Designation: D 387 – 86 (Reapproved 1994)

AMERICAN SOCIETY FOR TESTING AND MATERIALS

100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM

Standard Test Method for

Color and Strength of Color Pigments with a Mechanical
Muller1
This standard is issued under the fixed designation D 387; 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.

This standard has been approved for use by agencies of the Department of Defense.

1. Scope E 308 Practice for Computing the Colors of Objects by

1.1 This test method is intended to be used to compare the
color and strength of a pigment under test with a reference
standard of the same type and grade.
1.2 This test method does not apply to white pigments.
NOTE 1—Test Method D 3022 is similar to this test method, but it
utilizes a miniature sandmill rather than a mechanical muller, to disperse
the color pigment.
NOTE 2—Test Method D 332 and Test Method D 2745 are similar to
this test method, but they are intended for use with white pigments, rather
than color pigments.
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 appro-
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. Specific hazard
statements are given in Section 7.
2. Referenced Documents
2.1 ASTM Standards:
D 332 Test Method for Relative Tinting Strength of White
Pigments by Visual Observation2
D 1729 Practice for Visual Evaluation of Color Differences
of Opaque Materials2
D 2244 Test Method for Calculation of Color Differences
from Instrumentally Measured Color Coordinates2
D 2745 Test Method for Relative Tinting Strength of White
Pigments by Reflective Measurements2
D 3022 Test Method for Color and Strength of Color
Pigments by Use of a Miniature Sandmill2
D 3964 Practice for Selection of Coating Specimens for
Appearance Measurements2
E 97 Test Method for Directional Reflectance Factor, 45-
deg 0-deg, of Opaque Specimens by Broad-Band Filter
Reflectometry3
1
This test method is under the jurisdiction of ASTM Committee D-1 on Paint
and Related Coatings, Materials, and Applications and is the direct responsibility of
Subcommittee D01.26 on Optical Properties.
Current edition approved Aug. 26, 1986. Published October 1986. Originally
published as D 387 – 34 T. Last previous edition D 387 – 81.
2 4
Annual Book of ASTM Standards, Vol 06.01.
3
Discontinued; see 1992 Annual Book of ASTM Standards, Vol 14.02.
Using the CIE System2
3. Summary of Test Method
3.1 Pigments are dispersed in a suitable vehicle with a
mechanical muller. Test and standard pigments are treated
identically. Opaque drawdowns are made from the dispersions
and compared, either visually or instrumentally, for color and
strength differences.
4. Significance and Use
4.1 Color and tinting strength are the most important prop-
erties of a color pigment. This test method provides a means of
testing these properties for quality control.
4.2 This test method is intended as a referee method so that
such matters as the vehicle for preparing the dispersions and
the white for making tints have been suggested. However,
other vehicles and whites may be suitable for quality control
purposes, and changes in this test method are allowed by
agreement between the parties to a test.
4.3 It is assumed that the most exact comparison of mass
color and tinting strength occurs when the pigment is com-
pletely dispersed. By following the procedure described in
Annex A1, the conditions for achieving the maximum practical
degree of dispersion with a mechanical muller may be deter-
mined. Color and strength tests should be carried out under
these conditions.
4.4 The results obtained with a mechanical muller do not
necessarily correlate directly with an industrial situation where
different dispersing conditions exist. However, dispersion with
a mechanical muller is a quick and inexpensive way of testing
the color and strength of a pigment for routine quality control.
5. Apparatus
5.1 Balances—(1) A balance sensitive to 10 mg and (2) an
analytical balance sensitive to 1.0 mg.
5.2 Muller, Mechanical, 4 equipped with ground-glass plates
to which a variable but known force may be added in 50-lbf
(220-N) increments. The driven glass plate shall have a speed
of rotation of between 70 and 120 r/min and the apparatus shall
A satisfactory muller is supplied by the Hoover Color Corp., State Highway
693, P.O. Box 218, Hiwassee, VA 24347.

