Designation: C 461 – 81 (Reapproved 2003)

Standard Test Methods for

Mastics and Coatings Used With Thermal Insulation1
This standard is issued under the fixed designation C 461; 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.

1. Scope D 217 Test Method for Cone Penetration of Lubricating

1.1 These test methods cover procedures for sampling and Grease3
testing mastics and coatings for use as weather and vapor D 2196 Test Methods for Rheological Properties of Non-
barrier finishes on thermal insulations and for other accessory Newtonian Materials By Rotational (Brookfield type)
use. Viscometer5
1.2 The values stated in inch-pound units are to be regarded D 3278 Test Methods for Flash Point of Liquids by Small
as the standard. The metric equivalents of inch-pound units Scale Closed-Cup Apparatus5
may be approximate. 3. Terminology
1.3 The test methods appear in the following order:
Section
3.1 Definitions—For definitions of terms used in these test
Sampling 4 methods, see Terminology C 168.
Uniformity and Storage Stability 5
Stability Under Freezing 6 4. Sampling
Density and Weight per Gallon 7
Consistency 8 4.1 Prior to opening or sampling, or both, any mastic or
Solids Content 9 coating, its Material Safety Data Sheet (MSDS) should be
Content of Volatiles and Coverage of Mastics and Coatings 10
Build 11
reviewed to ensure appropriate precautions or personal protec-
Drying Time 12 tive equipment, or both, are utilized.
Flash Point 13 4.2 Take the samples for laboratory examination from the
1.4 This standard does not purport to address all of the original containers immediately after stirring to a uniform
safety concerns, if any, associated with its use. It is the condition. Determine the number of containers sampled as
responsibility of the user of this standard to establish appro- required to represent a shipment in accordance with Practice
priate safety and health practices and determine the applica- D 140. Restir the composite sample immediately before taking
bility of regulatory limitations prior to use. out portions for individual tests.

2. Referenced Documents 5. Uniformity and Storage Stability

2.1 ASTM Standards: 5.1 Open the original containers and examine them for
C 168 Terminology Relating to Thermal Insulation2 uniformity of contents. Record the degree of separation, if any,
C 419 Practice for Making and Curing Test Specimens of into portions of appreciably different consistency, such as thick
Mastic Thermal Insulation Coatings2 or thin layers, sedimentation or coagulation, etc., also of
D 56 Test Method for Flash Point by Tag Closed Tester3 difficulty encountered in stirring to a uniform condition.
D 71 Test Method for Relative Density of Solid Pitch and 5.2 Examine the contents of a full container of not less than
Asphalt (Displacement Method)3 1 qt (1 L) that has stood undisturbed for 48 h. Make notation
D 93 Test Methods for Flash Point by Pensky-Martens of any separation of solvent or water, coagulation, or settle-
Closed Cup Tester3 ment of suspended matter, that cannot be overcome by mod-
D 140 Practice for Sampling Bituminous Materials4 erate agitation.
5.3 Additionally, if required, examine and report the condi-
tion in the container after 3 months’ storage, examining for
1
These test methods are under the jurisdiction of ASTM Committee C16 on uniformity in accordance with 5.1.
Thermal Insulation and are the direct responsibility of Subcommittee C16.33 on
Insulation Finishes and Moisture.
Current edition approved April 10, 2003. Published July 2003. Originally
approved in 1960. Last previous edition approved in 1997 as C 461 – 81 (1997)e1.
2
Annual Book of ASTM Standards, Vol 04.06.
3
Annual Book of ASTM Standards, Vol 05.01.
4 5
Annual Book of ASTM Standards, Vol 04.03. Annual Book of ASTM Standards, Vol 06.01.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

