1、Designation: D4497 10Standard Test Method forDetermining the Open Time of Hot Melt Adhesives (ManualMethod)1This standard is issued under the fixed designation D4497; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last
2、 revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the manual determination of theopen-time range of hot-melt adhesives under the stated condi-tions.
3、1.2 The values stated in SI units are to be regarded as thestandard. The inch-pound units in parentheses are provided forinformation only.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to
4、establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D907 Terminology of AdhesivesE177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE691 Practice for Conducting an
5、Interlaboratory Study toDetermine the Precision of a Test Method3. Terminology3.1 DefinitionsMany of the terms found in this testmethod are defined in Terminology D907.3.2 Definitions of Terms Specific to This Standard:3.2.1 open time, nthe time available between applicationof the adhesive to the fi
6、rst substrate and the mating of thesecond substrate which still results in a minimum of 50 % fibertear when tested at ambient conditions.4. Summary of Test Method4.1 In this test method, open time is determined by bondingtogether with the adhesive, pieces of standard paper at intervalsof 5 s sequent
7、ially after the molten adhesive has been appliedusing a heated film applicator on one surface. The bondedspecimens are examined later to determine the longest timeperiod, between application of the adhesive to one surface andmating with a second surface, which allows substantial bond-ing.5. Signific
8、ance and Use5.1 This test method allows comparing the open time ofseveral hot melt adhesives.5.2 This test method is not intended to provide the open-time observed for a specific adhesive in a specific manufactur-ing operation. This test method can be used to compare theperformance of adhesives whic
9、h are represented to be identicalor to rank the open-time of a group of hot melt adhesives.6. Apparatus6.1 Oven, which meets the precision required by the proce-dure, should be used to heat the adhesive sample and theapplicator.6.2 Film ApplicatorMultiple clearance 0.125 to 1.25 mm(5 to 50 mil) squa
10、re P.G. and T. Number 2 Film Applicator3capable of providing an applied film of adhesive having anominal width of 50 mm (2 in.).6.3 Hand Thermometer, preferably metal, capable of mea-suring the temperature of the hot-melt with an accuracy of61C (62F).6.4 Primary Standard Substrate, 200 by 280 mm (8
11、by 11in.), NBS Standard Reference Material 1810 (Liner Board).4Substrates are to be conditioned as described in Practice E177.6.5 Secondary Standard Substrate, 125 mm (5 in.) length inthe material direction cut to 19 mm (0.75 in.) wide, NBSStandard Reference Material 1810 (Liner Board).36.6 Glass Be
12、akers (600 mL), for melting the adhesive.6.7 Watchglass, to cover beaker.6.8 Beakers, Tongs, and Protective gloves, for handling hotvessels and applicators.6.9 Transparent Pressure Sensitive Tape.1This test method is under the jurisdiction of ASTM Committee D14 onAdhesives and is the direct responsi
13、bility of Subcommittee D14.50 on Hot MeltPressure Sensitive Archive Adhesives.Current edition approved Oct. 1, 2010. Published October 2010. Originallyapproved in 1985. Last previous edition approved in 2004 as D4497 94 (2004)1.DOI: 10.1520/D4497-10.2For referenced ASTM standards, visit the ASTM web
14、site, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3FilmApplicator No. 2 is available from Precision Gage and Tool Company, 375Gargrave Rd., Dayton, OH 45449, www
15、.precisiongage-.4Available from National Institute of Standards and Technology (NIST), 2320Measurement Services Division, Gaithersburg, MD 20899-2320, www.nist.gov.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6.10 Stop Watch or Ot
16、her Timer, graduated to at least 0.5 s.6.11 Weighted Rectangular Block, having at least onesmooth 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 measuringto the nearest 0.025 mm (1 mil).7. Sa
17、mpling7.1 The test sample should be representative of the adhesivebeing tested.8. Procedure8.1 Add 300 6 10 g of the adhesive to the 600-mL glassbeaker and cover with a watch glass. Place the beakercontaining the adhesive into the oven and heat until at theapplication temperature recommended by the
18、manufacturer.8.2 Concurrently heat the film applicator in the same ovento condition it to the sample temperature as in 8.1.8.3 Perform testing in a relatively draft-free room. While thesample is melting, prepare the substrates for testing as shownin Figs. 1 and 2.8.3.1 Tape the long sides of a piece
19、 of primary standardsubstrate (see 6.4), minimum sheet size 100 by 280 mm (4 by11 in.), to a flat smooth surface of low thermal conductivity,specifically to a larger piece of chipboard (such as from theback of a tablet). Then tape the chipboard to an underlyingsurface.8.3.2 Place the strips of the s
20、econdary standard substrate(see 6.5) across the width of the primary substrate, as shown inFig. 1, leaving approximately 6 mm (14 in.) between the strips.The top strip should be approximately 75 mm (3 in.) below thetop edge of the primary substrate. Using pressure sensitivetape, attach one end of th
21、e strips to the primary substrate. Foldthe unattached end of each strip back over the attached end sothat the primary substrate is exposed for application of theadhesive (see Fig. 2).8.4 Remove the sample from the oven, and by stirring withthe metal thermometer, quickly verify that the temperature i
22、swithin 63C (65F) of the manufacturers recommendedapplication temperature.8.5 Quickly remove the adhesive applicator from the oven,and center it above the top strip of the secondary substrate. The0.5 mm (20 mil) gap should face down and be near the top endof the primary substrate.8.6 Fill the applic
