Astm d4541 17 602 [PDF]

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.



Designation: D4541  −  17



Standard Test Method for



Pull-Off Strength of Coatings Using Portable Adhesion Testers1 This standard is issued under the fixed designation D4541; the number immediately following the designation indicates the year of  original origin al adoption or, in the case of revis revision, ion, the year of last revision. revision. A number in paren parenthese thesess indicates the year of last reappr reapproval. oval. A superscript epsilon (´) indicates an editorial change since the last revision or reapproval.



1. Sco Scope* pe*



that co that coati ating ngss ca can n be tes teste ted d ev even en th thou ough gh on only ly on onee si side de is accessible. Measurements are limited by the strength of adhesive si ve bo bond ndss be betw twee een n th thee lo load adin ing g fix fixtu ture re an and d th thee sp speci ecime men n surface or the cohesive strengths of the glue, coating layers, and substrate.



1.1 This test method covers a procedure for evaluating evaluating the pull-offf str pull-o streng ength th (co (commo mmonly nly ref referr erred ed to as adh adhesio esion) n) of a coating coa ting sys system tem fro from m meta metall sub substr strates ates.. Pul Pull-o l-offf str streng ength th of  coatingss from concrete coating concrete is described in Test Method   D7234. D7234. This test offers two test protocols. Protocol 1 (test to fracture) determines the greatest perpendicular force (in tension) that a surface area can bear before a plug of material is detached. Protocol 2 (pass/fail) determines if the coated surface remains intact at a defined load criteria. Fracture will occur along the weakest plane within the system comprised of the test fixture, glue, coating system, system, and substr substrate, ate, and will be exposed by the fracture surface. This test method maximizes tensile stress as compared compar ed to the shear stress applied by other methods, methods, such as scratch or knife adhesion, and results may not be comparable.



1.4 Thi Thiss test can be destructiv destructivee and spot repairs repairs may be necessary. 1.5 The values stated in either SI units or inch-pound inch-pound units are to be regarded separately as standard. The values stated in each system may not be exa exact ct equ equival ivalent ents; s; ther therefo efore, re, eac each h system shall be used independently of the other. Combining values from the two systems may result in non-conformance with the standard. standard d doe doess not purport purport to add addre ress ss all of the 1.6   This standar safe sa fety ty co conc ncern erns, s, if an anyy, as asso socia ciated ted wi with th its us use. e. It is th thee responsibility of the user of this standard to establish appro priate safety, health and environmental practices and determine the applicability of regulatory limitations prior to use. 1.7   This inte interna rnatio tional nal sta standa ndard rd was dev develo eloped ped in acc accor or-dance with internationally recognized principles on standardizat iz atio ion n est estab ablis lishe hed d in th thee De Deci cisio sion n on Pr Prin incip ciples les fo forr th thee  Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical  Barriers to Trad Tradee (TBT) Committee.



NOTE   1—The 1—The pro proced cedure ure in thi thiss sta standa ndard rd was dev develo eloped ped for met metal al substrates, but may be appropriate for other rigid substrates such as plastic and wood. Factors such as loading rate and flexibility of the substrate must be addressed by the user/specifier. NOTE  2—The procedure in this standard was developed for use on flat surfaces. Depending on the radius of the surface, the results could have greater variability with lower values and averages.



1.2 Pull-o Pull-offf streng strength th measu measurements rements depend upon material material,, instrumentation and test parameters. Results obtained by each test method may give different results. Results should only be assessed for each test method and not be compared with other instruments. instru ments. There are five instrument types, identified as Test Methods B-F. It is imperative to identify the test method used when repor reporting ting results results..



2. Referenc Referenced ed Documents 2.1   ASTM Standards: 3 D2651 Guide D2651  Guide for Preparation Preparation of Metal Surfaces for Adhesive Bonding D3933 Gui Guide de for Pre Prepar paratio ation n of Alu Alumin minum um Sur Surfac faces es for Structural Structu ral Adhes Adhesives ives Bondi Bonding ng (Phos (Phosphor phoric ic Acid Anodizing) D7234 Test D7234  Test Method for Pull-Off Adhesion Strength of Coatings on Concrete Using Portable Pull-Off Adhesion Testers E691 Practic Practicee for Condu Conducting cting an Interl Interlabora aboratory tory Study to Determine the Precision of a Test Method



NOTE   3—Meth 3—Method od A, whi which ch app appear eared ed in pre previo vious us ver versio sions ns of thi thiss standard, has been eliminated as its main use is for testing on concrete substrates (see Test Method D7234 Method  D7234). ).



1.3 This test method describes describes a class of apparatus known as portable pull-off adhesion testers.2 They are capable of applying a concentric load and counter load to a single surface so



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This test method is under the jurisdiction of ASTM Committee D01 Committee  D01  on Paint and Related Coatings, Materials, and Applications and is the direct responsibility of  Subcommittee D01.46 Subcommittee  D01.46   on Industrial Protective Coatings. Current Curre nt editio edition n approv approved ed Aug. 1, 2017. Published Published Sept September ember 2017. Origin Originally ally approved in 1993. Last previous edition approved in 2009 as D4541 – 09 1. DOI: 10.1520/D4541-17. 2 The term adhesion tester may be somewhat of a misnomer, but its adoption by two manufacturers manufacturers and at least two patent patentss indica indicates tes continued usage.



3 For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [email protected]. For  Annual Book of ASTM  Standards volume information, refer to the standard’s Document Summary page on the ASTM website.



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*A Summary of Changes section appears at the end of this standard Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States



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D4541 − 17 3. Summ Summary ary of Test Test Method



5. Appar Apparatus atus



3.1 The gen genera erall pul pull-o l-offf test is per perfor formed med by sec securi uring ng a loading load ing fixt fixture ure (do (dolly lly,, stu stud) d) nor normal mal (pe (perpe rpendi ndicul cular) ar) to the surface of the coating with a glue. After the glue is cured, a testing apparatus is attached to the loading fixture and aligned to apply tension normal to the test surface. The force applied to the loading fixture is then gradually and uniformly increased and monitored until either the loading fixture is detached, or a specified load value is reached and the test terminated. The two common uses of this test are test to fracture (Protocol 1), and pass pa ss/f /fail ail tes testin ting g (P (Pro roto toco coll 2) 2).. Tes estt to fr frac actu ture re is us used ed to determine a maximum load that can be achieved when a plug of material is detached with the selected testing parameters. Pass/fail is used to verify the results of a testing procedure can meet a minimum load criterion. When the loading fixture is detached, the exposed surface represents the plane of limiting strength within the system. The nature of the plane of fracture is qua qualifi lified ed in acco accorda rdance nce wit with h the per percen centt of adh adhesiv esivee and cohesive failures, and the actual interfaces and layers involved. The reported load is computed based on the maximum indicated cate d loa load, d, the ins instru trumen mentt cali calibra bratio tion n dat data, a, and the ori origin ginal al surfac sur facee are areaa str stress essed. ed. Resu Results lts obt obtain ained ed usi using ng dif differ ferent ent test devices will vary because the results depend on instrumentation parameters. Variations in results are also expected when tests are performed under different test procedures or environmental conditions (see 4.2 4.2)).