1
 D 387
have an arrangement for pre-setting the number of revolutions
in multiples of 50.
5.3 Rubbing Surfaces—The rubbing surfaces of the ground
glass plates shall be kept sharp by removing them from the
muller and grinding them face-to-face with No. 303 optical
emery, or its equivalent, and water.
5.4 Small Glass Slab or other nonabsorbent material, suit-
able for weighing and mixing pigment pastes.
5.5 Spatula—A flexible spatula having a 3 to 6-in. (75 to
150-mm) blade.
5.6 Paper Charts,5 white with a black band and a surface
impervious to paint liquids.
5.7 Film Applicator,6 at least 3 in. (75 mm) wide with a
clearance of 4 mils (100 µm) to produce wet films about 2 mils
(50 µm) thick.
5.8 Color-Measuring Instrument, meeting the requirements
of Method D 2244.
6. Materials
6.1 Reference Standard—A standard pigment of the same
type and grade as the pigment to be tested, as agreed upon
between the purchaser and the seller.
6.2 Vehicle—A solvent-free vehicle, such as No. 1 litho-
graphic varnish, with 0.8 % each of cobalt and manganese
driers (6 % types).
6.3 White Tinting Paste—A white paint compatible with the
dispersion vehicle, such as 57 parts of rutile titanium dioxide
dispersed in 43 parts of the vehicle described in 6.2.
NOTE 3—Because the choice of vehicle and white tinting pigment may
affect the results, they should be agreed upon between the purchaser and
the seller.
7. Hazards
7.1 Some pigments may be potentially toxic and therefore
should be handled with care. Obtain specific precautions from
the manufacturer or supplier.
7.2 Many solvents and paint vehicles present explosion, fire,
and toxicity hazards, and they should accordingly be handled
with care. Again, obtain specific precautions from the manu-
facturer or supplier.
8. Dispersing Conditions
8.1 The conditions for dispersing the pigment on the me-
chanical muller should be such that the maximum tinting
strength is developed. For each pigment and each dispersing
vehicle the development of tinting strength by the mechanical
muller is influenced by the force applied, the number of
revolutions, the mass of the pigment, and the mass of the
vehicle. The conditions for obtaining the maximum tinting
strength with the mechanical muller can be determined by
following the procedure in Annex A1.
8.2 If these conditions are known for a particular pigment
with a particular vehicle, or if the purchaser and seller agree
5
White charts with a black band are preferred for judging opacity. Satisfactory
charts are available from the Morest Co., 211 Centre St., New York, NY 10073, and
the Leneta Co., 15 Whitney Rd., Mahwah, NJ 07430.
6
Satisfactory film applicators are available from Bird and Son, Walpole, MA
02081 and Precision Gage & Tool Co., 375 Gargrave Rd, Dayton, OH 45449.
2
upon a particular set of conditions, there is no need to carry out
the procedure in Annex A1.
9. Dispersion Procedure
9.1 Decide, by agreement or by experimentation, as dis-
cussed in Section 8, the following dispersing conditions:
9.1.1 Force applied to the muller plates;
9.1.2 Number of revolutions;
9.1.3 Mass of the pigment; and
9.1.4 Mass of the vehicle.
9.2 Applying these decisions, prepare a dispersion of the
reference standard pigment. Weigh onto a glass slab to within
2 mg, the appropriate quantities of the standard pigment and
the dispersing vehicle. Mix the pigment and vehicle together
thoroughly with the spatula and transfer the mixture to the
lower plate of the muller. Spread the mixture in a path
approximately 100 mm wide and halfway between the center
and rim of the lower plate, and clean the spatula as much as
possible by wiping it on the upper plate of the muller. Close the
plates and carry out the mulling stages of 50 revolutions; after
each stage collect the paste from both plates with the spatula
and spread it around the 100-mm path on the lower plate,
wiping the spatula on the upper plate as before. When the
mulling has been carried out for the prescribed number of
revolutions, collect the paste and store it. Clean the glass slab,
the muller plates, and the spatula, and repeat the procedure
with exactly the same quantities of the test sample and vehicle.
Collect the paste from this sample and store it. Clean the glass
slab, the muller plates, and the spatula.
NOTE 4—The most common sources of error in this procedure are
inaccurate weighing, incomplete transfer of the pigment and vehicle
mixture, and contamination of the plates by previous samples.
10. Masstone Color Procedure
10.1 Draw down a portion of the test and standard pastes in
juxtaposition on a paper chart over a vacuum-drawdown plate
or other suitable plane surface with the film applicator. Make
sure that the coating is opaque.
10.2 Immediately compare the colors visually while still
wet, using Practice D 1729, and record the results. Set the
drawdowns aside in a dust-free area to dry. When dry repeat the
visual color difference evaluation and record the results. See
Practice D 3964.
10.3 If desired, evaluate the color difference instrumentally
using Method D 2244, and report the color difference in units
as agreed upon between the purchaser and seller.
NOTE 5—Wet color difference evaluations may not agree with dry color
difference evaluations because of such phenomena as flooding and
flocculation. In the case of a difference between the wet and dry
evaluations, the purchaser and the seller should agree upon which
condition is the standard.
NOTE 6—Color difference measurements of wet paints may require a
special adapter to protect the instrument from fouling. Because color
difference-measuring instruments differ widely in their design, the user
may have to develop his own adapter.
11. Tint Color Procedure
11.1 Determine by calculation the amount of white pigment
paste that must be added to 0.5 g of the color pigment paste so
that the mixture contains 1 part of dry color pigment to 10 parts
 D 387
