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Astm D1475-13 (2020)
Astm D1475-13 (2020)
for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D1475 − 13 (2020)
TABLE 1 Absolute Density of Water, g/mL pycnometers may have filled weights that exceed the capacity of the usual
°C Density laboratory analytical balance. In such cases, use of a hanging pan,
triple-beam balance, with scales graduated to 0.01 g has been found to
15 0.999127
16 0.998971
provide results the mean of which was consistent with the overall
17 0.998772 precision and accuracy of the method.
18 0.998623 7.5 Desiccator and Desiccated Balance, or a room of
19 0.998433
20 0.998231 reasonably constant temperature and humidity are desirable.
21 0.998020
22 0.997798
23 0.997566
8. Calibration of Cup or Pycnometer
24 0.997324 8.1 Determine the volume of the container at the specified
25 0.997072
26 0.996811 temperature by employing the following steps:
27 0.996540 8.1.1 Clean and dry the container and bring it to constant
28 0.996260 weight. Chromic acid (see 8.1.1.1) or other effective glass
29 0.995972
30 0.995684 cleaner and nonresidual solvents may be used with glass
containers and solvents with metal containers. For maximum
accuracy, continue rinsing, drying, and weighing until the
5.2 This test method is suitable for the determination of difference between two successive weighings does not exceed
density of paint and related products and components when in 0.001 % of the weight of the container. Fingerprints on the
liquid form. It is particularly applicable when the fluid has too container will change the weight and must be avoided. Record
high a viscosity or when a component is too volatile for a the weight, M, in grams.
density balance determination. 8.1.1.1 Warning—Chromic acid cleaning solution is corro-
sive to skin, eyes and mucous membranes and can cause severe
5.3 This test method provides for the maximum accuracy
burns. Avoid contact with eyes, skin or clothing. In making
required for hiding power determinations. It is equally suitable
dilute solution, always add acid to water with care. Chromic
for work in which less accuracy is required, by ignoring the
acid cleaning solution is a strong oxidizer. Avoid contact with
directions for recalibration and consideration of temperature
organic or reducing substances as a fire could results. See
differentials, and using as the container a “weight-per-gallon”
supplier’s Material Safety Data Sheet for further information.
cup.
Other cleaners are much safer and may be equally effective.
5.4 Automatic equipment for measuring density is available 8.1.2 Fill the container with reagent water conforming to
(see Test Method D4052) from several manufacturers. Such Type II of Specification D1193 at a temperature somewhat
apparatus has been used for resins and latices as well as for oils below that specified. Cap the container, leaving the overflow
and solvents. Before such equipment is used for a given orifice open. Immediately remove excess overflowed water or
product, results must be checked very carefully. Particularly water held in depressions by wiping dry with absorbent
with paints, inks, and resins, there are possibilities of material. Avoid occluding air bubbles in the container.
gumming, fouling, and other interferences with operation. 8.1.3 Bring the container and contents to the specified
temperature using the constant-temperature bath or room if
6. Interferences
necessary. This will cause further slight flow of water from the
6.1 Highly viscous materials may entrap air and give overflow orifice due to the expansion of the water with the rise
erroneous low density values. of the temperature.
6.2 Paint or ink liquids may be trapped in the ground glass 8.1.4 Remove the excess overflow by wiping carefully with
or metal joints of the pieces of apparatus and give erroneous, absorbent material, avoiding wicking of water out of orifice,
high density values. and immediately cap the overflow tube where such has been
provided. Dry the outside of the container, if necessary, by
7. Apparatus wiping with absorbent material. Do not remove overflow that
7.1 Cup or Pycnometer—Any metal weight-per-gallon cup occurs subsequent to the first wiping after attainment of the
or glass pycnometer may be used, provided that it may be filled desired temperature (Note 3). Immediately weigh the filled
readily with a viscous liquid, adjusted to exact volume, covered container to the nearest 0.001 % of its weight (Note 4). Record
to exclude loss of volatile matter, and readily cleaned. this weight, N, in grams.
NOTE 1—For materials that contain solvents that evaporate rapidly, a NOTE 3—Handling the container with bare hands will increase the
glass pycnometer of the weld type, with a narrow stopper and a cover temperature and cause more overflow from the overflow orifice, and will
should be used. also leave fingerprints; hence, handling only with tongs and with hands
protected by clean, dry, absorbent material is recommended.
7.2 Thermometers, graduated in 0.1°C, such as are supplied NOTE 4—Immediate and rapid weighing of the filled container is
with glass pycnometers. recommended here to minimize loss of weight due to evaporation of the
water through orifices, and from overflow subsequent to the first wiping
7.3 Constant-Temperature Bath, held at 25 6 0.1°C is after attainment of temperature where this overflow is not retained by a
desirable. cap.