5.1   Adhesion Tester,  commercially available, or comparable apparatus appar atus to the specific examples listed in Annex in  Annex A1 – Annex A5.. A5 5.1.1  Loading Fixtures, having a flat surface on one end that can be adhered to the coating and a means of attachment to the tester on the other end. Optimal size of the loading fixture is determined by the adhesion tester capabilities. The fixture and tester test er com combin binatio ation n sho should uld be cho chosen sen so tha thatt the exp expecte ected d maximum pull load the coating will be subjected to during the test is within the range of the tester. 5.1.2   Detaching Assembly   (adhesion tester), having a central grip for engaging the fixture. 5.1.3   Base, on the detaching assembly, or an annular bearing ring rin g if nee needed ded for uni unifor formly mly pre pressin ssing g aga agains instt the coa coatin ting g surfac sur facee aro around und the fixt fixture ure either directly directly,, or by way of an interm int ermedi ediate ate bea bearin ring g rin ring. g. A mea means ns of alig alignin ning g the bas basee is needed so that the resultant force is normal to the surface. 5.1.4 Means of moving moving the grip away from from the base to allow the loading of the fixture in as smooth and uniform a manner as possible and so that a torsion free, co-axial (opposing pull of  the grip and push of the base along the same axis) force results between betwee n them. 5.1.5   Timer, or means means of limiting limiting the loading loading rate. A timer is the minimum equipment when used by the operator along with the force indicator in  5.1.6  5.1.6.. 5.1.6   Forc Forcee Ind Indica icator tor and Cal Calibr ibrati ation on Inf Inform ormatio ation, n, for determining the actual force delivered to the loading fixture.



4. Sign Significan ificance ce and Use



5.2   Solvent,  or other means for cleaning the loading fixture surface. surfa ce. Finger prints, moisture, oxides, and dust tend to be the primary contaminants.



4.1 Th 4.1 Thee pu pullll-of offf st stre reng ngth th of a co coati ating ng is a pe perf rfor orma manc ncee proper pro perty ty that may be ref refere erence nced d in spe specific cificatio ations. ns. Thi Thiss test method serves as a means for uniformly preparing and testing coated surfaces, and evaluating and reporting the results. This test method is applicable to any portable apparatus meeting the requirements for determining the pull-off strength of a coating in this standard (see Annexes).



5.3   Sandpaper,  or other means, used to roughen the surfaces for glue application and adherence to the coating. When using sandpaper it is recommended to use 100 grit or finer. 5.4   Glue— the the material used for securing the loading fixture to the coating. Two component epoxies and cyanoacrylates are two commonly used glues. Select a glue that does not affect the coatin coa ting g pro proper perties ties,, flow thr throug ough h the coa coatin ting g or atta attack ck the coating.



4.2 Vari ariatio ations ns in res result ultss with the same coating coating are lik likely ely when an when any y pa para rame meter ter of th thee tes testt is ch chan ange ged. d. Th This is in inclu clude dess change in glue, load fixture size, substrate coating cure time, pull rate, environmental conditions, if the coating is scored, or using a different device. Therefore, when a series of results will be compared with one another or used for statistical analysis, the type of apparatus, substrate, test procedures, glue type, and if scoring is used should be the same for the pulls considered. 4 It is recommended that these parameters and the environmental conditions allowed during the test be mutually agreed upon between the interested parties.



5.5   Clamps, magnetic, mechanical, tape or similar, if needed for holding the fixture in place while the glue cures. 5.6   Cotton Swabs,  or other means for removing excess glue and defi definin ning g the adh adhere ered d are area. a. Any meth method od for removing removing excess glue that damages the surface, such as scoring (see  6.7  6.7), ), mustt gen mus genera erally lly be avo avoide ided d sin since ce ind induce uced d sur surfac facee flaw flawss may cause premature failure of the coating. 5.7   Scoring Tool,  circular hole cutter, or similar tool to score through to the substrate around the loading fixture.



4.3 The purchaser purchaser or specifier shall shall designate a specific test method procedure; B, C, D, E, or F and test Protocol; 1, or 2, when wh en ca calli lling ng ou outt th this is st stan anda dard rd.. In cas cases es wh wher eree eit eithe herr th thee Protocol or a pass/fail criterion is not designated, Protocol 1 shall be used.



6. Test Preparation Preparation 6.1 The method for selecting selecting the coating coating sites to be prepared forr te fo test stin ing g de depe pend ndss up upon on th thee ob obje ject ctiv ives es of th thee te test st an and d agree ag reemen ments ts be betwe tween en the co contr ntract acting ing par partie ties. s. Th Ther eree ar are, e, however, a few physical restrictions imposed by the general method and apparatus. The following requirements apply to all sites:



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Reference to potential variability of the adhesion test has been made in various publications, including the assessment of variability completed for the test method found in ASTM Research Report RR:D01-1147.



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D4541 − 17 6.1.1 The selected test area must must be large enough to accomaccommodate the specified number of replicate tests. The surface may have any orientation with reference to gravitational pull. Each load lo adin ing g fix fixtu ture re mu must st be se sepa para rate ted d by at le least ast th thee di dist stan ance ce needed to accomm accommodate odate the detach detaching ing apparatus. For Proto Protocol col 1 or to sta statis tistic ticall ally y ch char aract acter erize ize a te test st ar area ea,, th thre reee or mo more re replications are required. 6.1.2 The selected test areas must also have enough enough perpendicular and radial clearance to accommodate the apparatus, be flat enough to permit alignment, and be rigid enough to support the counter force. It should be noted that measurements close to an edge may not be representative of the coating as a whole.



preventt micr preven micro-c o-crac rackin king g in the coa coating ting or glu glue, e, sin since ce suc such h cracks may cause reduced values. Scored samples constitute a different test procedure, and should be clearly reported with the resu re sults lts.. Sc Scor orin ing g may be re requ quir ired ed fo forr th thic ickk-film film co coati ating ngs, s, reinfor rein forced ced coat coatings ings and elas elastome tomeric ric coa coating tings. s. Sco Scoring ring,, if  performed, can be completed before or after the load fixture is glued to the coating. When performed, scoring shall be done in a manner that ensures the cut is made normal to the coating surface, in a manner that does not twist or torque the test area or impart the loading fixture, and minimizes heat generation, edge damage, or microcracks to the coating or glue and the substr sub strate. ate. For thi thick ck coa coatin tings gs it is rec recomm ommend ended ed to coo cooll the coatin coa ting g and sub substr strate ate dur during ing the cut cuttin ting g pro proces cesss with wat water er lubrication.



6.2 Since the rigidity of the substrate substrate affects affects results of the test an test and d is not a co con ntr tro oll llab able le te test st var aria iab ble in fie field ld measurements, some knowledge of the substrate thickness and compos com positio ition n sho should uld be rep report orted ed for sub subseq sequen uentt ana analys lysis is or laboratory labora tory comparisons. comparisons. For examp example, le, steel substrate of less than 3.2 mm (1 ⁄ 8   in.) thic thickne kness ss usu usually ally red reduce ucess test res result ultss 1 compared to 6.4 mm (  ⁄ 4-in.) thick steel substrates.



NOTE  5—A template made from wood with a hole of the same size as the scoring tool drilled through it and secured to the surface may be an effective method to limit sideways movement of the scoring tool. NOTE 6—-Scoring requirements will vary depending on coating system, chemistry, and thickness. A direct comparison of the unscored result to a scored result is one method to determine if scoring should be performed. Other Oth er met method hodss for mak making ing thi thiss det determ ermina inatio tion n may be emp employ loyed ed wit with h agreem agr eement ent bet betwee ween n the pur purcha chaser ser and sel seller ler.. Sco Scorin ring g sho should uld not be considered for coatings less than 20 mils.