of dry white pigment. For stronger or weaker pigments this
ratio may be adjusted accordingly, for example, 1:20 or 1:5,
respectively.
11.2 Weigh 500 6 2 mg of the standard color pigment paste
onto a glass slab. Then weigh the amount of white pigment
paste determined in 11.1, and place it next to the color pigment
paste on the glass slab. Thoroughly mix the two pastes together
with the spatula until a uniform color is observed.
11.3 Prepare a tint mixture of the test color pigment paste
and the white pigment paste on a separate glass slab by the
procedure described in 11.2.
11.4 Draw a portion of the test and standard tint pastes down
in juxtaposition on a paper chart as in 10.1. Evaluate the color
difference visually as in 10.2 and, if desired, instrumentally as
in 10.3. Clean the spatula blade and glass slabs.
12. Calculation of Tinting Strength
12.1 If the colors of the test tint paste and the standard tint
paste are visually the same, the tinting strength of the test
pigment is equal to that of the standard pigment, and the
relative tinting strength of the test pigment is 100 %. However,
if the test and standard colors are not the same, the difference
may be due to tinting strength or hue (shade).
12.2 To determine the relative tinting strength of the test
pigment, repeat the operations of Section 11, but this time use
an amount of the test pigment paste that is estimated to give the
closest color match to the standard pigment paste. Repeat this
procedure until satisfied that the closest color match has been
obtained. At this point any residual color difference between
the test and the standard pigments is attributed to a shade
difference, rather than a strength difference. Note and record
this shade difference.
12.3 Calculate the relative tinting strength of the test pig-
ment by dividing the mass of the standard paste by the mass of
the test paste used to obtain the closest color match; multiply
by 100 to express the result in percent.
12.4 If desired, the relative tinting strength of the sample
pigment can be calculated from instrumental measurements
(see Test Method E 97 or Practice E 308) using the following
equation:
TS 5 @~1 2 R`!2 / 2R`#u / @~1 2 R`!2 / 2R`#s ~T!
where:
TS 5 tinting strength of test pigment,
R` 5 measured reflectant factor (as a decimal),
T 5 assigned tinting strength of standard, usually 100 %,
and subscripts “u” and “s” refer to the test and
standard pigments, respectively.
12.4.1 For R` use the lowest reflectance value measured in
the range 420 to 680 nm with a spectrophotometer or abridged
3
spectrophotometer. This method of calculation is not valid
when any tristimulus value or filter colorimeter reading is
substituted for R` unless it can be demonstrated that with such
a substitution the function (1 − R`)2/2R` still varies linearly
with concentration for the pigments being tested over the range
of concentrations of interest. Because the use of different
parameters may give significantly different results for the
tinting strength, the choice of the parameter to be used as R`
shall be agreed on between the purchaser and the seller.
NOTE 7—This method is not applicable to metameric specimens, or to
specimens exhibiting large shade differences, or to specimens differing in
strength by more than about 30 %.
13. Report
13.1 Report the following information:
13.1.1 Type and identification of the test pigment, reference
standard pigment, white tinting pigment, and dispersing ve-
hicle.
13.1.2 Mass ratio of pigment to vehicle, and for tints mass
ratio of color pigment mass to white pigment.
13.1.3 Manufacturer and model number of the mechanical
muller employed.
13.1.4 Total force applied to the muller plates and total
number of revolutions.
13.1.5 Results of the visual evaluation of the color differ-
ence (masstone and tint) in accordance with Practice D 1729.
13.1.6 If an instrument was used to evaluate the color
difference, the results of the instrumental evaluation in accor-
dance with Method D 2244.
13.1.7 Relative tinting strength and method by which it was
determined (visual or instrumental). Also, for the instrumental
method, the parameter used as the measure of Rin.
13.1.8 Any deviation, by agreement or otherwise, from the
test procedure described above.
14. Precision
14.1 The precision of this test method depends on several
factors such as the type of pigment, the level of tinting, and the
magnitude and direction of the color difference. This point is
illustrated by the results in Table 1, which contains the
between-laboratories standard deviations obtained in an inter-
laboratory study involving five different laboratories and four
different pigments. The dispersing conditions used to obtain
these results are listed in Table 2.
14.2 Table 3 lists the maximum acceptable differences,
calculated at the 95 % confidence level from the results in
Table 1.
 D 387
TABLE 1 Between-Laboratories Standard Deviations for Various Color DifferenceA and Tinting StrengthB Parameters
Masstone Color Tint Color Tinting Strength
Pigment Type
Da Db DL DE Da Db DL DE Y T R V
Yellow Iron Oxide 0.10 0.46 0.22 0.42 0.13 0.20 0.19 0.08 2.0 2.2 3.0 0.7
BON Red 0.12 0.37 0.20 0.28 0.29 0.31 0.07 0.24 0.7 1.8 1.1 2.5
Molybdate Orange 0.09 0.14 0.06 0.11 0.11 0.12 0.05 0.14 0.5 0.8 0.6 1.0
Phthalocyanine GreenC 0.29 0.65 1.43 0.51 0.25 0.07 0.13 0.21 1.6 1.8 2.6 1.8
A
Color difference values were calculated with the CIE 1976 L*a*b* (CIELAB) equation.
B
Tinting strengths were calculated four different ways with the equation in 12.2: Y, based on Y tristimulus value; T, based on lowest tristimulus value; R, based on lowest
reflectance factor between 420 nm and 680 nm; and V, based on visual observation.
C
Severe bronzing occurred with the masstone of this pigment (more in the batch than the standard), which probably affected the color difference measurements made
with different types of instruments.

