NOTICE: This standard has either been superseded and replaced by a new version or discontinued.

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Designation: D 1693 – 00 An American National Standard

Standard Test Method for

Environmental Stress-Cracking of Ethylene Plastics1
This standard is issued under the fixed designation D 1693; 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 * 3. Terminology
1.1 This test method covers the determination of the sus- 3.1 Definitions:
ceptibility of ethylene plastics, as defined in Terminology 3.1.1 stress-crack, n—an external or internal rupture in a
D 883, to environmental stress-cracking when subjected to the plastic caused by tensile stresses less than its short-time
conditions herein specified. Under certain conditions of stressmechanical strength.
and in the presence of environments such as soaps, wetting 3.1.1.1 Discussion—The development of such cracks is
agents, oils, or detergents, ethylene plastics may exhibit frequently accelerated by the environment to which the plastic
mechanical failure by cracking. is exposed. The stresses which cause cracking may be present
1.2 The values stated in SI units are to be regarded as the internally or externally, or may be a combination of these
standard. stresses. The appearance of a network of fine cracks is called
1.3 This standard does not purport to address all of the crazing.
safety concerns, if any, associated with its use. It is the 3.1.2 stress-crack failure, n—for purposes of this test
responsibility of the user of this standard to establish appro-method, any crack visible to an observer with normal eyesight

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priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
shall be interpreted as a failure of the entire specimen (1).6
Extension of the controlled imperfection shall not be construed

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NOTE 1—There is no similar or equivalent ISO standard.
as a failure. The appearance of more than one crack in a single
specimen shall be construed as a single failure.
2. Referenced Documents 3.1.2.1 Discussion—Cracks generally develop at the con-
2.1 ASTM Standards: Document Preview
D 618 Practice for Conditioning Plastics and Electrical
trolled imperfection and run to the outer edge of the specimen
approximately at right angles to it (2). The cracks need not
Insulating Materials for Testing 2 extend completely through the specimen to constitute failure.
Cracks sometimes develop under the polymer surface, mani-
D 883 Terminology Relating to Plastics2 ASTM D1693-00
festing themselves as depressions on the surface. The time
D 1204 Test Method for Linear Dimensional Changes of
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Nonrigid Thermoplastic Sheeting or Film at Elevated when this occurs should be noted, and if the depression later
Temperature 2 develops into a crack, the time of dimpling should be consid-
D 1248 Specification for Polyethylene Plastics Molding and ered as the failure time.
Extrusion Materials2 4. Summary of Test Method
D 1928 Practice for Preparation of Compression-Molded
Polyethylene Test Sheets and Test Specimens2 4.1 Bent specimens of the plastic, each having a controlled
D 3350 Specification for Polyethylene Plastics Pipe and imperfection on one surface, are exposed to the action of a
Fittings Materials3 surface-active agent. The proportion of the total number of
D 4976 Specification for Polyethylene Plastics Molding and specimens that crack in a given time is observed.
Extrusion Materials4 5. Significance and Use
E 691 Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method5 5.1 This test method may be used for routine inspection
purposes by subjecting a required number of specimens to the
test conditions for a specified time and noting the number that
1
This test method is under the jurisdiction of ASTM Committee D-20 on Plastics fail. The cracking obtained with the test reagent is indicative of
and is the direct responsibility of Subcommittee D20.15 on Thermoplastic Materi- what may be expected from a wide variety of surface-active
als. agents, soaps, and organic substances that are not absorbed
Current edition approved Feb. 10, 2000. Published April 2000. Originally
published as D 1693 – 59 T. Last previous edition D 1693 – 99. appreciably by the polymer.
2
Annual Book of ASTM Standards, Vol 08.01.
3
Annual Book of ASTM Standards, Vol 08.02.
4 6
Annual Book of ASTM Standards, Vol 08.03. The boldface numbers in parentheses refer to the list of references at the end of
5
Annual Book of ASTM Standards, Vol 14.02. this test method.

*A Summary of Changes section appears at the end of this standard.

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

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 D 1693
5.2 Environmental stress-cracking is a property that is
highly dependent upon the nature and level of the stresses
applied and on the thermal history of the specimen (1). Under
the conditions of the test method, high local multiaxial stresses
are developed through the introduction of a controlled imper-
fection (2,3). Environmental stress-cracking has been found to
occur most readily under such conditions.
NOTE 2—Different types of polyethylene plastics as defined in Speci-
fication D 1248 are generally tested under different levels of strain and
stress. When it is expressly desired to compare the types at equal levels of
strain, the specimens for all types should be tested under Condition B,
Table 1 (4).
5.3 Information from this test method is not intended to be
used for direct application to engineering problems.
NOTE 3—Caution should be used in comparing and ranking various
ethylene plastics into distinct and separate groups by this test method (see mm in.
Section 13 and Note 12). A 3 1⁄8
As thermal history is recognized as an important variable, test results by B 18.9–19.2 0.745–0.755
this test method employing laboratory molded samples cannot necessarily C (radius) 1.5 max 1⁄16 max

be expected to show agreement with test results from samples obtained by

other means. The true performance potential of a given ethylene plastic FIG. 1 Nicking Jig
may, however, best be determined with specimens obtained from com-
mercially prepared items (5).
6.4 Test Tubes—Hard glass tubes nominally 200 mm long
6. Apparatus with an outside diameter of 32 mm.