6.3 Subje Subject ct to the requirements requirements of  6.1,  6.1 ,  select representative test areas and clean the surfaces in a manner that will not affect integrity of the coating or leave a residue. To reduce the risk of  glue fracture affecting the test, the surface of the coating can be lightly abraded to promote adhesion of the glue to the surface. If th thee su surf rfac acee is ab abra rade ded, d, ca care re mu must st be tak taken en to pr prev even entt significant loss of coating thickness. Clean the area to remove particulates after abrading. Use of a solvent may be necessary to remove all contaminants. If a solvent is required, select one that does not compromise the integrity of the coating.



6.8 Note the appro approximate ximate temperature, temperature, relativ relativee humid humidity ity,, and other pertinent environmental conditions during the time of  test. 7. Test Procedure Procedure 7.1 Test Methods: Methods: 7.1.1   Test Method A (discontinued). Test Metho Method d B — Fixed Alignment Alignment Adhes Adhesion ion Tester  Tester  7.1.2   Test Type II: 7.1.2.1 7.1.2 .1 Opera Operate te the instru instrument ment in accordance with Annex A1. A1. 7.1.3   Test Method C — Self-Alignment Adhesion Tester  Type III: 7.1.3.1 7.1.3 .1 Opera Operate te the instru instrument ment in accordance with Annex A2. A2. 7.1.4   Test Method D — Self-Alignment Adhesion Tester  Type IV: 7.1.4.1 7.1.4 .1 Opera Operate te the instru instrument ment in accordance with Annex A3. A3. 7.1.5  Test Method E — Self-Alignment Adhesion Tester  Type V: 7.1.5.1 7.1.5 .1 Opera Operate te the instru instrument ment in accordance with Annex A4. A4. 7.1.6  Test Method F — Self-Alignment Adhesion Tester  Type VI: 7.1.6.1 7.1.6 .1 Opera Operate te the instru instrument ment in accordance with Annex A5. A5.



6.4 Clea Clean n the loading loading fixt fixture ure surface surface as ind indicat icated ed by the apparatus manufacturer. Failures at the fixture-glue interface can of ofte ten n be av avoi oide ded d by tr treat eatin ing g th thee fix fixtu ture re su surf rfac aces es in accordance with an appropriate ASTM standard practice for preparing metal surfaces for glue bonding. NOTE 4—Guides  4—Guides D2651  D2651 and  and D3933  D3933 are  are typical of well-proven methods for improving adhesive bond strengths to metal surfaces.



6.5 Prepa Prepare re the glue in accord accordance ance with the glue manufacturer’s recommendations. Apply the glue to the fixture or the surface to be tested, or both, using a method and thickness recommended by the glue manufacturer. Be certain to apply the glue across the entire fixture surface. Position the fixture on the surface to be tested. Carefully remove any excess glue from around the fixture. (Warning ( Warning—Movement, —Movement, especially twisting, can cau cause se tin tiny y bub bubble bless to coa coalesc lescee into large large hol holida idays ys tha thatt constitute stress discontinuities during testing which may lead to glue fracture.) 6.6 Based on the glue manufacturer’s recommendations and the anticipated environmental conditions, allow enough time for the glue to cure. During the glue set and early cure stage, a constant contact pressure should be maintained on the fixture. Magnet Mag netic ic or mech mechanic anical al clam clampin ping g sys system temss wor work k well well,, but systems relying on tack, such as masking tape, should be used with care to ensure that they do not relax with time and allow air to intrude between the fixture and the test area.



7.2 Select an adhesion-tester adhesion-tester with a detaching assembly assembly and loading fixture size that has a force calibration spanning the range ran ge of exp expect ected ed val values ues.. Mid Mid-ra -range nge mea measur sureme ements nts are recommended, but read the manufacturer’s operating instructions before proceeding. The adhesion tester shall be calibrated at the lesser of the manufacturer’s recommended frequency or every three years.



6.7 Whe When n sco scorin ring g aro around und the test surface surface is agr agreed eed upon between the purchaser and seller, extreme care is required to 3



D4541 − 17 7.3 If a bea bearin ring g ring or com compar parable able device device (5.1.3 ( 5.1.3)) is to be used, place it concentrically around the loading fixture on the coating surface. If shims are required when a bearing ring is employed, employ ed, place them betwee between n the tester base and bearin bearing g ring rather than on the coating surface. 7.4 7. 4 Ca Care refu fully lly co conn nnec ectt th thee ce cent ntra rall gr grip ip of th thee de detac tachi hing ng assembly to the loading fixture without bumping, bending, or otherwise prestressing the sample and connect the detaching assembly to its control mechanism, if necessary. For nonhorizontal zon tal sur surfac faces, es, it may be nec necess essary ary with som somee dev devices ices to suppor sup portt the detaching detaching assembly assembly so tha thatt its wei weight ght does not impact the loading fixture and contribute to the force exerted in the test. Follow the manufacturer’s recommendations.



FIG. 1 Specimen Description



equivalent diameter diameter of the the original original surface surface area stressed stressed d  = equivalent having hav ing uni units ts of mill millime imeters ters (in (inche ches). s). Thi Thiss is usu usually ally equal to the diameter of the loading fixture.



7.5 Ali Align gn the dev device ice acc accord ording ing to the man manufa ufactu cturer’ rer’ss instructions and set the force indicator to zero.



8.3 For tests where the load fixture becomes becomes detached from the test tested ed sur surfac face, e, vis visuall ually y esti estimate mate the per percen centt of coa coatin ting g adhesive and cohesive fracture and glue failure in accordance to their respective areas and location within the test system comprised of coating and glue layers. Glue fracture or failure is defined as a visible separation of the glue from itself, the coating or load fixture. A convenient scheme that describes the total test system is outlined in 8.3.1 in  8.3.1 through  through  8.3.3  8.3.3.. 8.3.1 8.3 .1 Des Descri cribe be the spe specime cimen n as sub substr strate ate A, upo upon n whi which ch successive succes sive coatin coating g layers B, C , D, etc., have been applied, including the glue,  Y , that secures the fixture,  Z , to the top coat (Fig. 1). 1). 8.3.2 8.3 .2 Designat Designatee coh cohesi esive ve fra fractu ctures res by the lay layers ers wit within hin which they occur as  B ,  C ,  D ,  Y , etc., and the visually estimated percent of each. 8.3.3 Design Designate ate adhesive fractures fractures and glue failure by the interfaces at which they occur as  A/B ,  B/C ,  C/D ,  Y/Z , etc., and the visually estimated percent of each.



NOTE  7—Pr  7—Prope operr ali alignm gnment ent is crit critica ical. l. If alig alignm nment ent of the dev device ice is required, use the procedure recommended required, recommended by the manufacturer manufacturer of the adhesion tester and report the procedure used.



7.6 Incre Increase ase the load to the fixture in as smooth smooth,, consistent, consistent, and uniform a manner and rate as possible. The rate of pull shall be 1 MPa/s (150 psi/s) or less. The rate should be set so that the test is completed in less than 100 seconds. If multiple tests are required, the rate of pull shall be similar for each test. NOTE 8—A change in load fixture fixture size may result in a change in the rate of pull depending on the equipment used. A change in rate of pull or load fixture size will result in variation of results.



