2018..2.21 Designation: D 4541 - 09 Standard Test Method for ASTM D 4541 Adoroncia Pages 1 16. Tost Version| FipHTMLS Pull-Off Strength of Coatings Using Portable Adhesion Testers" Segal aan oe ae vic, Sere int eon Amt fn es nb Yo ot a pron A Sct pt eine eel ce sc Te tee napa 1. Scope 1.1 This tet method covers a procedure for evaluating the pull-off stength (commonly referred 19 as adhesion) of a coating system from metal substrates, Pull-off sivength of coatings from concrete is described in Test Method D 7234, ‘The test determines either the greatest perpendicular force (in tension) that a surface area can bear before a plug of material is detached, or whether the surface remains intact at a pre- seribed force (passal). Failure will occur along the weakest plane within the system comprised of the test fixture, adhesive, system, and substrate, and will be exposed by the fracture surface, This test method maximizes tensile stress a6 compared tothe shear stress applied by other methods, such as scratch or knife adhesion, and results may not be comparable Nom I-—The procedure in this stindand was developed for meal subse, tu may be appt for ther rig sabes sh as pit ‘and wood Factor sucha Touding rate and Nes of the subst mst be adresse bythe wien 1.2 Pulloff strength measurements depend upon both mi- terial and instrumental parameters. Results obtained by each test method may give different results, Results should only be assessed foreach test method and not be compared with other instruments. There are five instrument types, identified as Test ‘Methods B-F. It is imperative to identify the test method used ‘when reporting results. Nove 2—Matbod A, wich appeart in previous versions of this stand has here elicited ass mai we Tor testing on come Subse (60 Tet Method D728, 1.3 This test method uses a class of apparatus known a portable pull-off adhesion testers? They are capable of apply- ing a concentric load and counter load toa single surface so that coatings can be tested even though only one side is Sibconmitce DIAG on Inds Paine Coan. ‘Comat edton sored Fob 1. M09. Pulited Api 290%, Orin apna in 198 ta preven appved 200 st DASA accessible, Measurements are limited by the strength of adhe sion bonds between the loading fixture and the specimen surface or the cobesive strengths of the adhesive, coating layers, and substrate 1.4 This test can be destructive and spot repairs may be necessary 1.5 The values stted in MPa (inch-pound) units are 40 be regarded 38 the standard. The values given in parentheses are for information only. 1.6 This standard does nor purport 20 addvess all of the safety concerns, if any, associated with its use. It is the responsibilty of the user ofthis standard to establish appro- priate safers and health practices and determine the applica- Dility of regulatory limitations prior 10 use. 2, Referenced Documents 2.1 ASTM Standards:? 2651 Guide for Preparation of Metal Surfaces for Adhe- sive Bonding 3933 Guide for Preparation of Aluminum Surfaces for ‘Structural Adhesives Bonding (Phosphoric Acid Anodiz- ing) 1D 3980 Practice for Interlaboratory Testing of Paint and Related Mateials* 7234 Test Method for Pall-OM Adhesion Strength of ‘Coatings on Concrete Using Portable Pull-O Adhesion Testers E691 Practice for Conducting an Intelaboratory Study 10 Determine the Precision of a Test Method 2.2. ANSI Standard 512. Protective Coatings (Paints) for the Nuclear Indusry* 23-180 Standard: 180 4624 Paints and Varnish—Pull-OFF Test for Adhesion’ For rfeessd ASTAC un, he ASTAC es, wast oe const ASTM Cheer Serve at sectau. Fr A Bool of ASH ‘Sumit volune nfermason fri the stds Daca Samay Re Wathdn, * ay io can Nina Sed asitne ANS, 25 WB St, Summary of Clanges section appears atthe end ofthis lander Cape (CAST nat 10 Sa er De, P.O. ED Wa nec Pe KH R84, Ud Se ‘Copyih by ASTO Int (al ight reseed, Ta Noy 12 07:44:56 EST 2009 Dowland ty http:sfiphimis. com/ipxoffendbasie 1 Lacins Keer (WEG ExuipanenosEeios S.A.) pasa License Agreement, No fre repeductions sorzed 1ne2098, 2.24 [ASTM D 4541 Adgrencia Pages 1 - 16 - Tox! Version| FipHTMLS, lp 0 4501-09 A. Summary of Test Method 3.1 The general pull-off testis performed by securing a loading fixture (dolly, stud) normal (pexpendiculae) 10 the surface of the coating with an adhesive. After the adhesive is cured, «testing apparatus is altached to the loading fixture and aligned to apply tension normal to the test surface. The foree applied to the loading fixture is then gradually increased and monitored until either a plug of material is detached, or a specified vale is reached, When a phug of material is detached, the exposed surface represents the plane of liniting strength within the system. The nature of the failure is qualified in accordance with the percent of adhesive and cohesive failures, and the actual interfaces and layers involved. The pull-off Strength is computed based on the maximum indicated load, the instrument calibration data, and the original surface ares Stressed, Pull-off strength results obtained using. different devices may be different because the results depend on instrumental parameters (see Appendix X1). 