23、ator reservoir to approximately a14-in.level with conditioned hot adhesive.8.7 Move the applicator and the contained molten adhesivewith one smooth motion over the length of the paper takingapproximately2stocomplete the drawdown.NOTE 1Approximately2sissatisfactory. The purpose is to standard-ize on
24、a reasonable rate and eliminate an excessively fast or slowdrawdown which will affect the results.NOTE 2Trial applications should be made to determine the properapplicator gap to lay down a specified film thickness. Normally, a gap of0.50 mm (20 mil) will lay down a film of 0.25 mm (10 mil). Variati
25、ons inapplied film thickness will occur because of differences in the hot flowproperties of the adhesive.8.8 Immediately after the film has been drawn down, startthe timer.8.9At5sonthetimer, or a longer time if it is known thatan adhesive will have an open time longer than about 30 s, laythe top pie
26、ce of secondary substrate across the cooling film,and continue sequentially at 5 s intervals. Use the weightedblock to apply immediately a momentary load of 5 s durationto press the strips onto the adhesive, moving the block tosuccessive strips as they are laid onto the adhesive. See Fig. 3.The wood
27、 face of the block faces the substrate. Repeat thisoperation until it is obvious the adhesive film has solidified andwill not bond to the secondary substrate.8.10 Allow the adhesive film to cool at ambient temperaturefor 30 to 60 min before measuring.8.11 Measure the combined thickness of the adhesi
28、ve filmand the two substrates. Subtract the thickness of the twosubstrates to determine the nominal adhesive thickness to thenearest 0.025 mm (1 mil).8.12 With a uniform motion, peel off each strip of secondarysubstrate at an angle of 90 to the surface. Take about 10 s topeel off each strip. If the
29、paper tears near the initial edge, repeatthe peel from the opposite end of the strip. Record the percentarea of fiber tear for each strip and the time in seconds at whichthat strip was laid onto the cooling adhesive.8.13 Repeat the entire test procedure in 8.1-8.12 for a totalof three determinations
30、.FIG. 1 Secondary Substrate Strips on Primary Substrate BeforeHot Melt ApplicationFIG. 2 Strips Drawn Back to Allow Hot Melt ApplicationD4497 1029. Report9.1 Report the mean open-time of the three replicate deter-minations as the longest time, to the nearest 5 s, at which aminimum of 50 % fiber tear
31、 is obtained.9.2 Report the ambient temperature and relative humidity.9.3 Report nominal adhesive thickness, to the nearest 0.025mm (1 mil), as the mean of the three replicate determinations.9.4 Report the application temperature used (see 8.4).10. Precision and Bias10.1 The precision of this test m
32、ethod is based on aninterlaboratory study of D4447, Test Method for Determiningthe Open Time of Hot Melt Adhesives (Manual Method). Eachof six laboratories tested five different materials. Every “testresult” represents an individual determination, and all partici-pants reported triplicate test resul
33、ts. Practice E691 was fol-lowed for the design and analysis of the data; the details aregiven in ASTM Research Report RR:D141016.510.1.1 Repeatability Limit (r)Two test results obtainedwithin one laboratory shall be judged not equivalent if theydiffer by more that the “r” value for that material; “r
34、”istheinterval representing the critical difference between two testresults for the same material, obtained by the same operatorusing the same equipment on the same day in the samelaboratory.10.1.1.1 Repeatability limits are listed in Table 1.10.1.2 Reproducibility Limit (R)Two test results shall be
35、judged not equivalent if they differ by more than the “R” valuefor that material; “R” is the interval representing the criticaldifference between two test results for the same material,obtained by different operators using different equipment indifferent laboratories.10.1.2.1 Reproducibility limits
36、are listed in Table 1.10.1.3 The above terms (repeatability limit and reproduc-ibility limit) are used as specified in Practice E177.10.1.4 Any judgment in accordance with statements 10.1.1and 10.1.2 would have an approximate 95 % probability ofbeing correct.10.2 BiasAt the time of the study, there
37、was no acceptedreference material suitable for determining the bias for this testmethod, therefore no statement on bias is being made.10.3 The precision statement was determined through sta-tistical examination of 87 results, from six laboratories, on fivematerials.10.4 To judge the equivalency of t
38、wo test results, it isrecommended to choose the material in characteristics to thetest material.11. Keywords11.1 application temperature; open time5Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D14-1016.TABLE 1 Open Time (Secon
39、ds)Material AverageARepeatabilityStandardDeviationReproducibilityStandardDeviationRepeatabilityLimitReproducibilityLimitx srSRrREthylene-Vinyl Acetate 7.8 1.2 2.7 3.3 7.5Polyester 6.7 1.8 3.2 5.1 9.1Polyethylene 16.1 1.7 2.9 4.7 8.0Polyamide 17.5 2.6 5.2 7.4 14.4Polypropylene 20.8 2.0 8.4 5.7 23.5AT
40、he average of the laboratories calculated averages.FIG. 3 Strips Successively Placed onto Hot MeltD4497 103ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised th
41、at determination of the validity of any such patent rights, and the riskof 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 andif not revised, either reappr
42、oved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you f
43、eel that your comments have not received a fair hearing you shouldmake 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 re
44、prints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).D4497 104
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