Designation: D 4497 – 94 (Reapproved 1999)

Standard Test Method for

Determining the Open Time of Hot Melt Adhesives (Manual
Method)1
This standard is issued under the fixed designation D 4497; 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 specimens are examined later to determine the longest time

1.1 This test method covers the manual determination of the period, between application of the adhesive to one surface and
open-time range of hot-melt adhesives under the stated condi- mating with a second surface, which allows substantial bond-
tions. ing.
1.2 The values stated in SI units are to be regarded as the 5. Significance and Use
standard. The inch-pound units in parentheses are provided for
information only. 5.1 This test method allows comparing the open time of
1.3 This standard does not purport to address all of the several hot melt adhesives.
safety concerns, if any, associated with its use. It is the 5.2 This test method is not intended to provide the open-
responsibility of the user of this standard to establish appro- time observed for a specific adhesive in a specific manufactur-
priate safety and health practices and determine the applica- ing operation. This test method can be used to compare the
bility of regulatory limitations prior to use. performance of adhesives which are represented to be identical
or to rank the open-time of a group of hot melt adhesives.
2. Referenced Documents
6. Apparatus
2.1 ASTM Standards:
D 907 Terminology of Adhesives2 6.1 Oven, which meets the precision required by the proce-
E 171 Specification for Standard Atmospheres for Condi- dure, should be used to heat the adhesive sample and the
tioning and Testing Flexible Barrier Materials3 applicator.
E 691 Practice for Conducting an Interlaboratory Study to 6.2 Film Applicator— Multiple clearance 0.125 to 1.25 mm
Determine the Precision of a Test Method4 (5 to 50 mil) square P.G. and T. Number 2 Film Applicator5
capable of providing an applied film of adhesive having a
3. Terminology nominal width of 50 mm (2 in.).
3.1 Definitions— Several terms in this test method are 6.3 Hand Thermometer, preferably metal, capable of mea-
defined in accordance with Terminology D 907. suring the temperature of the hot-melt with an accuracy of
3.2 Definitions of Terms Specific to This Standard: 61°C (62°F).
3.2.1 open time—the time available between application of 6.4 Primary Standard Substrate, 200 by 280 mm (8 by 11
the adhesive to the first substrate and the mating of the second in.), NBS Standard Reference Material 1810 (Liner Board).6
substrate which still results in a minimum of 50 % fiber tear Substrates are to be conditioned as described in Specification
when tested at ambient conditions. E 171.
6.5 Secondary Standard Substrate, 125 mm (5 in.) length in
4. Summary of Test Method the material direction cut to 19 mm (0.75 in.) wide, NBS
4.1 In this test method, open time is determined by bonding Standard Reference Material 1810 (Liner Board).5
together with the adhesive, pieces of standard paper at intervals 6.6 Glass Beakers (600 mL), for melting the adhesive.
of 5 s sequentially after the molten adhesive has been applied 6.7 Watchglass, to cover beaker.
using a heated film applicator on one surface. The bonded 6.8 Beakers, Tongs, and Protective gloves, for handling hot
vessels and applicators.
6.9 Transparent Pressure Sensitive Tape.
1
This test method is under the jurisdiction of ASTM Committee D-14 on 6.10 Stop Watch or Other Timer, graduated to at least 0.5 s.
Adhesives and is the direct responsibility of Subcommittee D14.50 on Hot Melt and
Pressure Sensitive Adhesives.
Current edition approved Dec. 15, 1994. Published February 1995. Originally
5
published as D 4497 – 85. Last previous edition D 4497 – 89. Film Applicator No. 2 is available from Precision Gage and Tool Company, 28
2
Annual Book of ASTM Standards, Vol 15.06. Volkenand Street, Dayton, OH 45410.
3 6
Annual Book of ASTM Standards, Vol 15.09. Available from National Institute of Standards and Technology (NIST),
4
Annual Book of ASTM Standards, Vol 14.02. Gaithersburg, MD 20899.

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

1
 D 4497 – 94 (1999)
6.11 Weighted Rectangular Block, having at least one
smooth and flat wood face, 50 by 12.5 mm (2 by 0.5 in.)
weighing 100 g (3.5 oz), the mass being uniformly distributed.
6.12 Micrometer or Thickness Gage, capable of measuring
to the nearest 0.025 mm (1 mil).

