ASTM D153-84(2014)
(Test Method)Standard Test Methods for Specific Gravity of Pigments
Standard Test Methods for Specific Gravity of Pigments
ABSTRACT
These test methods cover three procedures for determining the specific gravity of pigments, as follows: Test Method A which is for routine testing of several samples simultaneously, Test Method B which is for tests requiring greater accuracy than Test Method A, and Test Method C which is for rapid and accurate testing of single samples. The specific gravity value obtained by these procedures may be used with the weight of a dry pigment to determine the volume occupied by the pigment in a coating formulation. For Test Method A, the following apparatus and materials shall be used: pycnometer, water bath, manometer, desiccator, vacuum pumps, thermometer, weighing bottle, and immersion liquid. For Test Method B, the following apparatus and materials shall be used: pycnometer, water bath, manometer, vacuum pump, thermometer, weighing bottle, bell jar, and bottle. For Test Method C, the following apparatus and materials shall be used: buret, flask, stopcocks, vacuum pump, manometer, thermometer, weighing bottle, and immersion liquid.
SCOPE
1.1 These test methods cover three procedures for determining the specific gravity of pigments, as follows:
Test Method A—For Routine Testing of Several Samples Simultaneously.
Test Method B—For Tests Requiring Greater Accuracy than Test Method A.
Test Method C—For Rapid and Accurate Testing of Single Samples.
1.2 The specific gravity value obtained by these procedures may be used with the weight of a dry pigment to determine the volume occupied by the pigment in a coating formulation.
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.4 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. For specific hazard statements, see Sections 5, 11, and 15.
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Designation:D153 −84 (Reapproved 2014)
Standard Test Methods for
Specific Gravity of Pigments
This standard is issued under the fixed designation D153; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope TEST METHOD A—FOR ROUTINE TESTING OF
SEVERAL SAMPLES SIMULTANEOUSLY
1.1 These test methods cover three procedures for determin-
ing the specific gravity of pigments, as follows:
4. Apparatus and Materials
Test Method A—For Routine Testing of Several Samples
4.1 Pycnometer—A pycnometer (Note 1) having a 50-mL
Simultaneously.
capacity.
Test Method B—For Tests Requiring Greater Accuracy than
Test Method A.
NOTE 1—The Weld type with the cap seal on the outside of the neck of
Test Method C—For Rapid and Accurate Testing of Single
the bottle is preferred because there is less danger of trapping air just
Samples. under the capillary tube than with types having the ground glass seal on
the inside of the neck.
1.2 The specific gravity value obtained by these procedures
4.2 Water Bath, maintained at 25 6 0.5°C and equipped
may be used with the weight of a dry pigment to determine the
with a stirring device.
volume occupied by the pigment in a coating formulation.
4.3 Manometer, open- or closed-tube (see Part f of the
1.3 The values stated in SI units are to be regarded as the
apparatus for Test Method C), made of glass tubing 6 mm in
standard. The values given in parentheses are for information
diameter, fitted with rubber pressure tubing attached to a
only.
T-joint leading to the desiccator and the pump. For the
1.4 This standard does not purport to address all of the
open-tube type 860 mm of mercury shall be used. The
safety concerns, if any, associated with its use. It is the
difference in levels of the mercury in the manometer when the
responsibility of the user of this standard to establish appro-
system is in operation, subtracted from the barometer reading
priate safety and health practices and determine the applica-
taken at the same time, shall be considered the absolute
bility of regulatory limitations prior to use. For specific hazard
pressure of the system in millimetres of mercury.
statements, see Sections 5, 11, and 15.
4.4 Desiccator, glass, constructed with heavy walls to with-
stand a vacuum of one atmosphere, and with an opening at the
2. Referenced Documents
side.
2.1 ASTM Standards:
4.5 VacuumPumps—Alaboratory water vacuum-type pump
D1193 Specification for Reagent Water
(Note 2), to remove the greater portion of air in the desiccator,
and an oil vacuum-type pump, motor-driven, and capable of
3. Purity of Reagents
reducing the absolute pressure of the system to 3 mm.
3.1 PurityofWater—Reference to water shall be understood
NOTE 2—The water vacuum pump may be omitted if the rate of
to mean reagent water as defined by Type II of Specification
evacuation with the oil pump can be controlled so as to avoid a rapid
D1193.
ebullition of entrapped air and possible loss of specimen.
