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D2448 − 85 (2012)
5.7.3 For specific resistances of reagent water or of over 7.2 Calculate the cell constant, K, as follows:
200 000 Ω · cm, use a cell with a constant of 0.1. K 25 5 ~ R m /R s !
6. Reagents where:
6.1 Purity of Reagents—Reagent grade chemicals shall be Rm = specific resistance at 25°C (see 8.2.2), and
used in all tests. Unless otherwise indicated, it is intended that Rs = specific resistance in ohm centimetres of an 0.002 N
all reagents shall conform to the specifications of the Commit- KCl solution at 25°C (Table 1) = 3427 Ω · cm.
tee on Analytical Reagents of the American Chemical Society, NOTE 2—In general the “cell constant” is not greatly affected by
where such specifications are available.4 Other grades may be variations in the strength of the KCl solution, but for greatest accuracy,
used, provided it is first ascertained that the reagent is of measurements should be made at or near the specific resistance of the
sufficiently high purity to permit its use without lessening the solution to be measured and at values that utilize the medium range of the
scale of the conductivity bridge, using the same multiplier tap.
accuracy of the determination.
7.3 The specific resistances of KCl solutions are shown for
6.2 Purity of Water—Unless otherwise indicated, references
concentrations from 0.001 N to 0.073 N at 25 C in Fig. 1. This
to water shall be understood to mean reagent grade water as
curve, almost a straight line, was made from published values
defined by Type II of Specification D1193.
of specific conductances and equivalent conductances of KCl
6.3 Methanol. solutions at 25 C. Table 1 gives values of the specific
6.4 Potassium Chloride, Standard Solution (0.02 N)— Pre- resistances of KCl solutions for those concentrations useful for
pare a 0.02 N potassium chloride (KCl) solution with water by pigment testing.
dissolving 1.491 g of KCl (heated before weighing for 1 h at
105°C) in water, followed by dilution to 1 L. 8. Procedure
8.1 Hydrophobicity Test—Test a small amount of pigment
7. Determination of Cell Constant with boiling water to see if it is water-wettable. Pigments that
7.1 Prepare a 0.002 N solution of KCl by diluting the 0.02 do not wet well with water are probably hydrophobic and
N KCl solution described in 6.4 with water. Cool and measure should be treated as described in 8.3. If the pigment wets
the specific resistance, Rm, at 25 60.5°C as described in 8.2.2. easily, proceed as described in 8.2.
8.2 Hydrophilic Pigments:
4
Reagent Chemicals, American Chemical Society Specifications, American 8.2.1 A 20.0-g specimen weight is usually sufficient for
Chemical Society, Washington, DC. For suggestions on the testing of reagents not pigments easily wet with water. Add 20.0 g of the pigment to
listed by the American Chemical Society, see Analar Standards for Laboratory
180 g of boiling water in a tared, 400-mL beaker with stirring
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, rod. (Usually a 250-mL beaker is sufficient for white pigments.
MD. Some white pigment, because of tendency to foam and crawl,
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D2448 − 85 (2012)
TABLE 1 Specific Resistances of Solutions of Potassium easily wet with water. Wet 30.0 g of pigment with 5 to 20 g of
Chloride at 25°C alcohol, as required, to produce a smooth wet paste. Complete
Normality Ω · cm the addition of water to bring the net weight to 300 g by
0.001 6802 (1) diluting with boiling water in a tared beaker (1000 mL has been
0.002 3427 (1)
0.005 1393 (1)
found satisfactory), with a stirring rod. Boil, cool, filter, and
0.01 707.3 (1,2) determine the reading as outlined in 8.2.2.
0.02 361.5 (3)
9. Calculation
can be handled better in a larger beaker. Usually 20-g speci- 9.1 Calculate the specific resistance, R25, in ohm
mens of organic pigments require a 600-mL beaker to allow centimetres, of the pigment at 25°C by taking the mean Ra, of
adequate room for foaming. Boil slowly for 5 min with the five or more readings made and divide by the cell constant,
occasional stirring. Cool to about 60°C and add water to bring K, determined in accordance with Section 7.
the net weight back to 200 g. Stir thoroughly. Filter directly
through fine-texture paper (Note 1) or separate the solids by 10. Precision and Bias
centrifuge using clean, dry cups, or cups washed with some of 10.1 On the basis of a laboratory study of this test method,
the slurry, followed by decanting the supernatant liquid the following criteria should be used for judging the accept-
through a filter. In either case discard the first 10 mL through ability of results at the 95 % confidence level:
the filter. 10.1.1 Repeatability—Two results obtained by the same
8.2.2 Cool the filtrate to about 20°C. Rinse the footed operator should be considered suspect if they differ by more
cylinder and the conductivity cell, previously rinsed with than 5 % for white pigments and 7 % for colored organic
water, with the leachate. Fill the footed cylinder with the pigments.
leachate to be measured and place the conductivity cell into the
10.1.2 Reproducibility—Two results obtained by operators
leachate. Move the dip cell up and down to remove all air
in different laboratories should be considered suspect if they
bubbles. Adjust the temperature slowly to 25°C and, with the
differ by more than 10 % for white pigments and 15 % for
cell submerged so that the vent is 1⁄2 in. (12.7 mm) below the
colored organic pigments.
surface of the liquid and centered upright in the cylinder, make
at least five measurements of the specific resistance at 25 6 10.2 Bias—Bias has not been determined for this test
0.5°C, using the conductivity bridge with the multiplier set to method.
give a reading near the center of the scale, following the
instructions supplied with the instrument to obtain a balance. 11. Keywords
8.3 Hydrophobic Pigments—A modification of the proce- 11.1 inorganic pigments; leachate; organic pigments; water
dure given in 8.2 is necessary for organic pigments that are not soluble salts; white pigments
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