7.7 The test is completed when the fixture fixture is detached from the sub substr strate, ate, pass/fail pass/fail test criteria criteria is met or max maximu imum m pul pulll strength for the instrument is reached. For pass/fail tests, the test may be terminated at any point after the test criterion has been reached.



8.4 A result that appears to be significantly significantly different different from other results (see repeatability limits in 10.1.1 in 10.1.1)) may be caused by a mist mistake ake in test pro proced cedure ure per perfor forman mance, ce, rec record ording ing or calculating. If any of these are not the cause, then examine the experimental exper imental circumstances circumstances surro surroundin unding g this run. If an irregu irregu-lar result can be attributed to an experimental cause, drop this result res ult fro from m the analysis. analysis. How Howeve everr, do not discard discard a res result ult unless unl ess ther theree are val valid id non nonstat statisti istical cal rea reason sonss for doing so or unless unl ess the res result ult is a stat statisti istical cal out outlier lier.. Valid non nonstat statisti istical cal reasons for dropping results include alignment of the apparatus that is not normal to the surface, poor definition of the area stressed due to improper application of the glue, poorly defined glue lines and boundaries, holidays in the glue caused by voids or inclusions, improperly prepared surfaces, improperly scored surfaces, varying the rate of loading during the test, varying the rate of loading between tests, and sliding or twisting the fixture duri du ring ng th thee in initi itial al cu cure re.. Sc Scra ratc tche hed d or sc scor ored ed sa samp mple less ma may y contain stress concentrations leading to premature fractures.



7.8 Record informatio information n required for the Report (see Section 9). 7.9 If a plu plug g of material material is det detach ached, ed, label and store the fixture for qualification of the failed surface in accordance with 8.3.. 8.3 7.10 Rep 7.10 Report ort any dep departu artures res fro from m the pro proced cedure ure such as possible misalignment, hesitations in the force application, etc. 8. Calc Calculat ulation ion or Inter Interpre pretati tation on of Resul Results ts 8.1 If ins instru tructed cted by the ins instru trumen mentt man manufa ufactu cturer rer,, use the instrument calibration factors to convert the indicated load for each test into the actual load applied. 8.2 Eith Either er use the cali calibra bration tion chart chart sup supplie plied d by the manufacturer or compute the relative load applied to each coating sample as follows:  X  5 4 F  / π d 2



(1 )



8.5 Doc Docume ument nt any tes testt whe where re the loa load d limi limitt of the test testing ing equipment is reached.



where: greates atestt mea mean n pul pull-o l-offf load applied applied during during a pas pass/f s/fail ail  X  = gre test, or the pull-off load achieved at fracture. Both have units of MPa (psi), F  = act actual ual load load applied applied to the test surfac surfacee as det determ ermine ined d in 8.1,, and 8.1



8.6 Proto Protocol col 1 (Test to fracture) fracture) see  Fig. 2 Flow 2  Flow Chart. 8.6.1 Unless otherwise otherwise agreed to between the purchaser purchaser and selle se llerr, di disr sreg egar ard d tes testt re resu sults lts wi with th vi visu sual ally ly es estim timate ated d gl glue ue fracture greater than 1/4 of the loading area. Use caution when using data from tests that include any visible glue fracture or 4



D4541 − 17



FIG. 2 Flow Chart



where the equipment capacity is exceeded for analysis as the results may not be statistically relevant.



the te the test st pr proc oced edur uree an and d ma make ke ad adju justm stmen ents ts to re redu duce ce gl glue ue fracture or indicate the test is indeterminate. NOTE  9—Any amount of glue fracture will result in a reduction of the maximum test load measured by the testing apparatus NOTE 10—When subjected to pull-off loads, an elastomeric coating may elongate, and if the elongation or strain is sufficient, then the failure can be induced by a simulated peel type load starting at the edges of the scored sample. To reduce this effect proper scoring and test fixture alignment techniques techni ques should be emplo employed. yed. As well, low loading rates shoul should d be avoided to reduce the time the elastomeric coating is under stress. These factors do not preclude pull-off strength testing of elastomeric materials but should be noted when evaluating results.



8.7 Proto Protocol col 2 (Pass/fail (Pass/fail test), see Fig. see  Fig. 2 Flow 2  Flow Chart. 8.7.1 The test can be terminated after the minimum minimum criterion has been met. 8.7.2 8.7 .2 A test is pas passin sing g whe when n the maximum maximum load applied applied is greater than or equal to the pass/fail criteria. 8.7.3 If the maximum load is less than the pass/fail criteria, criteria, the test is either a failing test or an indeterminate test due to glue fracture. A test result is indeterminate when there is a visible amount of glue fracture (visibly detectable glue fracture is defined as glue failure of 5 % or more of the loading area) that occurred during the test and the maximum load is less than the pass/fail criteria. An indeterminate test may be redone to determine a passing or failing result. If the test is redone, and glue fracture persists at a load below the test criteria, review



9. Repor Reportt 9.1 Report the following following information: information: 9.1.1 Date, test location, testing testing agent, 9.1.2 Brief description description of the general general nature of the test, such as, field or laboratory testing, generic type of coating, etc. 5



D4541 − 17 TABLE 1 Adhesion Testing Method B, Pull-Off Strength ( psi )



9.1.3 Tempe 9.1.3 Temperat rature ure and rel relativ ativee hum humidi idity ty and any oth other er pertinent environmental conditions during the test period. 9.1.4 Descrip Description tion of the apparatus used, including: including: apparatus man manufa ufactu cturer rer and mod model el num number ber,, las lastt cali calibra bratio tion n dat date, e, loading loadin g fixture type and dimensions, dimensions, and bearin bearing g ring type and dimensions. 9.1. 9. 1.5 5 De Descr scrip iptio tion n of th thee te test st sy syste stem, m, if po poss ssib ible, le, by th thee indexing scheme outlined in 8.3 in 8.3 including:  including: product identity and generic type for each coat and any other information supplied, and the substrate identity (thickness, type, orientation, etc.). 9.1.6 Glue used and cure time before before test. 9.1.7 Method used used to secure the loading fixture during during glue cure, if any. 9.1.8 9.1 .8 Rate of pull. pull. 9.1.9 Test results. 9.1.9. 9.1 .9.1 1 Deta Detailed iled test res results ults as des descri cribed bed in in   Fig. 2, 2,   Flow Chart.



Repeatability Reproducibility Standard Standard Deviation Deviation x¯ sr sR B 1195 27 8 3 30 C 5 49 10 9 117 D 1 21 2 12 41 2 4 83 E 1 38 5 19 2 2 76   Repeatability Coating Coatin g Avera Average ge Limit x¯ r % of average B 1195 77 7 6 9. 1 C 5 49 30 5 5 5. 6 D 1 21 2 1155 9 5 .3 E 1 38 5 53 7 3 8. 8 Avg. 6 4 .7 Coating Coatin g Avera Average ge



Repeatability Limit



Reproducibility Limit



r R 7 77 92 5 305 32 6 1155 1 3 51 5 37 77 4 Reproducibility Limit R % of average 9 25 7 7 .4 326 5 9 .0 1 35 1 111.5 7 74 5 5 .9 7 6 .0



material were included in the statistical analysis. Practice E691 Practice E691 was followed for the design and analysis of the data; the details are given in Research Report No. RR:D01-1147.