4.6 Thermometer, having a range from 0 to 60°C, and
graduated in 0.1°C divisions.
These test methods are under the jurisdiction of ASTM Committee D01 on
4.7 WeighingBottle, wide-mouth cylindrical glass (about 30
Paint and Related Coatings, Materials, and Applications and are the direct
responsibility of Subcommittee D01.31 on Pigment Specifications.
mm in height and 70 mm in diameter), provided with a
Current edition approved Dec. 1, 2014. Published December 2014. Originally
ground-glass stopper.
approved in 1923. Last previous edition approved in 2008 as D153 – 84 (2008).
DOI: 10.1520/D0153-84R14.
4.8 Immersion Liquid—Kerosine has been found to be a
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
good wetting vehicle for most pigments, and shall be used
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
generally as the immersion liquid. Refined, white kerosine of
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. narrow evaporation and boiling range shall be used.With some
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D153−84 (2014)
pigments that are not wetted well with kerosine, other immer- pigments very rapidly, then this action gradually decreases and
sion liquids such as glycerin, ethylene glycol, finally stops. The time required for complete removal of air
tetrahydronaphthalene, etc., may be substituted. The liquid may vary from 30 min to 24 h, depending upon the nature of
must have a low evaporation rate and narrow boiling range, the pigment. When no more bubbles can be seen, it may be
and the same procedure shall be followed as with kerosine. assumed that the occluded air has been removed and that the
Water is not a preferred liquid because of the possibility of pigment is thoroughly wet with kerosine. Then slowly admit
frothing. air to the desiccator by means of the pinchcock.
7.6 Filling and Bringing to Temperature—Remove the py-
5. Hazards
cnometer from the desiccator, fill with kerosine at 24 to 25°C
5.1 Before a desiccator is used for the first time, wrap it in
taking care to add a sufficient quantity to prevent air bubbles
a towel and test under an absolute pressure of under 3 mm.
wherethepycnometerisclosed,andpermittocometoconstant
Exercise care in handling the desiccator when under vacuum,
temperature at 25 6 0.5°C in the water bath. Carefully stopper
since a sudden jar may cause it to collapse.
the pycnometer and remove excess kerosine with lens paper.
Take the pycnometer out of the bath, allow to come to room
6. Standardization of Pycnometer
temperature, and weigh.
6.1 Fill the pycnometer with freshly boiled water at 23 to
8. Calculation
24°C, gradually bring to 25 6 0.5°C, and then dry and weigh
as specified in 7.6. Empty the pycnometer, and clean, dry, and
8.1 Calculate the specific gravity, S, of the pigment as
reweigh it. Next fill the pycnometer with kerosine at 23 to
follows:
24°C, bring to 25 6 0.5°C, dry, and weigh as before. Calculate
P
the specific gravity, S, of the kerosine at 25/25°C as follows: S 5 (2)
K
W 2
S 5A/B (1)
D
where:
where:
A = weight of kerosine, g, and
P = weight of pigment used, g,
B = weight of water, g.
W = weight of water to fill the pycnometer, g,
K = weight of kerosine added to the pigment, g, and
7. Procedure
D = specific gravity of the kerosine.
7.1 Drying—Dry the pigment, preferably in an electric
9. Precision
oven, at 105 6 2°C for 2 h.
9.1 Duplicate determinations by this test method should not
7.2 Weighing—Transfer to a clean, dry, weighed
differ by more than 0.02.
pycnometer,sufficientsampletoformalayerapproximately20
mm ( ⁄4 in.) deep. For black, blue, and lake pigments of low
TEST METHOD B—FOR TESTS REQUIRING
specific gravity, use about1gof sample; for inert crystalline
GREATER ACCURACY THAN TEST METHOD A
pigments, about 4 g; for opaque white pigments, 7 to 10 g; and
for red lead, from 15 to 20 g.Weigh pigments of a hydroscopic
10. Apparatus (see Fig. 1 and Fig. 2)
nature from the weighing bottle.
10.1 Pycnometer, Water Bath, Manometer, Vacuum Pump,
7.3 Number of Specimens—Run all samples at least in
Thermometer, Weighing Bottle, and Immersion Liquid—See
duplicate.
Section 4; also Fig. 2 (e) and (f ).
