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

1
 D 387
have an arrangement for pre-setting the number of revolutions upon a particular set of conditions, there is no need to carry out
in multiples of 50. the procedure in Annex A1.
5.3 Rubbing Surfaces—The rubbing surfaces of the ground 9. Dispersion Procedure
glass plates shall be kept sharp by removing them from the
muller and grinding them face-to-face with No. 303 optical 9.1 Decide, by agreement or by experimentation, as dis-
emery, or its equivalent, and water. cussed in Section 8, the following dispersing conditions:
5.4 Small Glass Slab or other nonabsorbent material, suit- 9.1.1 Force applied to the muller plates;
able for weighing and mixing pigment pastes. 9.1.2 Number of revolutions;
5.5 Spatula—A flexible spatula having a 3 to 6-in. (75 to 9.1.3 Mass of the pigment; and
150-mm) blade. 9.1.4 Mass of the vehicle.
5.6 Paper Charts,5 white with a black band and a surface 9.2 Applying these decisions, prepare a dispersion of the
impervious to paint liquids. reference standard pigment. Weigh onto a glass slab to within
5.7 Film Applicator,6 at least 3 in. (75 mm) wide with a 2 mg, the appropriate quantities of the standard pigment and
clearance of 4 mils (100 µm) to produce wet films about 2 mils the dispersing vehicle. Mix the pigment and vehicle together
(50 µm) thick. thoroughly with the spatula and transfer the mixture to the
5.8 Color-Measuring Instrument, meeting the requirements lower plate of the muller. Spread the mixture in a path
of Method D 2244. approximately 100 mm wide and halfway between the center
and rim of the lower plate, and clean the spatula as much as
6. Materials possible by wiping it on the upper plate of the muller. Close the
6.1 Reference Standard—A standard pigment of the same plates and carry out the mulling stages of 50 revolutions; after
type and grade as the pigment to be tested, as agreed upon each stage collect the paste from both plates with the spatula
between the purchaser and the seller. and spread it around the 100-mm path on the lower plate,
6.2 Vehicle—A solvent-free vehicle, such as No. 1 litho- wiping the spatula on the upper plate as before. When the
graphic varnish, with 0.8 % each of cobalt and manganese mulling has been carried out for the prescribed number of
driers (6 % types). revolutions, collect the paste and store it. Clean the glass slab,
6.3 White Tinting Paste—A white paint compatible with the the muller plates, and the spatula, and repeat the procedure
dispersion vehicle, such as 57 parts of rutile titanium dioxide with exactly the same quantities of the test sample and vehicle.
dispersed in 43 parts of the vehicle described in 6.2. Collect the paste from this sample and store it. Clean the glass
slab, the muller plates, and the spatula.
NOTE 3—Because the choice of vehicle and white tinting pigment may
affect the results, they should be agreed upon between the purchaser and NOTE 4—The most common sources of error in this procedure are
the seller. inaccurate weighing, incomplete transfer of the pigment and vehicle
mixture, and contamination of the plates by previous samples.
7. Hazards
10. Masstone Color Procedure
7.1 Some pigments may be potentially toxic and therefore
should be handled with care. Obtain specific precautions from 10.1 Draw down a portion of the test and standard pastes in
the manufacturer or supplier. juxtaposition on a paper chart over a vacuum-drawdown plate
7.2 Many solvents and paint vehicles present explosion, fire, or other suitable plane surface with the film applicator. Make
and toxicity hazards, and they should accordingly be handled sure that the coating is opaque.
with care. Again, obtain specific precautions from the manu- 10.2 Immediately compare the colors visually while still
facturer or supplier. wet, using Practice D 1729, and record the results. Set the
drawdowns aside in a dust-free area to dry. When dry repeat the
8. Dispersing Conditions visual color difference evaluation and record the results. See
8.1 The conditions for dispersing the pigment on the me- Practice D 3964.
chanical muller should be such that the maximum tinting 10.3 If desired, evaluate the color difference instrumentally
strength is developed. For each pigment and each dispersing using Method D 2244, and report the color difference in units
vehicle the development of tinting strength by the mechanical as agreed upon between the purchaser and seller.
muller is influenced by the force applied, the number of NOTE 5—Wet color difference evaluations may not agree with dry color
revolutions, the mass of the pigment, and the mass of the difference evaluations because of such phenomena as flooding and
vehicle. The conditions for obtaining the maximum tinting flocculation. In the case of a difference between the wet and dry
strength with the mechanical muller can be determined by evaluations, the purchaser and the seller should agree upon which
condition is the standard.
following the procedure in Annex A1. NOTE 6—Color difference measurements of wet paints may require a
8.2 If these conditions are known for a particular pigment special adapter to protect the instrument from fouling. Because color
with a particular vehicle, or if the purchaser and seller agree difference-measuring instruments differ widely in their design, the user
may have to develop his own adapter.
5
White charts with a black band are preferred for judging opacity. Satisfactory 11. Tint Color Procedure
charts are available from the Morest Co., 211 Centre St., New York, NY 10073, and
the Leneta Co., 15 Whitney Rd., Mahwah, NJ 07430.
11.1 Determine by calculation the amount of white pigment
6
Satisfactory film applicators are available from Bird and Son, Walpole, MA paste that must be added to 0.5 g of the color pigment paste so
02081 and Precision Gage & Tool Co., 375 Gargrave Rd, Dayton, OH 45449. that the mixture contains 1 part of dry color pigment to 10 parts