4.1 The pulloff strength of a coating is an_ important performance property that has been used in specifications. This test method Serves as a means for uniformly preparing and testing coated surfeces, and evaluating and reporting the results, Ths test method is applicable to any portable apparatus meeting the basic requirements for determining the. pull-off strength of a coating 42 Variations in results obtained using different devices or diferent subsirites with the same coating are possible (see Section 10). Therefore, it is recommended that the type of apparatus and the substrate he rmutually agreed upon between the interested parties, 43 The purchaser or specifier shall designate a specific test method, that i, B.C, D,E, or F when calling out this standard 5. Apparatus 5.1 Adhesion Tester. commercially available, or comparable apparatus. specific examples of which are listed in Al-Annex AS. 5.1.1 Loading Fixtures, having flat surface on one end ‘can be adhered to the coating and a means of attachment to the tester on the other end 5.1.2 Detaching Assembly (adhesion teste), having a een: ‘wal grip for engaging the fixture 5.13 Base, on the detaching assembly, or an annular bearing ring if needed for uniformly pressing against the coating surtace around the fixture either directly, or by way of an intermediate bearing ring. A means of aligning the base is needed so thatthe resultant force is normal to the surface, 5.14 Means of moving the grip away from the base in as smooth and continuous @ manner as possible so that a torsion free, co-axial (opposing pull of the grip and push of the base along the same axis) Ove results between them. 5.1.5 Timer, or means of limiting the loading rate to | MPa/s (150 pss) or less for 2 20 mm loading fixture so thatthe test is completed in about 100 s oF less. A timer is the minimam equipment when used by the operator along with the force indicator in 5.16 « 2 {Conrgh by ASTM lt (alight esse; Ths Nov 1207456 EST 2000 Sottaidedpaaed by ‘ 54.6 Force Indicator and Calibration Information, for detecmining the actual force delivered to the loading fixture 5.2 Solvent, or other means for cleaning the loading fixture surface, Finger prints, moisture, and oxides (end 10 be the Primary contaminants 5.3 Fine Sandpaper, or other means of cleaning the coating ‘that wil not alerts integrity by chemical or solvent attack. I any light sanding is anticipated, choose only a very fine grade abrasive (400 grit or fines) that Will ot introduce Haws or leave a residue, 54 Adhesive", for securing the fixture 10 the coating that does not alfet the coating properties, Two Component epoxies and acrylics have been found (o be the most versatile, 5.5 Magnetic or Mechanical Clamps, if needed, for holding the fixture in place while the adhesive cures, 56 Cotton Swabs, of other means for removing excess adhesive and defining the adhered area Any method for removing excess adhesive that damages the surface, such as scoring (See 6.7), must generally be avoided since induced surface Maws may cause premature failure of the coating 517 Circular Hole Cuter (optional) to score through (0 the substrate around the loading fixture, 6. Test Preparation 6.1 The method for selecting the coating sites vo be prepared for testing depends upon the objectives of the test and agreements between the contracting parties. There are, hows ever, afew physical restrictions imposed by the general method and apparatus. The following requirements apply to all sites G.1.1 The selected test area mast be a flat surface large enough to accommodate the specified number of replicate tests The surfsce may have any orientation with reference to gravitational poll. Each test site must be separated by at least the distance needed to accommodate the detaching apparatus, ‘The size ofa test site is essentially chat ofthe secured loading fixture. At least three replications are usually required in order to statistically characterize the test area. 6.1.2 The selected test areas must also have enough perpen dicular and radial clearance to accommodate the apparatus, be flatenough to permit alignment, and be rigid enough to support the counter force. It should be noted that measurements close oan edge may not be representative of the coating as a whole. 62 Since the rigidity of the substrate affects pull-of strength results and is not a controllable test variable in field ‘measurements, some knowledge of the substrate thickness and ‘composition should be reported for subsequent analysis or Iuboratory comparisons. For example, steel subsiate of less ‘than 3.2 mm (4 in.) thickness usually reduces pull-off sength results compared to 64 mam (Vein) thick steel substrates. 63 Subject to the requirements of 6.1, select representative test areas and clean the surfaces in a manner that will not affect integrity of the coating or eave a residue. To reduce the tisk of alue failures, the surface of the coating can be lightly abraded {o promote adhesion of the adhesive to the surface. I the surlace is abraded, care must be taken fo prevent damage to the * Seach Weld {20 aval rom IM, Aaesives,Ctigs an Sse Di [SM Cea, SP MN SSL, ae wo te rand an {octna Koen (WEG Equipanents trices S.A) panuan te License Ageiment. No father erodctionsaubried httpuMiphtmiS.convipxolferdbasic 262018.2.21 [ASTM D 4541 Adorencia Pages 1-16 - Tex! Version | FipHTMLS. Wp 0450109 7.1.2.1 Operate the instrument in accordance with Annes Al 7.4.3 Test Method C coating oF significant loss of coating thickness, Solvent clean the area to remove particulates after abrading. Selecta solvent that does not comprosnise the integrity of the coating. 