7.4 Addition of Kerosine—Add enough kerosine to the
10.2 BellJar,glass,withatwo-holerubberstopper.Intoone
pycnometer to form a clear layer approximately ⁄4 in. (6 mm)
hole of the stopper shall be fitted a separatory funnel with a
above the pigment. When necessary, stir the specimen with a
well-ground stopcock (Fig. 1 (c)), extending into the pycnom-
polished round-bottom glass rod until completely covered by
eter. Into the other hole of the stopper shall be fitted a glass
kerosine, adding more kerosine if necessary.Wash the rod with
tube with a well-ground three-way stopcock (Fig. 2 (d)) and
kerosine, adding the washings to the pycnometer.
7.5 Removal of Occluded Air—Place the pycnometer in the
desiccator. Close the desiccator and attach to the water pump
until the greater part of the air is removed from the system.
Complete this procedure within a period of 5 to 10 min. Close
the system with a pinchcock and attach the desiccator to the oil
pump for the removal of the small amounts of air given off at
the low pressures obtainable with the oil pump. Use the
manometer to indicate whether the oil pump is giving the
proper vacuum. When the manometer indicates that the abso-
lute pressure is 3 mm and constant, cut off the oil pump for
short periods, taking care that
...
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: D153 − 84 (Reapproved 2008) D153 − 84 (Reapproved 2014)
Standard Test Methods for
Specific Gravity of Pigments
This standard is issued under the fixed designation D153; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope
1.1 These test methods cover three procedures for determining the specific gravity of pigments, as follows:
Test Method A—For Routine Testing of Several Samples Simultaneously.
Test Method B—For Tests Requiring Greater Accuracy than Test Method A.
Test Method C—For Rapid and Accurate Testing of Single Samples.
1.2 The specific gravity value obtained by these procedures may be used with the weight of a dry pigment to determine the
volume occupied by the pigment in a coating formulation.
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.4 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. For specific hazard statements, see Sections 5, 11, and 15.
2. Referenced Documents
2.1 ASTM Standards:
D1193 Specification for Reagent Water
3. Purity of Reagents
3.1 Purity of Water—Reference to water shall be understood to mean reagent water as defined by Type II of Specification
D1193.
TEST METHOD A—FOR ROUTINE TESTING OF SEVERAL SAMPLES SIMULTANEOUSLY
4. Apparatus and Materials
4.1 Pycnometer—A pycnometer (Note 1) having a 50-mL capacity.
NOTE 1—The Weld type with the cap seal on the outside of the neck of the bottle is preferred because there is less danger of trapping air just under
the capillary tube than with types having the ground glass seal on the inside of the neck.
4.2 Water Bath, maintained at 25 6 0.5°C and equipped with a stirring device.
4.3 Manometer, open- or closed-tube (see Part f of the apparatus for Test Method C), made of glass tubing 6 mm in diameter,
fitted with rubber pressure tubing attached to a T-joint leading to the desiccator and the pump. For the open-tube type 860 mm of
mercury shall be used. The difference in levels of the mercury in the manometer when the system is in operation, subtracted from
the barometer reading taken at the same time, shall be considered the absolute pressure of the system in millimetres of mercury.
4.4 Desiccator, glass, constructed with heavy walls to withstand a vacuum of one atmosphere, and with an opening at the side.
4.5 Vacuum Pumps—A laboratory water vacuum-type pump (Note 2), to remove the greater portion of air in the desiccator, and
an oil vacuum-type pump, motor-driven, and capable of reducing the absolute pressure of the system to 3 mm.
These test methods are under the jurisdiction of ASTM Committee D01 on Paint and Related Coatings, Materials, and Applications and are the direct responsibility of
Subcommittee D01.31 on Pigment Specifications.
Current edition approved Feb. 1, 2008Dec. 1, 2014. Published February 2008December 2014. Originally approved in 1923. Last previous edition approved in 20032008
as D153 – 84 (2003).(2008). DOI: 10.1520/D0153-84R08.10.1520/D0153-84R14.
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’sstandard’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
D153 − 84 (2014)
NOTE 2—The water vacuum pump may be omitted if the rate of evacuation with the oil pump can be controlled so as to avoid a rapid ebullition of
entrapped air and possible loss of specimen.
4.6 Thermometer, having a range from 0 to 60°C, and graduated in 0.1°C divisions.
4.7 Weighing Bottle, wide-mouth cylindrical glass (about 30 mm in height and 70 mm in diameter), provided with a
ground-glass stopper.