NOTE   11—Whe 11—When n tes testin ting g in a spe specifi cificc loc locatio ation, n, the hig highes hestt res result ultss obtained may be the most representative. The most common errors made during the testing process lead to artificially lower results, typically not higher results. Characterizing a test area based on an apparent low or high individual result should be done with caution.



NOTE 13—The pull-off strength of two of the coatings, identified during the round robin as Coating A and Coating F, exceeded the measurement limits of the testers with the accessories available at the time of testing, and were theref therefore ore elimin eliminated ated from the statistical analysis.



9.1.9. 9.1 .9.2 2 If correctio corrections ns of the res results ults have been made, or if  certain values have been omitted such as the lowest or highest values or others, reasons for the adjustments and criteria used. 9.1.9.3 9.1.9 .3 For any test where scoring was employed, employed, indicate it by pl plac acin ing g a fo foot otno note te su supe pers rscr crip iptt be besi side de eac each h da data ta po poin intt affected and a footnote to that effect with information of the scoring apparatus used at the bottom of each page on which such data appears. Note any other deviations from the procedure. 9.1.9.4 9.1.9 .4 Note any other deviations from the procedure. procedure.



10.1.1   Repeatability— Two Two test results obtained within one laboratory shall be judged not equivalent if they differ by more than th an th thee “r ” va valu luee fo forr th that at ma mate teri rial al;; “r ” is th thee in inte terv rval al representing the critical difference between two test results for the same material, obtained by the same operator using the same equipment on the same day in the same laboratory. 10.1.1.1 10.1. 1.1 Repeatab Repeatability ility limits are listed in Tables in  Tables 1-5. 1-5. 10.1.2   Reproducibility— Two Two test results shall be judged not equivalent if they differ by more than the “ R” value for that material; materia l; “ R” is the int interv erval al rep repres resent enting ing the dif differ ferenc encee between tw een tw two o te test st re resu sults lts fo forr th thee sa same me ma mate teri rial, al, ob obta tain ined ed by different operators using different equipment in different laboratories. 10.1.2.1 10.1. 2.1 Reprod Reproducibili ucibility ty limits are listed in Tables in  Tables 1-5. 1-5. 10.1.3 10. 1.3 Any judgment judgment in acco accorda rdance nce with the these se two sta statetements would have an approximate 95 % probability of being correct.



NOTE   12—Us 12—Usee cau cautio tion n wit with h sta statis tistica ticall ana analys lysis is of dat data, a, suc such h as averaging of results, for test results that include glue failure, termination of the test, or exceeding the capacity of the test equipment. The reported load for these types of test results are not representative of the maximum load capacity of the coating tested.



10. Pre Precisi cision on and Bias5 10.1 10 .1 The pr prec ecis isio ion n of th this is te test st me meth thod od is ba base sed d on an interlabor interla borato atory ry stu study dy of Test Met Method hod D45 D4541 41 con conduc ducted ted in 6 2006, using the parameters of Test Method D4541-09. Analysts lys ts fro from m sev seven en lab labora orator tories ies test tested ed six dif differ ferent ent coa coating tingss applied to 1 ⁄ 4  in. thick hot-rolled carbon steel plates using five differ dif ferent ent adh adhesi esion on tes testers ters.. Eve Every ry “tes “testt res result ult”” rep repres resent entss an individual determination. In order to standardize and balance the data, any pull which exceeded the tester’s upper limit with the available accessories at the time of testing was eliminated from the statistical analysis. Any pull in which there was 50 % or more glue fracture was also eliminated from the statistical analysis. If four valid pulls were obtained from one operator for a given material, the fourth was eliminated and the first three valid replicate test results (from one operator) for each



10.2   Bias— At At the time of the study, there was no accepted reference material suitable for determining the bias for this test method, therefore no statement is being made. 10.3 The precision statement statement was determ determined ined through through statistical examination of 394 results, produced by analysts from seven sev en lab labora orator tories, ies, on fou fourr coa coatin tings, gs, usi using ng five dif differ ferent ent inst in stru rume ment nts. s. Di Difffe fere rent nt co coati ating ngss we were re us used ed as a me mean anss to achievee a range of pull-o achiev pull-offf streng strengths ths covering the opera operating ting range of all the instruments. 10.3.1 10.3. 1 Results obtained obtained by the same operator operator using instruments from the same Method should be considered suspect if  they differ differ in percent relative by more than the Intral Intralaborat aboratory ory values given in Table in  Table 6. 6.  Triplicate results obtained by different operators using instruments from the same Method should be considered suspect if they differ in percent relative by more than the Interlaboratory values given in  Table 6. 6.



5



Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D01-1147. Contact ASTM Customer Service at [email protected]. 6 Scotch Weld Weld 420, available from 3M, Adhesives, Coatings and Sealers Div., 3M Center, St. Paul, MN 55144, was used in the Interlaboratory Study round robin.



6



D4541 − 17 TABLE 2 Adhesion Testing Method C, Pull-Off Strength ( psi ) Repeatability Reproducibility Standard Standard Deviation Deviation x¯ sr sR B 1 9 74 26 1 32 4 C 1 2 21 13 6 54 8 D 2110 25 2 31 6 E 2012 20 23 9 35 9   Repeatability Coating Coatin g Avera Average ge Limit x¯ r % of average B 1 9 74 73 2 3 7 .1 C 1 2 21 38 2 3 1 .3 D 2110 70 6 3 3 .5 E 2 0 12 66 9 3 3 .3 Avg. 3 0 .4 Coating Coatin g Avera Average ge



Repeatability Limit



TABLE 4 Adhesion Testing Method E, Pull-Off Strength ( psi ) Repeatability Reproducibility Standard Standard Deviation Deviation x¯ sr sR B 2 21 0 17 3 2 15 C 1120 115 1 55 D 2 48 1 24 36 1 4 22 E 2 44 9 17 3 1 98   Repeatability Coating Coatin g Avera Average ge Limit x¯ r % of average B 2 21 0 48 3 2 1. 9 C 1120 32 1 2 8. 7 D 2 48 1 1011 4 0 .7 E 2 44 9 48 5 1 9. 8 Avg. 2 7 .8



Reproducibility Limit



Coating Coatin g Avera Average ge



r R 7 32 9 07 3 82 15 35 7 06 8 86 6 69 10 04 Reproducibility Limit R % of average 907 4 5 .9 15 35 1 2 5 .7 886 4 2 .0 10 04 4 9 .9 7 0. 5



TABLE 3 Adhesion Testing Method D, Pull-Off Strength ( psi ) Repeatability Reproducibility Standard Standard Deviation Deviation x¯ sr sR B 2 4 58 14 6 27 0 C 1 2 32 31 116 D 2 7 07 15 5 23 3 E 2 3 54 16 3 27 3   Repeatability Coating Coatin g Avera Average ge Limit x¯ r % of average B 2 4 58 40 8 1 6 .6 C 1 2 32 87 7 .1 D 2 7 07 43 4 1 6 .0 E 2 3 54 45 6 1 9 .4 Avg. 1 4 .8 Coating Coatin g Avera Average ge