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6.1 Blanking Die—A rectangular die or other means suit-
able for cutting specimens 38 6 2.5 mm by 13 6 0.8 mm
NOTE 4—It is recommended to mount the jig permanently to ensure the
notching consistency.

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(1.5 6 0.1 in. by 0.50 6 0.03 in.). These specimens must be NOTE 5—Hard glass (borosilicate) tubes have been found satisfactory.
cut with square edges. Beveled ends in particular are to be 6.5 Corks—No. 15.
avoided.
Document Preview
6.6 Aluminum Foil—Approximately 0.08 to 0.13 mm
6.2 Jig—A jig for making a controlled imperfection in (0.003 to 0.005 in.) thick, for wrapping.
specimens of the dimensions shown in Table 1, parallel to the 6.7 Constant-Temperature Bath—A constant-temperature
long edges of the specimen and centered on one of the broad liquid bath maintained at 50.0 6 0.5°C for Conditions A and B
faces. The jig shown in Fig. 17 shall be used. ASTM D1693-00
of Table 1 and 100.0 6 0.5°C for Condition C of Table 1.
6.3 Specimen Holders—Lengths of hard or half-hard brass 6.8 Test Tube Rack—A rack to hold test tubes immersed to
channel https://standards.iteh.ai/catalog/standards/sist/c521f485-407b-4418-ab20-432a834ebeab/astm-d1693-00
having the dimensions shown in (B) of Fig. 2 shall be reagent level.
used. The sides of the channel shall be parallel and the inside 6.9 Bending Clamp 4 —As shown in Fig. 3.
corners sharp and square. Any burrs present on the inside of the 6.10 Transfer Tool 4 —As shown in Fig. 4.
channel shall be removed. The inside width is critical (see
Dimension F in Fig. 2). 7. Reagent
7.1 The test reagent may be a surface-active agent, soap, or
any liquid organic substance that is not absorbed appreciably
7 by the polymer.8
Detail drawings of the apparatus are available from ASTM Headquarters.
Request PCN 12-416931-00, 12-416932-00, and 12-416933-00. This apparatus may NOTE 6—This is a nonylphenoxy poly(ethyleneoxy)ethanol. The re-
be purchased from Standard Scientific Supply Co., Bethlehem, PA. agent should be stored in closed metal or glass containers because it is
somewhat hygroscopic.
TABLE 1 Standard Test Conditions NOTE 7—The manufacturer has stated that this aggressive agent under-
Specimen Thickness Notch Depth goes no known degradation when used as follows: A 10 % volume
Condition
A
Bath Temperature, °C solution in water at 50°C for 1000 h of testing.
mm in. mmA in.
NOTE 8—The appearance of carbonyl bands in an Igepal Fourier
AB min 3.00 0.120 0.50 0.020 50 transform infrared (FT-IR) scan is an indication of degradation.
max 3.30 0.130 0.65 0.025
BB min 1.84 0.0725 0.30 0.012 50 8. Test Specimen
max 1.97 0.0775 0.40 0.015
C C
min 1.75 0.070 0.30 0.012 100 C
8.1 Unless otherwise specified, the test specimens shall be
max 2.00 0.080 0.40 0.015 molded in accordance with Procedure C of Practice D 1928.
A
Dimensional values are not exactly equivalent. However, for referee purposes
the metric units shall apply.
B
For referee purposes, concentration of Igepal will be 10 % volume.
8
C
At a temperature of 100°C, a full-strength reagent, rather than an aqueous For referee purposes Igepal CO-630 should be obtained from Rhone-Poulenc,
solution of a reagent, is generally used because solutions tend to change their Prospect Plains, Cranbury, NJ 08512. Use at full strength for Condition C and 10 %
compositions by water evaporation losses during the period of test. volume for Conditions A and B.