TABLE 2 Dispersing Conditions Used in Interlaboratory Study

Molybdate
Pigment type Pthalocyanine Green Yellow Iron Oxide BON Red
Orange
Force applied to the muller plates, lb (N) 100 (440) 100 (440) 100 (440) 100 (440)
Total number of revolutions 400 (8 3 50) 100 (2 3 50) 200 (4 3 50) 100 (2 3 50)
Mass of color pigment, g 0.75 1.0 0.6 2.0
Mass of dispersing vehicle, g 1.8 1.7 1.4 1.0

TABLE 3 Maximum Acceptable Differences for Various Color DifferenceA and Tinting StrengthB Parameters
Masstone Color Tint Color Tinting Strength
Pigment Type Y
Da Db DL DE Da Db DL DE T R V

Yellow Iron Oxide 0.28 1.30 0.62 1.19 0.37 0.57 0.54 0.23 5.7 6.2 8.5 2.0
BON Red 0.34 1.05 0.57 0.79 0.82 0.88 0.20 0.68 2.0 5.1 3.1 7.1
Molybdate Orange 0.25 0.40 0.17 0.31 0.31 0.34 0.14 0.40 1.4 2.3 1.7 2.8
Pthalocyanine GreenC 0.82 1.84 4.04 1.44 0.71 0.20 0.37 0.59 4.5 5.1 7.4 5.1
A
Color difference values were calculated with the CIE 1976 L*a*b* (CIELAB) equation.
B
Tinting strengths were calculated four different ways with the equation in 12.2: Y, based on Y tristimulus value; T, based on lowest tristimulus value; R, based on lowest
reflectance factor between 420 nm and 680 nm; and V, based on visual observation.
C
Severe bronzing occurred with the masstone of this pigment (more in the batch than the standard), which probably affected the color difference measurements made
with different types of instruments.