Repeatability Limit



Repeatability Limit



Reproducibility Limit



r SR 4 83 60 1 3 21 43 3 1011 1181 4 85 55 5 Reproducibility Limit R % of average 6 01 2 7. 2 4 33 3 8. 7 1181 4 7. 6 5 55 2 2. 7 3 4. 1



TABLE 5 Adhesion Testing Method F, Pull-Off Strength ( psi ) Repeatability Reproducibility Standard Standard Deviation Deviation x¯ sr sR B 2 07 0 10 2 1 25 C 1106 60 1 08 D 2 36 8 12 4 1 60 E 2 32 7 21 7 2 37   Repeatability Coating Coatin g Avera Average ge Limit x¯ r % of average B 2 07 0 28 7 1 3. 9 C 1106 16 9 1 5. 3 D 2 36 8 34 7 1 4. 7 E 2 32 7 60 9 2 6. 2 Avg. 1 7 .5



Reproducibility Limit



Coating Coatin g Avera Average ge



r SR 4 08 7 55 87 324 4 34 6 51 4 56 7 64 Reproducibility Limit R % of average 7 55 3 0 .7 32 4 2 6. 3 6 51 2 4 .0 7 64 3 2 .5 2 8 .4



11.. Keywo 11 Keywords rds 11.1 11 .1 adhesi adhesion; on; coatings; field; metal subst substrates; rates; paint; portable; pull-off strength; tensile test



7



Repeatability Limit



Reproducibility Limit



r SR 28 7 3 51 1 69 304 34 7 4 49 60 9 6 64 Reproducibility Limit R % of average 35 1 1 7. 0 30 4 2 7. 5 44 9 1 9. 0 66 4 2 8. 5 2 3. 0



D4541 − 17 TABLE 6 Precision of Adhesion Pull-Off Measurements (averaged across coating types for each instrument) instrument) Intralaboratory M e th o d B M e th o d C M e th o d D M e th o d E M e th o d F



Maximum Recommended Difference, % 6 4 .7 3 3 .8 1 4 .8 2 7 .8 1 7 .5



Interlaboratory M e th o d B M e th o d C M e th o d D M e th o d E M e th o d F



Maximum Recommended Difference, % 7 6. 0 6 5. 9 2 8. 4 3 4. 1 2 3 .0



ANNEXES (Mandatory Information) A1. FIXED-ALIGN FIXED-ALIGNMENT MENT ADHESION ADHESION TESTER TYPE II (TEST METHOD B)



A1.1   Apparatus:



A1.2.1 A1.2 .1 Cente Centerr th thee be bear arin ing g ri ring ng on th thee co coat atin ing g su surf rface ace concentric with the loading fixture. Turn the hand wheel or nut of the tester counterclock counterclockwise, wise, lowering lowering the grip so that it slips under the head of the loading fixture.



A1.1.1 This is a fixed-alignment portable portable tester, as shown shown in 7,8 Fig. A1.1. A1.1. NOTE  A1.1—Precision data for Type II instruments shown in   Table 6 were obtained using the devices described in Fig. in Fig. A1.1. A1.1.



A1.2.2 Align or shim the three instrument swivel pads of the tripod base so that the instrument will pull perpendicularly to the surface at the bearin bearing g ring. The annular ring can be used on flexible substrates.



A1.1.2   The The test tester er is com compri prised sed of det detach achabl ablee alu alumin minum um loading fixtures having a flat conic base that is 20 mm (0.8 in.) in di diam amete eterr on on onee en end d fo forr sec secur urin ing g to th thee co coat atin ing, g, an and d a circu cir cula larr TT-bo bolt lt he head ad on th thee ot othe herr en end, d, a ce cent ntra rall gr grip ip fo for  r  engaging the loading fixture that is forced away from a tripod  base by the interaction of a hand wheel (or nut), and a coaxial bolt bo lt co conn nnect ected ed th thrrou ough gh a se seri ries es of be belle llevil ville le wa wash sher ers, s, or  springs in later models, that acts as both a torsion relief and a spring that displaces a dragging indicator with respect to a scale.



A1.2.3 Take up the slack between the various members members and slide the dragging (force) indicator located on the tester to zero. A1.2.4 A1. 2.4 Fir Firmly mly hold the ins instru trumen mentt wit with h one hand. hand. Do not allow the base to move or slide during the test. With the other hand, han d, tur turn n the hand whe wheel el clo clockw ckwise ise usi using ng as smo smooth oth and constant motion as possible. Do not jerk or exceed a stress rate of 150 psi/s (1 MPa/s) that is attained by allowing in excess of  7 s/7 MPa (7 s/1000 psi), stress. If the 14 or 28 MPa (2000 or 4000 psi) models are used, the hand wheel is replaced with a nut requiring a wrench for tightening. The wrench must be used in a plane parallel to the substrate so that the loading fixture will not be removed by a shearing force or misalignment, thus negatin neg ating g the res result ults. s. The max maximu imum m loa load d mus mustt be rea reache ched d within about 100 s.



A1.1.3 The force is indicated by measuring the maximum A1.1.3 spring displacement when loaded. Care should be taken to see that substrate bending does not influence its final position or the actual force delivered by the spring arrangement. A1.1.4 The devices are available A1.1.4 available in four ranges: ranges: From 3.5, 7.0, 14, and 28 MPa (0 to 500, 0 to 1000, 0 to 2000, and 0 to 4000 psi).



A1.2.5 The pulling A1.2.5 pulling for force ce app applied lied to the loading loading fixt fixture ure is increased to a maximum or until the system fails at its weakest locus. loc us. Upo Upon n fra fractur cture, e, the sca scale le will rise slig slightl htly y, whi while le the draggi dra gging ng ind indicat icator or reta retains ins the app appare arent nt loa load. d. The app appara aratus tus scale sca le ind indicat icates es an app approx roximat imatee loa load d dir directl ectly y in pou pounds nds per square inch, but may be compared to a calibration curve.



A1.2   Procedure: 7



The sole source of supply of the Elcometer, Model 106, adhesion tester known to the committee at this time is Elcometer Instruments, Ltd., Edge Lane, Droylston, Manchester M35 6UB, United Kingdom, England. 8 If you are aware of alternative suppliers, please provide this information to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee,1 which you may attend



A1.2.6 Record the highest highest value attained by readin reading g along the bottom of the dragging indicator.



8



D4541 − 17



(a)



(b)



FIG. A1.1 Photograph (a) and Schematic (b) of Type II, Fixed Alignment Pull-Off Tester



9



D4541 − 17



A2. SELF-ALIGNIN SELF-ALIGNING G ADHESION TESTER TESTER TYPE III (TEST METHOD C)



A2.1   Apparatus:



A2.1.5 The testers are available in three standard standard working ranges: 0 to 10 MPa (0 to 1500 psi), 0 to 15 MPa (0 to 2250 psi), 0 to 20 MPa (0 to 3000 psi). Special loading fixtures shaped to test tubular sections are available.



A2.1.1 A2.1 .1 This This is a se self lf-a -alig ligni ning ng te teste sterr, as sh show own n in   Fig. 9,8 A2.1.. A2.1 NOTE  A2.1—Precision data for Type III instruments shown in Table in  Table 6 were obtained using the devices described in Fig. in Fig. A2.1. A2.1.



A2.2   Procedure: A2.2.1 Follo Follow w the gener general al procedures procedures described in Sections 6  and  and 7  7..  Procedures specific to this instrument are described in this section section..



