. In the case of
test method and reduces the overall uncertainty of the weighing coatings, that is likely to be Standard Illuminant D65 and the
of the colorant. 1964 10° Standard Observer.
X1.1.6 In 11.1.2 and 11.2.2, it is required that the standard X1.1.13 In 11.2.1, the appraiser is required to maintain a
sample and the test sample to be made by weight even though standard white base for each white base material put under test.
the strength value sought is with reference to volume. A The proliferation of materials in this class is such that users of
convenient conversion factor to use is 3.5437 g · gallons per
this test method usually fulfill this requirement by maintaining
fluid ounce · pound avoirdupois. The weight per gallon will
a stronger white standard component and a clear (or neutral)
usually be known for both materials in the mixture. Multiply-
base that can be blended with each other to form the required
ing the conversion factor times the percent volume concentra-
tion (as a decimal fraction) times the total volume of the standard white base. These are blended in a proportion whose
sample (in fluid ounces) times the weight (in pounds) per formula thereafter determines the standard strength of the
gallon yields the weight in grams of the ingredient. material under consideration. Such an arrangement complies
with the intent of this test method as long as the mixture of
X1.1.7 In 11.1.6, three methods of drying are allowed that
surface active agents used to maintain the dispersions are
are conventionally used in paint laboratories. It is a best
equivalent and compatible and the grade and crystalline
practice that, once one such method of drying is chosen, all
structure of titanium dioxide used is identical in both materials.
other tests of that same material under test be dried in exactly
the same manner. Each of these three methods of drying is
likely to achieve slightly different results from each other. X1.2 RATIONALE USED IN THE TEST METHOD’S
DEVELOPMENT
X1.1.8 In 11.1.10, one is allowed to choose any parameter
in Table 1 as the reflection factor for the test. The preferred X1.2.1 Because of the complexity of the test method and the
value is that tristimulus value near the largest absorption of the contribution to uncertainty of several large components of the
reflection function. This is preferred to the actual wavelength test method, it was apparent that a major task in developing the
of maximum absorption as a result of averaging of multiple test method would be to put constraints on all sources of
wavelengths under the tristimulus regime. However, any value uncertainty. The three largest sources of uncertainty are be-
in Table 1 may be selected, and this is often done when lieved to be the weight-per-gallon assessment, the weighing of
common agreement between buyer and seller dictates so. the colorant, and the measurement of the reflectance factors of
X1.1.9 No matter what value is chosen for the reflection the drawdowns. However, there are a number of items listed as
factor, it is to be expressed as a decimal fraction when used in interferences and sources of uncertainty that, if present, would
Eq 1. make equal or larger contributions to uncertainty than these
X1.1.10 In the area under the K-over-S curve method, the named contributors. Should even one such additional contribu-
reflectances between 420 and 680 nm are converted to tor be present, it is possible that the uncertainty of the method
K-over-S values by Eq 1 and then these K-over-S values are could exceed what is expected to be allowed by the tolerances
averaged. This average value is then used as Pstd or Ptest in Eq presently associated with strength of colorant and strength of
2 or Eq 3. bases.

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D8163 − 18
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