7.4 Laboratory Analytical Balance. 8.1.5 Calculate the container volume as follows:
NOTE 2—The usual weight-per-gallon cup and similar specialized V 5 ~ N 2 M ! /ρ (1)
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D1475 − 13 (2020)
where: 11. Precision and Bias
V = volume of container, mL, 11.1 Paints—The precision estimates are based on an inter-
N = weight of container and water, g (8.1.4), laboratory study in which one operator in each of six different
M = weight of dry container, g (8.1.1), and laboratories analyzed in duplicate on two different days five
ρ = absolute density of water at specified temperature, samples of paint ranging in density from 8.5 to 12.5 lb/gal. The
g/mL (see Table 1). results were analyzed statistically in accordance with Practice
8.1.6 Obtain the mean of at least three determinations. E180. The within-laboratory coefficient of variation was found
to be 0.20 % relative with 25 df and the between-laboratory
9. Procedure coefficient of variation was 0.61 % relative with 20 df. Based
9.1 Repeat the steps in Section 8, but do two determinations on these coefficients, the following criteria should be used for
rather than three. Substitute the sample for the reagent water in judging the acceptability of results at the 95 % confidence
Section 8 and a suitable nonresidual solvent for the acetone or level:
alcohol (see Note 5). Record the weight of the filled container, 11.1.1 Repeatability—Two results, each the mean of dupli-
W, and the weight of the empty container, w, in grams. cate determinations, obtained by the same operator on different
days should be considered suspect if they differ by more than
NOTE 5—Trapping of paint or ink liquids in ground glass or metal joints 0.6 % relative.
is likely to result in high values of density that appear to increase with the
viscosity and density of the material; such errors should be minimized by
11.1.2 Reproducibility—Two results, each the mean of du-
firm seating of the joints. plicate determinations, obtained by operators in different labo-
NOTE 6—Trapping of air bubbles results in low values for density. The ratories should be considered suspect if they differ by more
tendency to trap air increases with increasing viscosity. Specimens should than 1.8 % relative.
not be tested if they contain bubbles or foam. Slow stirring, standing, or
the application of a vacuum may remove bubbles. If these do not work, a 11.2 Inks—A separate interlaboratory study of this test
dilution may be necessary (see Appendix X1). method was carried out for inks. In this study, one operator in
9.2 Calculate the density in grams per millilitre as follows: each of seven laboratories made three determinations on four
different paste ink samples. Paste inks were chosen because
D m 5 ~ W 2 w ! /V (2) their viscosities are high and they would be expected to provide
where: a difficult test for the method. The inks represented a density
Dm = density, g/mL. range of 8.4 to 8.9 lb/gal and exhibited viscosities ranging from
a very soft news black to a relatively heavy sheet-fed offset ink.
9.3 Calculate the density in pounds per gallon as follows: The results were analyzed statistically in accordance with
D 5 ~ W 2 w ! K/V (3) Practice E691. The within-laboratory standard deviation was
0.030 lb/gal and the pooled laboratory standard deviation was
where:
0.045 lb/gal. Based on these values, the following criteria
D = density, lb/gal, should be used for judging the acceptability of results at the
K = 8.3454 (Note 7), and 95 % confidence level:
V = volume of container, mL (see 8.1.6).
11.2.1 Repeatability—Two results obtained by the same
NOTE 7—The factor K, 8.3454, is calculated from volume-weight
relationship as follows: operator should be considered suspect if they differ by more
8.345404 = [(2.54)3A × (231.00)B ]/(453.59237)C
than 0.084 lb/gal (1 %).
A 3
11.2.2 Reproducibility—Two results obtained by operators
(2.54) is the conversion factor for millilitres to cubic inches.
B
231.00 is the conversion factor for cubic inches to gallons. in different laboratories should be considered suspect if they
C
453.59237 is the conversion factor for grams to pounds. differ by more than 0.125 lb/gal (1.5 %).
11.3 Bias (Paint and Inks)—Since there is no accepted
10. Report
reference material, bias cannot be determined.
10.1 In reporting the density, state the test temperature to the
nearest 0.1°C, the units, and the value calculated to three places 12. Keywords
(for example, D = x.xxx lb/gal at 25°C); state the mean, the 12.1 density; pycnometer; weight per gallon; weight per
range, and the number of replicate determinations. gallon cup
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D1475 − 13 (2020)
APPENDIXES
(Nonmandatory Information)
X2.1 To reduce the variation in the density method, air is X2.3.2 Turn on the centrifuge and set the speed control to
removed from the specimen by centrifuging the material, 2/3 power to attain a speed of 2700 to 3000 r/min.
resulting in greater homogeneity between replicates. This X2.3.3 Continue to run for 15 to 20 s, stop the centrifuge,
greatly improves reproducibility and repeatability and results applying the brake as needed.
in slightly higher density readings.
X2.3.4 Pour off the top foam layer.
X2.2 Apparatus X2.3.5 Transfer the specimen to a calibrated density cup
X2.2.1 Centrifuge, capable of a maximum of 4000 r/min4, and follow the procedure under Section 9.
X2.2.2 Standard Density Cup, X2.4 Precision and Bias
X2.2.3 Thermometer. X2.4.1 An interlaboratory study in one company showed
that the centrifuge procedure resulted in a 2-fold improvement
X2.3 Procedure in repeatability and reproducibility, as well as better accuracy.
X2.3.1 Fill the centrifuge tube to the top (approximately X2.4.1.1 Repeatability—Two results obtained by the same
150 % of the density cup volume), adjust to the recommended operator should be considered suspect if they differ by more
temperature of 25°C 6 1. Place the tube in the centrifuge. than 0.0054 g/mL (0.045 lb/gal).
X2.4.1.2 Reproducibility—Two results obtained by opera-
tors in different laboratories should be considered suspect if
4
The centrifuge used in this study was a Dynac II. they differ by more than 0.0080 g/L (0.067 lb/gal).
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