A2.1.2 Loa A2.1.2 Load d is app applied lied through through the center of the loading loading fixture by a hydraulic piston and pin. The diameter of the piston bore is sized so that the area of the bore is equal to the net area of the loading fixture. Therefore, the pressure reacted by the loading fixture is the same as the pressure in the bore and is transmitted directly to a pressure gauge.



A2.2.2 Inser Insertt a decreas decreased ed TFE-fluorocarb TFE-fluorocarbon on plug into the loading fixture until the tip protrudes from the surface of the loadin loa ding g fixt fixture ure.. Whe When n app applyin lying g glu gluee to the load loading ing fixt fixture ure,, avoid getting glue on the plug. Remove plug after holding the loading fixture in place for 10 s.



A2.1.3 A2.1. 3 The apparatus apparatus is comprised of: a loading fixture, fixture, 19 mm (0 (0.7 .75 5 in in.) .) ou outs tsid idee di diam amete eterr, 3 mm (0 (0.1 .125 25 in in.) .) in insi side de diameter, hydraulic piston and pin by which load is applied to the loading fixture, hose, pressure gauge, threaded plunger and handle.



A2.2.3 Ensur Ensuree that the black needle of the tester is reading zero. Connect a test loading fixture to the head and increase the pressure by turning the handle clockwise until the pin protrudes from the loading fixture. Decrease pressure to zero and remove the test loading fixture.



A2.1.4 A2. 1.4 The force is ind indicat icated ed by the max maximu imum m hyd hydrau raulic lic pressure as displayed on the gauge, since the effective areas of  the piston bore and the loading fixture are the same.



A2.2.4 Conne Connect ct the head to the loadin loading g fixture to be tested, by pu pulli lling ng ba back ck th thee sn snap ap-o -on n ri ring ng,, pu push shin ing g th thee he head ad an and d releasing the snap-on ring. Ensure the tester is held normal to the surface to be tested and that the hose is straight.



9 The sole source of supply of the Hate Mark VII adhesion tester known to the committee at this time is Hydraulic Adhesion Test Equipment, Ltd., 629 Inlet Rd., North Palm Beach, FL 33408.



A2.2.5 Incre Increase ase the pressu pressure re slowly by turnin turning g the handle clockwise until either the maximum load or fracture is reached.



10



D4541 − 17



(a)



(b)



FIG. A2.1 Photograph (a) and Schematic (b) of Type III, Self-Alignment Tester



11



D4541 − 17



A3. SELF-ALIGNME SELF-ALIGNMENT NT ADHESION TESTER TESTER TYPE IV (TEST METHOD D)



A3.1   Apparatus:



A3.2.1 Follo Follow w the gener general al procedures procedures described in Sections 6  and  and 7  7.. Procedures specific to Type IV testers are described in the following section.



A3.1.1 This is a self-al A3.1.1 self-aligning igning automated automated tester, tester, which may have a self-contained pressure source and has a control module thatt co tha cont ntro rols ls a ch choi oice ce of dif diffe fere rent nt lo load ad ra rang ngee de detac tachi hing ng assemblies, or pistons. It is shown in  Fig. A3.1. A3.1.



A3.2.2 Adher Adheree a loadin loading g fixture to the coating based on the epoxy manufacturer’s instructions, employing either a cut-off  ring or glue mask to reproducibly define the area being tested. On lar larger ger size sized d loa loadin ding g fixt fixture ures, s, simp simply ly wip wipee awa away y exc excess ess epoxy with a cotton tipped applicator or rag.



NOTE A3.1—Precision data for Type IV instruments shown in  Table 6 were obtained using the devices described in Fig. in Fig. A3.1. A3.1.



A3.1.2 The apparatus A3.1.2 apparatus is comprised comprised of: ( 1) a loading fixture, (2) a detaching assembly, or piston, ( 3) one of several control modules, and (4) a pressurized air source.



A3.2.3 Place the piston over the loading fixture fixture and gently thread the reaction plate (top of piston) onto the loading fixture.



A3.1.3 A3.1. 3 The loading fixtures fixtures are availab available le on many different different sizes (3 to 75 mm) based on the particulars particulars of the system being tested. test ed. The sta standa ndard rd loading loading fixt fixture ure is 12. 12.5 5 mm (0. (0.5 5 in) in diameter. The face of the loading fixture can be rough, smooth, curved, machined, etc.



A3.2.4 Attach the appropriate appropriate pneumatic hoses and ensur ensuree that the control module has an air supply of at least 0.67 Mpa (100 psi) as read on the supply gauge. Zero the Piston Pressure gauge/display. A3.2.5 A3. 2.5 Ensure Ensure that the Rate Valv alvee is clo closed sed (cl (clock ockwis wisee finger tight) and then press and hold the Run button. Slowly open the Rate Valve (counterclockwise) and monitor the Piston Pressure gauge/display to obtain a rate of pressure increase of  less than 1 MPa/s (100 psi/s) yet allowing for the entire test to be complete within 100 s. When the loading fixture detaches from the surface or the required pressure is attained, release the Run button.



A3.1.4 The pis A3.1.4 piston tonss are als also o ava availab ilable le in sev severa erall dif differ ferent ent sizes, or load ranges. It is recommended that a piston is chosen so th that at th thee mi midp dpoi oint nt of th thee ra rang ngee is clo close se to th thee su susp spec ected ted tensile strength of the coating to be tested. This will provide the most forgiveness in errors of assumed coating strength. A3.1.5 Sev A3.1.5 Severa erall mod models els of con contro troll mod module uless are ava availab ilable. le. The digital models may include optional accessories allowing for features such as wireless real-time transmission of pull-tests via Bluetooth and your PC, LabVIEW-created software, USB camera attachment to photo document your pulls, and computer generated reporting capabilities.



A3.2.6 A3. 2.6 Ope Open n the Rate Valv alvee eve even n fur further ther (co (count unterc erclock lock-wise) to relieve the residual pressure so the loading fixture can be removed from the piston to prepare for the next test. A3.2.7 Record both both the maximum pressure pressure attained and the specific piston used. Convert the maximum Piston Pressure to the load applied to the coating using the conversion charts or set the specific testing parameters within the software to have this step completed automatically.



A3.1.6 A3.1 .6 The The pr press essur uriz ized ed air so sour urce ce ma may y be ( 1) a self lf-contained miniature air cylinder for maximum portability, ( 2) shop (bottled) air, or ( 3) air from an automated pump. A3.2   Procedure:



12



D4541 − 17



(a)



FIG. A3.1 Photograph Photograph (a) and Schematic of Piston (b) of Type IV Self-A Self-Alignme lignment nt Adhesion Tester Tester



13



D4541 − 17



A4. SELF-ALIGNIN SELF-ALIGNING G ADHESION TESTER TESTER TYPE V (TEST METHOD E)



A4.1   Apparatus:



A4.2   Procedure:



A4.1.1 A4.1 .1 This This is a se self lf-a -alig ligni ning ng te teste sterr, as sh show own n in   Fig. 10,8 A4.1.. A4.1



A4.2.1 Follo Follow w the gener general al procedures procedures described in Sections 6  and  and 7  7..  Procedures specific to Type V Testers are described in this section section..