ANNEX

(Mandatory Information)

A1. DISPERSING CONDITIONS FOR MAXIMUM TINTING STRENGTH

A1.1 The following describes a test method for determining
the conditions for achieving the maximum level of tinting
strength with the mechanical muller.
A1.2 Determine the appropriate ratio of color pigment to
dispersing vehicle by performing the following operations:
Tare off the weight of a glass slab on a balance. Weigh 1.00 6
0.01 g of the standard pigment on to the glass slab. Add
dispersing vehicle to the pigment in small amounts and mix
them together with the spatula. Keep adding the vehicle and
mixing the paste until the pigment is completely wetted and a
workable paste is obtained. At this point the consistency of the
paste should be such that a dab of the paste will drop from the
spatula when it is gently tapped with the finger. Weigh the
paste, and subtract the mass of the pigment to determine the
mass of the vehicle. Calculate the pigment to vehicle mass
ratio. Repeat the operations described above for the test
pigment.
A1.3 Determine the appropriate amount of pigment to use
by estimating, to within 0.2 mL, the volume of that paste
prepared in A1.2 that has the smallest pigment-to-vehicle mass
ratio. Calculate the masses of pigment and vehicle needed to
give a paste having a volume of about 2.0 mL. Round the
amount of pigment down and the amount of vehicle up to the
nearest 0.1 g.
A1.4 Apply 100 lbf (440 N) to the muller plates and prepare
a tint of the standard pigment in accordance with the procedure
in Sections 9 and 11. Use the amounts of the color pigment and
dispersing vehicle determined in A1.3 and mull the paste for
100 revolutions in two stages of 50 revolutions each.
A1.5 Prepare three more specimens from the same sample
following the procedure described in A1.4, but mull these
specimens, in stages of 50 revolutions, for 200, 300, and 400
revolutions, respectively.
A1.6 Compare each of the four specimens, one to the other,
for tinting strength using one of the methods described in
Section 12, and determine the minimum number of revolutions
necessary to achieve full tinting strength. If the tinting strength

4
 D 387
is still developing after 400 revolutions, repeat A1.4-A1.6 with A1.8 Table 2 lists, as examples, the dispersing conditions
50 lbf (220 N) more force on the mechanical muller plates. used in the interlaboratory study that established the precision
given in Table 1 and Table 3. The vehicle used was No. 1
A1.7 Record the appropriate amounts of pigment and lithographic varnish with 0.8 % each of cobalt and manganese
vehicle (by A1.3), the force applied to the mechanical muller
driers (6 % types).
plates and the minimum number of revolutions required for
maximum tinting strength.

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if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
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5
 Designation: D 402 – 97 American Association State
Highway and Transportation Officials Standard
AASHTO No.: T78

27/74 (88)

Standard Test Method for

Distillation of Cut-Back Asphaltic (Bituminous) Products1
This standard is issued under the fixed designation D 402; 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.

This standard has been approved for use by agencies of the Department of Defense. This method was adopted as a joint ASTM-IP
standard in 1961.

1. Scope distillation, and also the distillate, may be tested as required.

1.1 This test method covers a distillation test for cut-back
asphaltic (bituminous) products.
1.2 The values given in SI units are to be regarded as the
standard.
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 appro-
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
2. Referenced Documents
2.1 ASTM Standards:
D 86 Test Method for Distillation of Petroleum Products2
D 370 Test Method for Dehydration of Oil-Type Preserva-
tives3
E 1 Specification for ASTM Thermometers4
E 133 Specification for Distillation Equipment5
2.2 IP Standards:
IP 123/ASTM D 86, Distillation of Petroleum Products
Thermometers as specified in IP Standards
Crow Receiver as specified in British Standards 658:1962
C.O.3—Standard Methods for Testing Tar and its Products
(Published by the U.K. Standardization of Tar Products
Tests Committee)
3. Summary of Method
3.1 Two hundred millilitres of the sample are distilled in a
500-mL flask at a controlled rate to a temperature in the liquid
of 360°C (680°F) and the volumes of distillate obtained at
specified temperatures are measured. The residue from the
1
This test method is under the jurisdiction of ASTM Committee D-4 on Road
and Paving Materials and is the direct responsibility of Subcommittee D04.46on
Durability Tests.
Current edition approved Nov. 10, 1997. Published February 1998. Originally
published as D 402 – 34 T. Last previous edition D 402 – 94.
In the IP, this method is under the jurisdiction of the Standardization Committee.
2
Annual Book of ASTM Standards, Vol 05.01.
3
Annual Book of ASTM Standards, Vol 04.09.
4
Annual Book of ASTM Standards, Vol 14.03.
5
Annual Book of ASTM Standards, Vol 14.02.
4. Significance and Use
4.1 This procedure measures the amount of the more vola-
tile constituents in cut-back asphaltic products. The properties
of the residue after distillation are not necessarily characteristic
of the bitumen used in the original mixture nor of the residue
which may be left at any particular time after application of the
cut-back asphaltic product. The presence of silicone in the
cut-back may affect the distillation residue by retarding the loss
of volatile material after the residue has been poured into the
residue container.
5. Apparatus
5.1 Distillation Flask, 500-mL side-arm, having the dimen-
sions shown in Fig. 1.
5.2 Condenser, standard glass-jacketed, of nominal jacket
length from 200 to 300 mm and overall tube length of 450 6
10 mm (see Fig. 3).
5.3 Adapter, heavy-wall (1-mm) glass, with reinforced top,
having an angle of approximately 105°. The inside diameter at
the large end shall be approximately 18 mm, and at the small
end, not less than 5 mm. The lower surface of the adapter shall
be on a smooth descending curve from the larger end to the
smaller. The inside line of the outlet end shall be vertical, and
the outlet shall be cut or ground (not fire-polished) at an angle
of 45 6 5° to the inside line.
5.4 Shield, steel, lined with 3-mm fire proof insulation and
fitted with transparent mica windows, of the form and dimen-
sions shown in Fig. 2, used to protect the flask from air currents
and to reduce radiation. The cover (top) shall be made in two
parts of 6.4-mm (1⁄4-in.) fire proof insulation.
5.5 Shield and Flask Support—Two 15-cm2 sheets of 16-
mesh Chromel wire gauze on a tripod or ring.
5.6 Heat Source—
5.6.1 Adjustable Tirrill-type gas burner or equivalent.
5.6.2 An electric heater equipped with a transformer ca-
pable of controlling from 0 to 750 W. The shield and support
shall be a refractory with an opening of 31⁄8in. (79 mm), with
the upper surface beleveled to 33⁄8 in. (86 mm) to accommodate