4.8 Immersion Liquid—Kerosine has been found to be a good wetting vehicle for most pigments, and shall be used generally
as the immersion liquid. Refined, white kerosine of narrow evaporation and boiling range shall be used. With some pigments that
are not wetted well with kerosine, other immersion liquids such as glycerin, ethylene glycol, tetrahydronaphthalene, etc., may be
substituted. The liquid must have a low evaporation rate and narrow boiling range, and the same procedure shall be followed as
with kerosine. Water is not a preferred liquid because of the possibility of frothing.
5. Hazards
5.1 Before a desiccator is used for the first time, wrap it in a towel and test under an absolute pressure of under 3 mm. Exercise
care in handling the desiccator when under vacuum, since a sudden jar may cause it to collapse.
6. Standardization of Pycnometer
6.1 Fill the pycnometer with freshly boiled water at 23 to 24°C, gradually bring to 25 6 0.5°C, and then dry and weigh as
specified in 7.6. Empty the pycnometer, and clean, dry, and reweigh it. Next fill the pycnometer with kerosine at 23 to 24°C, bring
to 25 6 0.5°C, dry, and weigh as before. Calculate the specific gravity, S, of the kerosine at 25/25°C as follows:
S 5 A/B (1)
where:
A = weight of kerosine, g, and
B = weight of water, g.
7. Procedure
7.1 Drying—Dry the pigment, preferably in an electric oven, at 105 6 2°C for 2 h.
7.2 Weighing—Transfer to a clean, dry, weighed pycnometer, sufficient sample to form a layer approximately 20 mm ( ⁄4 in.)
deep. For black, blue, and lake pigments of low specific gravity, use about 1 g of sample; for inert crystalline pigments, about 4
g; for opaque white pigments, 7 to 10 g; and for red lead, from 15 to 20 g. Weigh pigments of a hydroscopic nature from the
weighing bottle.
7.3 Number of Specimens—Run all samples at least in duplicate.
7.4 Addition of Kerosine—Add enough kerosine to the pycnometer to form a clear layer approximately ⁄4 in. (6 mm) above the
pigment. When necessary, stir the specimen with a polished round-bottom glass rod until completely covered by kerosine, adding
more kerosine if necessary. Wash the rod with kerosine, adding the washings to the pycnometer.
7.5 Removal of Occluded Air—Place the pycnometer in the desiccator. Close the desiccator and attach to the water pump until
the greater part of the air is removed from the system. Complete this procedure within a period of 5 to 10 min. Close the system
with a pinchcock and attach the desiccator to the oil pump for the removal of the small amounts of air given off at the low pressures
obtainable with the oil pump. Use the manometer to indicate whether the oil pump is giving the proper vacuum. When the
manometer indicates that the absolute pressure is 3 mm and constant, cut off the oil pump for short periods, taking care that the
vacuum does not change materially due to leakage. At first bubbles of air rise from the pigments very rapidly, then this action
gradually decreases and finally stops. The time required for complete removal of air may vary from 30 min to 24 h, depending
upon the nature of the pigment. When no more bubbles can be seen, it may be assumed that the occluded air has been removed
and that the pigment is thoroughly wet with kerosine. Then slowly admit air to the desiccator by means of the pinchcock.
7.6 Filling and Bringing to Temperature—Remove the pycnometer from the desiccator, fill with kerosine at 24 to 25°C taking
care to add a sufficient quantity to prevent air bubbles where the pycnometer is closed, and permit to come to constant temperature
at 25 6 0.5°C in the water bath. Carefully stopper the pycnometer and remove excess kerosine with lens paper. Take the
pycnometer out of the bath, allow to come to room temperature, and weigh.
8. Calculation
8.1 Calculate the specific gravity, S, of the pigment as follows:
P
S 5 (2)
K
W 2
D
D153 − 84 (2014)
where:
P = weight of pigment used, g,
W = weight of water to fill the pycnometer, g,
K = weight of kerosine added to the pigment, g, and
D = specific gravity of the kerosine.
9. Precision
9.1 Duplicate determinations by this test method should not differ by more than 0.02.
TEST METHOD B—FOR TESTS REQUIRING GREATER ACCURACY THAN TEST METHOD A
10. Apparatus (see Fig. 1 and Fig. 2)
10.1 Pycnometer, Water Bath, Manometer, Vacuum Pump, Thermometer, Weighing Bottle, and Immersion Liquid—See Section
4; also Fig. 2 (e) and (f ).
10.2 Bell Jar, glass, with a two-hole rubber stopper. Into one hole of the stopper shall b
...
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