2
 D 387
of dry white pigment. For stronger or weaker pigments this spectrophotometer. This method of calculation is not valid
ratio may be adjusted accordingly, for example, 1:20 or 1:5, when any tristimulus value or filter colorimeter reading is
respectively. substituted for R` unless it can be demonstrated that with such
11.2 Weigh 500 6 2 mg of the standard color pigment paste a substitution the function (1 − R`)2/2R` still varies linearly
onto a glass slab. Then weigh the amount of white pigment with concentration for the pigments being tested over the range
paste determined in 11.1, and place it next to the color pigment of concentrations of interest. Because the use of different
paste on the glass slab. Thoroughly mix the two pastes together parameters may give significantly different results for the
with the spatula until a uniform color is observed. tinting strength, the choice of the parameter to be used as R`
11.3 Prepare a tint mixture of the test color pigment paste shall be agreed on between the purchaser and the seller.
and the white pigment paste on a separate glass slab by the
NOTE 7—This method is not applicable to metameric specimens, or to
procedure described in 11.2. specimens exhibiting large shade differences, or to specimens differing in
11.4 Draw a portion of the test and standard tint pastes down strength by more than about 30 %.
in juxtaposition on a paper chart as in 10.1. Evaluate the color
difference visually as in 10.2 and, if desired, instrumentally as 13. Report
in 10.3. Clean the spatula blade and glass slabs.
13.1 Report the following information:
12. Calculation of Tinting Strength 13.1.1 Type and identification of the test pigment, reference
standard pigment, white tinting pigment, and dispersing ve-
12.1 If the colors of the test tint paste and the standard tint hicle.
paste are visually the same, the tinting strength of the test
13.1.2 Mass ratio of pigment to vehicle, and for tints mass
pigment is equal to that of the standard pigment, and the
ratio of color pigment mass to white pigment.
relative tinting strength of the test pigment is 100 %. However,
if the test and standard colors are not the same, the difference 13.1.3 Manufacturer and model number of the mechanical
may be due to tinting strength or hue (shade). muller employed.
12.2 To determine the relative tinting strength of the test 13.1.4 Total force applied to the muller plates and total
pigment, repeat the operations of Section 11, but this time use number of revolutions.
an amount of the test pigment paste that is estimated to give the 13.1.5 Results of the visual evaluation of the color differ-
closest color match to the standard pigment paste. Repeat this ence (masstone and tint) in accordance with Practice D 1729.
procedure until satisfied that the closest color match has been 13.1.6 If an instrument was used to evaluate the color
obtained. At this point any residual color difference between difference, the results of the instrumental evaluation in accor-
the test and the standard pigments is attributed to a shade dance with Method D 2244.
difference, rather than a strength difference. Note and record 13.1.7 Relative tinting strength and method by which it was
this shade difference. determined (visual or instrumental). Also, for the instrumental
12.3 Calculate the relative tinting strength of the test pig- method, the parameter used as the measure of Rin.
ment by dividing the mass of the standard paste by the mass of 13.1.8 Any deviation, by agreement or otherwise, from the
the test paste used to obtain the closest color match; multiply test procedure described above.
by 100 to express the result in percent.
12.4 If desired, the relative tinting strength of the sample 14. Precision
pigment can be calculated from instrumental measurements
(see Test Method E 97 or Practice E 308) using the following 14.1 The precision of this test method depends on several
equation: factors such as the type of pigment, the level of tinting, and the
magnitude and direction of the color difference. This point is
TS 5 @~1 2 R`!2 / 2R`#u / @~1 2 R`!2 / 2R`#s ~T! illustrated by the results in Table 1, which contains the
where: between-laboratories standard deviations obtained in an inter-
TS 5 tinting strength of test pigment, laboratory study involving five different laboratories and four
R` 5 measured reflectant factor (as a decimal), different pigments. The dispersing conditions used to obtain
T 5 assigned tinting strength of standard, usually 100 %, these results are listed in Table 2.
and subscripts “u” and “s” refer to the test and 14.2 Table 3 lists the maximum acceptable differences,
standard pigments, respectively. calculated at the 95 % confidence level from the results in
12.4.1 For R` use the lowest reflectance value measured in Table 1.
the range 420 to 680 nm with a spectrophotometer or abridged