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

1
 D 402

FIG. 1 Distillation Flask

FIG. 2 Shield

the specified 500-mL flask. When the flask is placed on the
refractory, there should be a distance of approximately 1⁄8 in. (3
mm) between the bottom of the flask and the heating elements.
5.7 Receiver—A standard 100-mL graduated cylinder con-
forming to dimensions of Fig. 4 of Specification E 133, or
a 100-mL crow receiver as shown in Fig. 4 of this test method.
NOTE 1—Receivers of smaller capacity having 0.1-mL divisions may
be used when low volumes of total distillate are expected and the added
accuracy required.
5.8 Residue Container—An 8-oz seamless metal container
with slip on cover of 75 6 5 mm in diameter, and 55 6 5 mm
in height.
5.9 Thermometer— ASTM Thermometers 8C (8F) con-
forming to Specification E 1, or IP Thermometer 6C conform-
ing to IP Specifications for Standard Thermometers.
6. Sampling
6.1 Stir the sample thoroughly, warming if necessary, to
ensure homogeneity before removal of a portion for analysis.
6.2 If sufficient water is present to cause foaming or
bumping, dehydrate a sample of not less than 250 mL by
heating in a distillation flask sufficiently large to prevent
foaming over into the side arm. When foaming has ceased, stop
the distillation. If any light oil has distilled over, separate and