NOTE  A4.1—Precision data for Type V instruments shown in Table in  Table 6 were obtained using the devices described as “Manual” in Fig. in  Fig. A4.1. A4.1.



A4.2.2 A4.2 .2 En Ensu sure re th thee pr pres essu sure re re relie lieff va valv lvee on th thee pu pump mp is completely open. Push the actuator handle completely down into the actuator assembly.



A4.1.2 A self-a A4.1.2 self-alignin ligning g spherical loading loading fixture head is used by this tester. Load evenly distributes pulling force over the surface being tested, ensuring a perpendicular, balanced pulloff. A loading fixture of 20 mm (0.78 in.) is equal to the area of the pos positio ition n bor boree in the actu actuato atorr. The Theref refore ore,, the pre pressu ssure re reacted by the loading fixture is the same as the pressure in the actuator and is transmitted directly to the pressure gauge. The tester performs automatic conversion calculations for the 50 mm (1.97 in.) loading fixtures and other common sizes of 10 and 14 mm (0.39 in. and 0.55 in. respectively).



A4.2.3 Place the actuator assembly assembly over the loading fixture head and attach the quick coupling to the loading fixture. Close the pressure relief valve on the pump. Select the appropriate loadin loa ding g fixt fixture ure size on the dis displa play y and then press the zer zero o button.



A4.1.4 A4. 1.4 The dis display play on the pre pressu ssure re gau gauge ge ind indicat icates es the maximum force and the rate of pull.



A4.2.4 Pri A4.2.4 Prime me the pump by pum pumpin ping g the handle handle unt until il the displa dis played yed rea readin ding g app approa roache chess the pri primin ming g pre pressu ssure re as explained in the instruction manual. Return the pump handle to its full upright position and then complete a single stroke at a uniform rate of no more than 1 MPa/s (150 psi/s) as shown on the display until the actuator pulls the loading fixture from the surface.



A4.1.5 The tester is available with accessories A4.1.5 accessories for finishes on plastics, metals, and wood. Special loading fixtures, typically 10 mm (0.39 in.) and 14 mm (0.55 in.) are available for use on curved surfaces and when higher pull-off pressures are required.



A4.2.5 Immed Immediately iately following following the pull, open the press pressure ure relief valve on the pump to release the pressure. The display will maintain the maximum pressure reading. Record this pull offf pre of pressu ssure re into the tes tester’ ter’ss mem memory ory and mar mark k the loa loadin ding g fixture for future qualitative analysis.



A4.1.3 A4.1. 3 The apparatus apparatus is comprised of: a loading fixture, fixture, 10 to 50 mm (0.39 and 1.97 in. respectively) diameter, hydraulic actuator by which the load is applied to the loading fixture, pressure gauge with LCD display, and hydraulic pump.



A4.2.6 A versio version n of this tester is available available with an automatic automatic hydraulic pump.



10 The sole sou source rce of sup supply ply of the Pos PosiT iTest est Pull-Off Pull-Off Tester Tester kno known wn to the committee at this time is DeFelsko Corporation, 802 Proctor Avenue, Ogdensburg, NY 13669 USA.



14



D4541 − 17



(a)



(b)



FIG. A4.1 Photograph (a) and Schematic (b) of Type V, Self-Aligning Tester



15



D4541 − 17



A5. SELF-ALIGNIN SELF-ALIGNING G ADHESION TESTER TESTER TYPE VI (TEST METHOD F)



A5.1   Apparatus: NOTE A5.1—Precision data for Type VI instruments shown in  Table 6 were obtained using the devices described in Fig. in Fig. A5.1. A5.1.



A5.2.2 Ens A5.2.2 Ensure ure that the pressure pressure in the pull mech mechani anism sm is released by opening the valve at the bottom of the cylinder. Turn Tu rn the dra draggi gging ng indicator indicator to zer zero o in lin linee wit with h the gauge indicator needle.



A5.1.2 A5. 1.2 The self self-al -align igning ing test testing ing hea head d use usess fou fourr ind indepe epenndently operated feet to ensure that the pull stress on the loading fixture is evenly distributed independently of the shape of the substrate or the angle of the loading fixture to the surface. See Fig. A5.1



A5.2.3 A5. 2.3 Att Attach ach the self self-ali -aligni gning ng test hea head d to the hyd hydrau raulic lic cable mechanism mechanism using the quick release connector on the side of the test head. Return the crank handle to the start position and ensure that the four pistons of the self-aligning head are level by pushing the head against a flat surface.



A5.1.1 A5.1. 1 This is a self-a self-alignin ligning g tester, as shown in Fig. in  Fig. A5.1. A5.1.



A5.1.3 The apparatus A5.1.3 apparatus comprises comprises a crank handle handle pull mechanism with a hydraulic cable mechanism, a self-aligning test head rated at 6.3 kN and loading fixtures.



A5.2.4 Place the rel A5.2.4 releva evant nt sup suppor portt rin ring g ove overr the loa loadin ding g fixture. fixtur e. A suppo support rt ring is not required required for 25 mm, 50 mm, or 70 mm diameter loading fixtures or for 50 mm square loading fixtures.



A5.1.4 A5.1 .4 A ra rang ngee of lo load adin ing g fix fixtu ture res, s, fr from om 2. 2.8 8 to 70 mm diameter is available. The 20 mm diameter loading fixtures are directly connected to the test head by means of a quick release connector. Other loading fixture sizes are supplied with threads machined to allow connection to the self-aligning test head using an adapter. Loading fixtures with diameters in the range 2.8 to 5.7 mm are used with a micro self-aligning test head rated at 1 kN.



A5.2.5 Attach the test head to the loading A5.2.5 loading fixt fixture ure either either directl dir ectly y or usi using ng the ada adapte pter, r, whe where re app approp ropriat riate. e. Clos Closee the valve. A5.2.6 Ens A5.2.6 Ensure ure that the hydrauli hydraulicc cab cable le mec mechan hanism ism is not pulled tight. Hold the pull mechanism in one hand and operate the crank with the other using a smooth and regular motion to ensuree that the force is applie ensur applied d evenly until the desire desired d value is reached or the fracture occurs.



A5.1.5 The force applied to the loading fixture is displayed A5.1.5 displayed on a hydraulic pressure gauge with a dragging indicator that shows the maximum reading at the point where the loading fixture is removed from the surface. The gauge carries both PSI and MPa values on two scales.



A5.2.7 Immed Immediately iately following following the comple completion tion of the pull, open the valve to release any residual pressure and return the crank handle handle to the start position. The unit is now ready for the next pull.



A5.2   Procedure:



A5.2.8 Note the value indicated by the dragg dragging ing indicator and mark the loading fixture for further analysis as described in Section 8.



A5.2.1 Follow A5.2.1 Following ing the gener general al procedures described described in Sections 6 and 7,   proced procedure uress spe specific cific to Type VI test testers ers are described in the following section.



16



D4541 − 17



(a)



(b)



FIG. A5.1 Photograph (a) and Schematic (b) of Type VI, Self-Aligning Tester



17



D4541 − 17



SUMMARY OF CHANGES Committ Comm ittee ee D0 D01 1 ha hass id iden enti tified fied th thee lo loca catio tion n of sel select ected ed ch chan ange gess to th this is st stan anda dard rd sin since ce th thee las lastt is issu suee 1 (D4541-09 ) that may impact the use of this standard. (Approved August 1, 2017.) ɛ



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