7. Sampling
7.1 The test sample should be representative of the adhesive
being tested.

8. Procedure
8.1 Add 300 6 10 g of the adhesive to the 600-mL glass
beaker and cover with a watch glass. Place the beaker
containing the adhesive into the oven and heat until at the
application temperature recommended by the manufacturer.
8.2 Concurrently heat the film applicator in the same oven
to condition it to the sample temperature as in 8.1. FIG. 2 Strips Drawn Back to Allow Hot Melt Application
8.3 Perform testing in a relatively draft-free room. While the
sample is melting, prepare the substrates for testing as shown
in Figs. 1 and 2. 8.6 Fill the applicator reservoir to approximately a 1⁄4 -in.
8.3.1 Tape the long sides of a piece of primary standard level with conditioned hot adhesive.
substrate (see 6.4), minimum sheet size 100 by 280 mm (4 by 8.7 Move the applicator and the contained molten adhesive
11 in.), to a flat smooth surface of low thermal conductivity, with one smooth motion over the length of the paper taking
specifically to a larger piece of chipboard (such as from the approximately 2 s to complete the drawdown.
back of a tablet). Then tape the chipboard to an underlying
surface. NOTE 1—Approximately 2 s is satisfactory. The purpose is to standard-
ize on a reasonable rate and eliminate an excessively fast or slow
8.3.2 Place the strips of the secondary standard substrate
drawdown which will affect the results.
(see 6.5) across the width of the primary substrate, as shown in
NOTE 2—Trial applications should be made to determine the proper
Fig. 1, leaving approximately 6 mm (1⁄4 in.) between the strips. applicator gap to lay down a specified film thickness. Normally, a gap of
The top strip should be approximately 75 mm (3 in.) below the 0.50 mm (20 mil) will lay down a film of 0.25 mm (10 mil). Variations in
top edge of the primary substrate. Using pressure sensitive applied film thickness will occur because of differences in the hot flow
tape, attach one end of the strips to the primary substrate. Fold properties of the adhesive.
the unattached end of each strip back over the attached end so
8.8 Immediately after the film has been drawn down, start
that the primary substrate is exposed for application of the
the timer.
adhesive (see Fig. 2).
8.9 At 5 s on the timer, or a longer time if it is known that
8.4 Remove the sample from the oven, and by stirring with
an adhesive will have an open time longer than about 30 s, lay
the metal thermometer, quickly verify that the temperature is
the top piece of secondary substrate across the cooling film,
within6 3°C (65°F) of the manufacturers recommended
and continue sequentially at 5-s intervals. Use the weighted
application temperature.
block to apply immediately a momentary load of 5-s duration
8.5 Quickly remove the adhesive applicator from the oven,
to press the strips onto the adhesive, moving the block to
and center it above the top strip of the secondary substrate. The
successive strips as they are laid onto the adhesive. See Fig. 3.
0.5 mm (20-mil) gap should face down and be near the top end
The wood face of the block faces the substrate. Repeat this
of the primary substrate.
operation until it is obvious the adhesive film has solidified and
will not bond to the secondary substrate.
8.10 Allow the adhesive film to cool at ambient temperature
for 30 to 60 min before measuring.
8.11 Measure the combined thickness of the adhesive film
and the two substrates. Subtract the thickness of the two
substrates to determine the nominal adhesive thickness to the
nearest 0.025 mm (1 mil).
8.12 With a uniform motion, peel off each strip of secondary
substrate at an angle of 90° to the surface. Take about 10 s to
peel off each strip. If the paper tears near the initial edge, repeat
the peel from the opposite end of the strip. Record the percent
area of fiber tear for each strip and the time in seconds at which
that strip was laid onto the cooling adhesive.
FIG. 1 Secondary Substrate Strips on Primary Substrate Before 8.13 Repeat the entire test procedure in 8.1-8.12 for a total
Hot Melt Application of three determinations.

2
 D 4497 – 94 (1999)
9.2 Report the ambient temperature and relative humidity.
9.3 Report nominal adhesive thickness, to the nearest 0.025
mm (1 mil), as the mean of the three replicate determinations.
9.4 Report the application temperature used (see 8.4).

10. Precision and Bias

10.1 The precision and bias of this test method is based
upon the testing of five typical hot melt adhesives by six
laboratories. Statistical analysis of these data is tabulated in
Appendix X1.
10.2 The within-laboratory, single operator standard devia-
tion of this test method for determining the open-time of a hot
melt adhesive is equal to or less than 2.6 s. This was
determined for typical hot melt adhesives having mean open-
times by this test method of 20.8 s or less. The between-
laboratory standard deviation including within- and between-
FIG. 3 Strips Successively Placed onto Hot Melt
laboratory variability is equal to or less than 8.4 s.