2
 D 402
FIG. 3 Distillation Apparatus
All dimensions are in millimetres
FIG. 4 Crow Receivers of Capacity 25, 50, and 100 mL
pour this back into the flask when the contents have cooled just
sufficiently to prevent loss of volatile oil. Mix the contents of
the flask thoroughly before removal for analysis. An alternative
procedure is described in Test Method D 370.
7. Preparation of Apparatus
7.1 Calculate the weight of 200 mL of the sample from the
specific gravity of the material at 15.6/15.6°C (60/60°F).
Weigh this amount 6 0.5 g into the 500-mL flask.
7.2 Place the flask in the shield supported by two sheets of
gauze on a tripod or ring. Connect the condenser tube to the
tubulature of the flask with a tight cork joint. Clamp the
condenser so that the axis of the bulb of the flask through the
center of its neck is vertical. Adjust the adapter over the end of
the condenser tube so that the distance from the neck of the
flask to the outlet of the adapter is 650 6 50 mm (see Fig. 3).
7.3 Insert the thermometer through a tightly fitting cork in
the neck of the flask so that the bulb of the thermometer rests
on the bottom of the flask. Raise the thermometer 6.4 mm (1⁄4
in.) from the bottom of the flask using the scale divisions on the
3
thermometer to estimate the 6.4-mm (1⁄4-in.) distance above the
top of the cork.
7.4 Protect the burner by a suitable shield or chimney. Place
the receiver so that the adapter extends at least 25 mm but not
below the 100-mL mark. Cover the graduate closely with a
piece of blotting paper, or similar material, suitably weighted,
which has been cut to fit the adapter snugly.
7.5 The flask, condenser tube, adapter, and receiver shall be
clean and dry before starting the distillation. Place the 8-oz
residue container on its cover in an area free from drafts.
7.6 Pass cold water through the condenser jacket. Use warm
water if necessary to prevent formation of solid condensate in
the condenser tube.
8. Procedure
8.1 Correct the temperatures to be observed in the distilla-
tion if the elevation of the laboratory at which the distillation
is made deviates (150 m) 500 ft or more from sea level.
Corrected temperatures for the effect of altitude are shown in
Table 1 and Table 2. If the prevailing barometric pressure in
millimetres of mercury is known, correct the temperature to be
observed with the corrections shown in Table 3. Do not correct
for the emergent stem of the thermometer.
NOTE 2—Table 3 covers a wide range of temperatures from 160 to
360°C and is to be preferred for world-wide specifications other than
ASTM/IP specifications.
8.2 Apply heat so that the first drop of distillate falls from
the end of the flask side-arm in 5 to 15 min. Conduct the
distillation so as to maintain the following drop rates, the drop
count to be made at the tip of the adapter:
50 to 70 drops per minute to 260°C (500°F)
20 to 70 drops per minute between 260 and 316°C (500 and 600°F)
Not over 10 min to complete distillation from 316 to 360°C (600 to 680°F)
8.2.1 Record the volumes of distillate to the nearest 0.5 mL
in the receiver at the corrected temperatures. If the volume of
distillate recovered is critical, use receivers graduated in
 D 402
TABLE 1 Corrected Fractionation Temperatures for Various (600°F). In this case it becomes impractical to maintain the above
Altitudes, °C distillation rates. For such cases the intent of the method shall be met if the
Elevation above rate of rise of temperature exceeds 5°C (9°F)/min.
Fractionation Temperatures for Various Altitudes, °C
Sea Level, m (ft)
8.3 When the temperature reaches the corrected temperature
−305 (−1000) 192 227 363 318 362
of 360°C (680°F), cut off the heat and remove the flask and
−152 (−500) 191 226 261 317 361
0 (0) 190 225 260 316 360 thermometer. With the flask in a pouring position, remove the
152 (500) 189 224 259 315 359 thermometer and immediately pour the contents into the
305 (1000) 189 224 258 314 358
457 (1500) 188 223 258 313 357
residue container. The total time from cutting off the heat to
610 (2000) 187 222 257 312 356 starting the pour shall not exceed 15 s. When pouring, the
762 (2500) 186 221 256 312 355 side-arm should be substantially horizontal to prevent conden-
914 (3000) 186 220 255 311 354
1067 (3500) 185 220 254 310 353
sate in the side-arm from being returned to the residue.
1219 (4000) 184 219 254 309 352 NOTE 4—The formation of skin on the surface of a residue during
1372 (4500) 184 218 253 308 351
1524 (5000) 183 218 252 307 350
cooling entraps vapors which will condense and cause higher penetration
1676 (5500) 182 217 251 306 349 results when they are stirred back into the sample. If skin begins to form
1829 (6000) 182 216 250 305 349 during cooling, it should be gently pushed aside. This can be done with a