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 D 1693

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(https://standards.iteh.ai) Dimensions

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mm in.
A 38 6 2.5 1.5 6 0.1
B 13 6 0.8 0.5 6 0.03
C see Table 1
D see Table 1
E ASTM D1693-00 165 6 ⁄ 12

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F
(outside) 16 ⁄ 58

(inside) 11.75 6 0.05 0.463 6 0.002

G 10 3⁄8

H 15 37⁄64

I 2 0.081 (12 B & S)

J ten 5-mm holes ten 3⁄16-in. holes, 19⁄32-in.
15-mm centers centers

FIG. 2 Test Equipment

NOTE 9—Use no liquid release agents, waxes, polishes, etc., when 9. Conditioning
molding. However, inert materials such as polyester film, unplasticized
cellophane, polytetrafluoroethylene, and aluminum foil have been found 9.1 Unless otherwise specified, the test specimens should be
satisfactory. conditioned in accordance with Procedure A of Practice D 618.
8.2 Sheets may be examined for internal stresses by taking Do not bend the test specimens, nick, or treat them with the
specimens from random locations in the sheet and placing them reagent until immediately prior to the test. Testing should be
in a Petri dish containing 3 mm (1⁄8in.) of talc and setting the started a minimum of 40 h and a maximum of 96 h after
dish in an air oven at 130°C for Types I and II polyethylene conditioning the specimens has begun.
plastic and at 150°C for Types III and IV polyethylene plastic
for 30 minutes. If shrinkage of the specimens is less than 10 % 10. Procedure
in the lengthwise direction, the molded sheet can be considered 10.1 Select the condition desired from Table 1.
satisfactory (see also Test Method D 1204).
8.3 Cut specimens from smooth sheet pressed from granules NOTE 10—Generally, polyethylene plastics with densities between
0.910 and 0.925 are tested under Condition A. Polyethylenes with
or mill-massed material to the dimensions given in Fig. 2 (A). densities >0.925 are tested under Condition B. Condition C may be used
Use a die or other device that produces specimens with to accelerate testing for materials with extremely high ESCR values. The
clean-cut, square, unbeveled edges. The specimens should be user of this test method should refer to the material specifications such as
cut within 24 h after the sheets are prepared. D 1248, D 3350, or D 4976 for specific test conditions.

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 D 1693

FIG. 3 Bending Clamp Assembly

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NOTE 1—X 5 10.5 6 0.5 mm (0.41 6 0.02 in.)
FIG. 4 Transfer Tool Assembly
ASTM D1693-00
10.2 Give each conditioned specimen a controlled imper- NOTE 13—The notch depth correlates with the depth of blade setting,
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fection (notch) on one surface as shown in (A) of Fig. 2. Use which is measured by a depth micrometer (see 10.2). The notch depth can
a sharp blade, mounted in the jig shown in Fig. 1, for making be verified by microtoming the cross section of the specimen followed by
examining the slice under microscope. It also can be done by fracturing a
this imperfection. A depth micrometer may be used for setting notched specimen after it is cooled with liquid nitrogen then examine the
the blade in the jig so that the notch depth is controlled as fracture surface under microscope.
specified in Table 1. The difference between the height at the NOTE 14—Check notch quality for straight edge, sharp notch and free
top of the blade edge and the channel of the jig where the top of stress concentration area by examining the cross section of the
of the specimen rests when being nicked is measured to ensure specimen under microscope equipped with a polarized light.
the proper setting of the blade. 10.3 Inspect the edge of the blade for notches and burrs
NOTE 11—Where it is desired to nick specimens to a notch depth under normal vision prior to the first nicking and at least after
required by Conditions B and C in Table 1 and the available jig has been each 30 successive nicks have been performed. In no case shall
designed for nicking specimens to a notch depth required by Condition A a blade be used for more than 100 specimens. Replace the
in Table 1, brass shim stock 0.21 mm (0.008 in.) thick may be used to blade whenever there is any question of its having become dull
make the more shallow notch. Brass shim stock is cut wide enough so that or damaged.
it fits snugly inside the jig channel where the specimen rests when nicked.
10.4 Place ten specimens, with the controlled imperfection
The length of the shim should be such that it extends over the blade,
around the end of the jig, and under the end so that the jig will rest on up, in the slots provided in the bending clamp. Close the clamp
about 1 or 2 in. of the shim stock. The weight of the jig resting on the shim by means of a vise, arbor press, or other suitable aid, taking 30
stock prevents deformation of the shim stock during the nicking operation. to 35 s for the complete closing operation. Place the transfer
An oblong hole long enough to fit completely over the protruding blade is tool in position on top of the closed clamp and close it over the
cut in the other end of the shim stock. Discard shim stock that becomes specimens. Then lift the specimens from the clamp with the
wrinkled or deformed in such a way as to prevent the specimen from lying transfer tool and place them in the channel by releasing the
horizontal in the jig.
NOTE 12—In order to maintain notch consistency, it is recommended to
transfer tool. The ends of all the specimens should rest against
keep the force applied to the jig handle constant. This can be done by the base of the brass channel. If some specimens are riding too
applying the force at the same location of the jig handle each time using high in the holder they should be forced down by manual
a torque wrench. pressure.