9. Report 11. Keywords

9.1 Report the mean open-time of the three replicate deter-
11.1 application temperature; open time
minations as the longest time, to the nearest 5 s, at which a
minimum of 50 % fiber tear is obtained.

APPENDIX

(Nonmandatory Information)

X1. STATISTICAL ANALYSIS FOR TEST METHOD D 4497

TABLE X1.1 Hot Melt Adhesive Open Time—Basic DataA

Adhesive Type
Ethylene-Vinyl Polypropylene Polyamide
Laboratory Polyester Polyethylene
Acetate
(1) (2) (3) (1) (2) (3) (1) (2) (3) (1) (2) (3) (1) (2) (3)
1. Open Time,s 5 10 5 5 5 5 20 20 15 30 30 35 10 10 15
Temperature,° F 350 350 350 425 425 425 350 350 350 350 350 350 425 425 425
Film Thickness, mil 10 10 10 12 12 12 10 10 10 12 11 9 11 11 11
2. Open Time, s 5 5 5 40B 40B 40B 15 15 15 20 20 20 20 20 20
Temperature, °F 349 348 352 420 422 425 352 351 352 321 326 324 420 421 420
Film Thickness, mil 11 11.5 11 11 12 12.5 10 10.5 10 12.5 11 11 10 10 10
3. Open Time, s 10 10 10 5 5 5 20 20 20 30 30 30 20 20 25
Temperature, °F 350 350 350 425 425 425 350 350 350 325 325 325 425 425 425
Film Thickness, mil 8 9 9 9 9 9 9 9 8 9 9 9 9 9 9
4. Open time, s 10 10 10 10 15 10 15 15 15 20 15 15 15 20 20
Temperature, °F 350 350 350 425 425 425 350 350 350 325 325 325 425 425 425
Film Thickness, mil 10 10 10 11–12 12 11–12 9–10 10 10–11 10–11 10–11 10–11 10–11 10–11 10–11
5. Open Time, s 10 10 10 5 10 5 15 15 10 10 10 15 20 25 20
Temperature,° F 350 350 350 425 425 425 350 350 350 350 350 350 425 425 425
Film Thickness, mil 6 5 7 8 8 9 4 3 5 3 5 5 8 8 7
6. Open Time, s 5 5 5 5 5 5 15 15 15 15 15 15 10 15 10
Temperature, °F 350 350 350 425 425 425 350 350 350 350 350 350 425 425 425
Film Thickness, mil 9 9 8 12 12 13 8 9 9 10 9 10 9 9 10
A
Values reported as <5 s are entered into the statistical analysis as 0.
B
Outlier values were eliminated from statistical analysis according to Practice E 691.

3
 D 4497 – 94 (1999)
TABLE X1.2 95 % Repeatability and Reproducibility Intervals
95 % Repeatability 95 % Reproducibility
Adhesive Type Intervals Within Intervals Between
Laboratory, s Laboratories, s
Ethylene-Vinyl Acetate 3.3 7.6
Polyester 7.5 12.7
Polyethylene 4.7 8.2
Polypropylene 5.8 23.8
Polyamide 7.5 14.7

TABLE X1.3 95 % Confidence Intervals

Adhesive Type s
Ethylene-Vinyl Acetate 63.1
Polyester 66.8
Polyethylene 64.4
Polypropylene 65.3
Polyamide 66.9

TABLE X1.4 Precision Estimates of Open Time of Hot Melt

Adhesives
Mean Open
Vr, VL,
Adhesive Type Time, Sr SL SR
% %
s
Ethylene-Vinyl Acetate 7.8 1.2 2.4 15 31 2.7
Polyester 4.7 2.6 3.7 56 78 4.5
Polyethylene 16.1 1.7 2.3 10 14 2.9
Polypropylene 20.8 2.0 8.1 10 39 8.4
Polyamide 17.5 2.6 4.4 15 25 5.2
Average ... ... ... 21 38 ...

where:
Sr = estimated repeatability standard deviation within-laboratories for that
adhesive,
SL = estimated between-laboratory standard deviation for that adhesive,
Vr = estimated standard deviation within-laboratories as a percent of the
mean open time,
VL = estimated between-laboratories standard deviation as a percent of the
mean open time, and
SR = between-laboratory estimate of standard deviation including within-
and between-laboratory variability.

ASTM International 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 International 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, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or [email protected] (e-mail); or through the ASTM website
(www.astm.org).