1
 C 461 – 81 (2003)
6. Stability Under Freezing between filling the cup and the reading to avoid temperature
6.1 Fill a 1-pt (500-mL) press-top tin can three quarters full change of the sample. Report the average of the three tests to
with the coating, and hold the filled and closed container in a the nearest 0.1 mm as the penetration of the sample.
chamber at a temperature of 0 6 5°F (−18 6 3°C) for a 8.4 The practical limit of cone penetration is 375. If
minimum of 12 h consecutively under natural convection readings above this value are obtained, or if specified, an
conditions. aluminum cone and shaft with a total weight of 50 g may be
6.2 At the expiration of the freezing period, permit the used in place of the 150-g cone and shaft specified in Test
coating to warm to room temperature by exposure of the Method D 217. If with this modification, readings exceed a
container to the temperature of the laboratory for a minimum of penetration of 375, consistency alternatively may be deter-
6 h. After the first operation of freezing and thawing, repeat the mined by Test Method D 2196. The helipath stand and T-bar
procedure twice so that the coating will have been subjected to spindles may be used.
three cycles of freezing and thawing.
6.3 After the completion of the third cycle, open the 9. Solids Content
container, and note any separation of solvent or water, coagu-
9.1 Weigh about 5 g of material to the nearest 0.01 g into a
lation, settlement of suspended matter, or the presence of
weighed flat-bottom metal dish or container (Note 1). Place the
distinct layers, or a combination of these. If the compound
dish and its contents in an oven at 105 6 2°C (220 6 5°F) for
cannot be rendered homogeneous by moderate stirring at
2 to 4 h, or until the material shows a loss of not greater than
laboratory temperature, report that it has coagulated.
0.02 g on successive hourly weighings; then cool in a desic-
7. Density and Weight per Gallon cator and weigh.
7.1 Apparatus: NOTE 1—A friction-top can plug, 50 to 80 mm in diameter, has been
7.1.1 Container—Any suitable container of known volume found convenient.
may be used. 7.1.1.1 describes one such container.
7.1.1.1 Brass Cylinder, short, about 3 in. (80 mm) high and 9.2 From the weight of the dried residue and the weight of
1.5 in. (40 mm) in diameter, with the inside bottom angles the original sample, calculate the percent nonvolatile matter.
rounded is most convenient. Adjust the capacity of such a
cylinder to hold 83.3 6 0.1 g of water at 77°F (25°C). 10. Content of Volatiles and Coverage of Mastics and
7.2 Procedure—Condition the sample at 77°F (25°C) and Coatings
fill the tared container with a slight excess. In filling the 10.1 Scope—This test method covers the determination of
container, take precautions to ensure that no air is entrapped, the volume of volatile matter and the coverage per unit of dry
jarring or vibrating the container until no further change in film thickness of mastics and coatings. The volume of volatile
volume occurs is satisfactory. Remove excess with a straight- matter is expressed as the percent of the original compound.
edge flush with the top of the container and wipe the outside of The coverage is expressed in square feet per gallon of coating
the container clean. Then weigh the container and contents to as received per 0.10 in. (2.5 mm) of dried film thickness. For
within 60.5 g. supplementary procedures, refer to Test Method D 71 and
7.3 Calculations—Subtract the weight of the empty con- Section 7 of these test methods.
tainer and divide the remainder by the capacity of the container
10.2 Test Specimens—To determine the density of the cured
in cubic centimetres. The quotient is the density in grams per
film, use two or more test specimen portions at least 1 by 1 in.
cubic centimetre which, multiplied by 83.3, gives the weight
(25.4 by 25.4 mm) in area and from films of the wet thickness
per gallon in pounds.
specified by the manufacturer. Prepare and cure these films on
7.3.1 If the cylinder described in 7.1.1.1 is used, the weight
dextrin-coated paper as specified in Practice C 419, or on
of the contents in grams, divided by 10, is the weight per gallon
cellophane or other suitable sheet material that can readily be
in pounds.
removed after cure of the mastic or coating at room condition.
8. Consistency Cure the film to constant weight at 150°F (65°C) and the paper
8.1 Refer to Test Method D 217 for apparatus and general removed before determination of density in accordance with
procedure, with exceptions as noted in 8.2-8.4. Test Method D 71.
8.2 In a closed container bring to test temperature sufficient 10.3 Calculations—From values for density of the coating
material to overfill the cup of the standard grease worker. Do as received (Section 7), and of the cured film, and the weight
this either in an air bath or water bath, being careful if the latter content of solids (Section 9), calculate the volume of volatile
is used not to permit water to enter the container. Transfer the matter as follows:
material to the standard cup, occasionally jarring the cup V 5 100 2 Sv 5 100 2 Sw ~D1/Ds! (1)
sharply on a hard surface and using a spatula for filling to avoid
the inclusion of air. Scrape off the excess material extending where:
above the rim of the cup by moving the blade of the spatula, V = volume of volatile matter, %,
held inclined toward the direction of motion at an angle of 45° Sv = volume of solids, %,
across the rim of the cup. Sw = weight of solids (Section 9),
8.3 Determine the cone-penetration reading in accordance D1 = density of the coating as received, and
Ds = density of the cured film.
with Section 5 of Test Method D 217, with minimum time

2
 C 461 – 81 (2003)
10.3.1 Knowing the percent volume of volatile matter, V, set-to-touch, and at 30-min intervals to determine the time to
calculate the coverage, expressed in square feet per gallon of reach practical hardness. The film is considered to have
coating as received per 0.10 in. (2.5 mm) of dried film set-to-touch when a light pressure of the finger shows no
thickness as follows: material adhering to the finger. Practical hardness is that
Coverage 5 16 @1 2 ~V/100!# (2) condition when firm pressure of the film between the thumb
and the finger shows a slight tacky condition, but the film is not
ruptured and none of the coating adheres to the finger.
11. Build
11.1 Application of the material to the test panels may be in 13. Flash Point
accordance with Practice C 419, or to the thickness and by the
method to be followed in practice, such as spray, brush, or 13.1 Refer to Method B of Test Methods D 93.
trowel. The compound shall be at 77 6 5°F (25 6 3°C) unless 13.2 Alternatively, refer to Test Method D 56.
otherwise specified such as for hot spray. Apply the material to 13.3 Alternatively, refer to Test Methods D 3278.
10 by 10-in. (254 by 254-mm) smooth calcium silicate insu-
lation blocks, primed or unprimed in accordance with the 14. Precision and Bias
instructions of the manufacturer, at a temperature of 77 6 5°F.
Other insulation types may be substituted, and shall be identi- 14.1 The precision and bias of the procedures detailed in
fied in the report. Mask the panel for 1 in. (25.4 mm) along the this standard have not been determined.
edges. Immediately after application remove the masking and 14.2 The precision and bias of the test methods identified
suspend the panel in a vertical position in a room at 77 6 5°F. herein in other ASTM test methods are as specified in those test
After 1 h observe the coating for any flow, slippage, and methods.
sagging. Record the maximum movement to the nearest 1⁄32 in.
(0.8 mm). 15. Keywords
12. Drying Time 15.1 coatings; consistency; density; mastics; thermal
12.1 Test the coated panel prepared in accordance with insulation
Section 11 at 15-min intervals to determine the time required to

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