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

The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection
with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such
patent rights, and the risk of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible
technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your
views known to the ASTM Committee on Standards, 100 Barr Harbor Drive, West Conshohocken, PA 19428.

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

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

2
 D 402

FIG. 3 Distillation Apparatus

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.

All dimensions are in millimetres 8. Procedure

FIG. 4 Crow Receivers of Capacity 25, 50, and 100 mL 8.1 Correct the temperatures to be observed in the distilla-
tion if the elevation of the laboratory at which the distillation
pour this back into the flask when the contents have cooled just is made deviates (150 m) 500 ft or more from sea level.
sufficiently to prevent loss of volatile oil. Mix the contents of Corrected temperatures for the effect of altitude are shown in
the flask thoroughly before removal for analysis. An alternative Table 1 and Table 2. If the prevailing barometric pressure in
procedure is described in Test Method D 370. millimetres of mercury is known, correct the temperature to be
observed with the corrections shown in Table 3. Do not correct
7. Preparation of Apparatus for the emergent stem of the thermometer.
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). 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
Weigh this amount 6 0.5 g into the 500-mL flask.
ASTM/IP specifications.
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 8.2 Apply heat so that the first drop of distillate falls from
tubulature of the flask with a tight cork joint. Clamp the the end of the flask side-arm in 5 to 15 min. Conduct the
condenser so that the axis of the bulb of the flask through the distillation so as to maintain the following drop rates, the drop
center of its neck is vertical. Adjust the adapter over the end of count to be made at the tip of the adapter:
the condenser tube so that the distance from the neck of the 50 to 70 drops per minute to 260°C (500°F)
flask to the outlet of the adapter is 650 6 50 mm (see Fig. 3). 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)
7.3 Insert the thermometer through a tightly fitting cork in
the neck of the flask so that the bulb of the thermometer rests 8.2.1 Record the volumes of distillate to the nearest 0.5 mL
on the bottom of the flask. Raise the thermometer 6.4 mm (1⁄4 in the receiver at the corrected temperatures. If the volume of
in.) from the bottom of the flask using the scale divisions on the distillate recovered is critical, use receivers graduated in

3
 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: percentages differ by more than 1.0 volume % of the original
Up to 190°C (374°F) sample.
Up to 225°C (437°F) 10.1.2 Reproducibility— The values reported by each of
Up to 260°C (500°F) two laboratories, shall not be considered suspect unless the
Up to 316°C (600°F) reported percentages differ by more than the following:
9.4 Where penetration, viscosity, or other tests have been Distillation Fractions, volume percent of the original sample:
carried out, report with reference to this test method as well as Up to 175°C (347°F) 3.5
to any other method used. Example—Penetration (ASTM D5 Above 175°C (347°F) 2.0
Residue, Volume percentage by difference from the original sample 2.0
or IP 49) of residue from ASTM D402/IP 27.
10. Precision and Bias 10.2 Criteria for judging variability of test results on the
distillation residue have not been determined.
10.1 The following criteria shall be used for judging the
acceptability of results (95 % probability):
11. Keywords
10.1.1 Repeatability— Duplicate values by the same opera-
tor shall not be considered suspect unless the determined 11.1 cut-back asphalt; distillate; residue

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