1981 (6500) 181 215 250 305 348 spatula with a minimum of disturbance to the sample.
2134 (7000) 180 215 249 304 347
2286 (7500) 180 214 248 303 346 8.4 Allow the condenser and any distillates trapped in the
2438 (8000) 179 213 248 302 345 condenser neck to drain into the receiver and record the total
volume of distillate collected as total distillate to 360°C
(680°F).
TABLE 2 Corrected Fractionation Temperatures for Various
8.5 When the residue has cooled until fuming just ceases,
Altitudes, °F
stir thoroughly and pour into the receptacles for testing for
Elevation above
sea level, m (ft)
Fractionation Temperatures for Various Altitudes, °F properties such as penetration, viscosity, or softening point.
Proceed as required by the appropriate ASTM or IP method
−305 (−1000) 377 440 503 604 684
−152 (−500) 375 438 502 602 682 from the point that follows the pouring stage.
0 (0) 374 437 500 600 680 8.6 If desired, the distillate, or the combined distillates from
152 (500) 373 436 498 598 678 several tests, may be submitted to a further distillation, in
305 (1000) 371 434 497 597 676
457 (1500) 370 433 495 595 675 accordance with Test Method D 86 – IP 123, or, when the
610 (2000) 369 431 494 593 673 distillate is of coal-tar origin, Method C.O.3.
762 (2500) 367 430 492 592 671
914 (3000) 366 429 491 590 669
1067 (3500) 365 427 490 588 667
9. Calculation and Report
1219 (4000) 364 426 488 587 666 9.1 Asphaltic Residue—Calculate the percent residue to the
1372 (4500) 363 425 487 585 665
1524 (5000) 361 423 485 584 663 nearest 0.1 as follows:
1676 (5500) 360 422 484 582 661 R 5 @~200 2 TD!/200# 3 100 (1)
1829 (6000) 359 421 483 581 660
1981 (6500) 358 420 481 580 658
2134 (7000) 357 418 480 578 656
where:
2286 (7500) 356 417 479 577 655 R 5 residue content, in volume percent, and
2438 (8000) 355 416 478 575 653 TD 5 total distillate recovered to 360°C (680°F), mL.
9.1.1 Report as the residue from distillation to 360 (680°F),
percent volume by difference.
TABLE 3 Factors for Calculating Temperature Corrections 9.2 Total Distillate— Calculate the percent total distillate to
CorrectionA per 10 mm the nearest 0.1 as follows:
Nominal Temperatures,
Difference in Pressure,
°C (°F)
°C (°F) TD % 5 ~TD/200! 3 100 (2)
160 (320) 0.514 (0.925) 9.2.1 Report as the total distillate to 360°C (680°F), volume
175 (347) 0.531 (0.957)
190 (374) 0.549 (0.989)
percent.
225 (437) 0.591 (1.063) 9.3 Distillate Fractions:
250 (482) 0.620 (1.116) 9.3.1 Determine the percentages by volume of the original
260 (500) 0.632 (1.138)
275 (527) 0.650 (1.170)
sample by dividing the observed volume (in millilitres) of the
300 (572) 0.680 (1.223) fraction by 2. Report to the nearest 0.1 as volume percent as
315.6 (600) 0.698 (1.257) follows:
325 (617) 0.709 (1.277)
360 (680) 0.751 (1.351)
Up to 190°C (374°F)
A
To be subtracted in case the barometric pressure is below 760 mm Hg; to be
Up to 225°C (437°F)
added in case barometric pressure is above 760 mm Hg. Up to 260°C (500°F)
Up to 316°C (600°F)
0.1-mL divisions and immersed in a transparent bath main- 9.3.2 Determine the percentages by volume of total distil-
tained at 15.6 6 3°C (60 6 5°F). late by dividing the observed volume in millilitres of the
NOTE 3—Some cut-back asphaltic products yield either no distillate or fraction by the millilitres recovered to 360°C (680°F) and
very little distillate over portions of the temperature range to 316°C multiply by 100. Report to the nearest 0.1 as the distillate,

4
 D 402
volume percent of total distillate to 360°C (680°F) as follows:
Up to 190°C (374°F)
Up to 225°C (437°F)
Up to 260°C (500°F)
Up to 316°C (600°F)
9.4 Where penetration, viscosity, or other tests have been
carried out, report with reference to this test method as well as
to any other method used. Example—Penetration (ASTM D5
or IP 49) of residue from ASTM D402/IP 27.
10. Precision and Bias
10.1 The following criteria shall be used for judging the
acceptability of results (95 % probability):
10.1.1 Repeatability— Duplicate values by the same opera-
tor shall not be considered suspect unless the determined
percentages differ by more than 1.0 volume % of the original
sample.
10.1.2 Reproducibility— The values reported by each of
two laboratories, shall not be considered suspect unless the
reported percentages differ by more than the following:
Distillation Fractions, volume percent of the original sample:
Up to 175°C (347°F) 3.5
Above 175°C (347°F) 2.0
Residue, Volume percentage by difference from the original sample 2.0
10.2 Criteria for judging variability of test results on the
distillation residue have not been determined.
11. Keywords
11.1 cut-back asphalt; distillate; residue

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