64 Clean the loading fixture surface as indicated by the apparatus manufacturer. Failures atthe fsture-adhesive inter face can often be avoided by treating the fixture surfaces in accordance with an appropriate ASTM standard practice for preparing metal surfaces for adhesive bonding [None 3—Ciides D 2851 ott D 3938 ae typical of well ponent ‘ols for improving adbeve ad steagihs to met sles 65 Prepare the adhesive in accordance with the adhesive manufacturer's recommendations, Apply the adhesive to the fixture or the surface 10 be tested, oF oth, using method recommended by the adhesive manufacturer, Be certain (0 apply the adhesive across dhe entire surface. Position fixture on the surface to be tested. Carefully remove the excess adhesive from around the fixture. (Warning—Movement, especially twisting, can cause tiny bubbles to coalesce ino large holidays that constitute stress discontinuities during testing.) [Now 4—Aéding abou | pereat of #S gli heads 10 the adhesive sss in even alignment of he test fixture these. 66 Based on the adhesive manufacturet’s recommendations ‘and the anticipated environmental conditions, allow enough time for the adhesive to set up and reach the recommended core, During the adhesive set and early eure stage, a constant contact pressure should be maintained on the fixture, Magnetic for mechanical clamping systems work well, but systems relying on tek, such as masking tap, should be used with care fo ensure that they do not relax with time and allow air 0 intrude between the fixture and the test aea, 627 Scoring around the fixture violates the fundamental in situ test criterion that an unaltered coating be tested, If scoring around the test surface is employed, extreme care is required 10 prevent micro-cracking in the coating, since such cracks may cause reduced adbesion values. Scored samples coastitute 3 different test, and this procedure should be cleasly reported with the results. Scoring is only recommended for thicker-flm coatings, that is, thicknesses greater than 500 yim (20 mils), reinforced coatings and elastomeric coatings. Scoring, if per formed, shall be done in a manner that ensures the cutis made normal (0 the coating surface and in a manner that does not {twist or forgue the test area and minimizes heat generated and edge damage or microcracks to the coating and the substrate. FFor thick coatings itis recommended to cool the coating and substrate during the cutting process with water lubrication, Noms 5—A template male (ram plywond with aoe ofthe same size led ehrugh it has been found to be an eflcive method to init soway’s movement ofthe dil bit, 6.8 Nove the approximate temperature and relative humidity during the time of tes, 7. Test Procedure 71 Test Methods 2.4 Test Method A (discontinued) 7.12 Test Method B— Fixed Alignment Adhesion Tester Type Mt: Ms eee Th Now 12 074486 57 2009 Corsi by AST at (al Docs pnt Self Alignment Adhesion Tester Tipe Self Alignment Adhesion Tester Type rn F141 Operate the instrum re TAS Test Method E a 7.1.5.1 Operate the instrument in accordance with Annex AA, 7.16 Test Method F: vr 7.1.6.1 Operate the instrument in accordance with Annex AS. 72 Select an adhesion-tester with a detaching assembly having a force calibration spanning the range of expected values’ along with its compatible loading fixture. Mid-range measurements are usually the best, but read the manufacturer's ‘operating instructions before proceeding. 73 Ia bearing ring or comparable device (5.1.3) is to be wed, place it concentrically around the loading fixture on the coating surface. If shims are required when a bearing ring is ‘employed, place them borween the teste base and bearing ring rather than on the coating surface. 7.4 Carefully connect the central grip of the detaching assembly to the loading finture without bumping, bending, or ‘otherwise prestessing the sample and connect the detaching assembly fo its control mechanism, if necessary. For nonbori- zontal surfaces, support the detaching assembly so. that is ‘weight does not contribute to the force exerted inthe tes. 75 Align the device aeconfing 10 the manufacturer's ‘structions and set the force indicator to zero. [Nort 6—Properallanment is ria, see Appendix Xt. algnment is sequied, se the procedare recommended hy th manufetier of the eso tester and et the proce usd. 7.6 Increase the load w the fixture in as smooth and continuous 2 manner as possible, ata rate of 1 MPais (150 sis) or less for a 20 mm loading fixture so that the testis ‘completed in about 100 s oF less. 7.7 Record the force attained at force applied, 78 I? a plug of material is detached, label and store the fixture for qualification of the failed surface in accordance with 83. 79 Report any departures from the procedure such as possible misalignment, esitations in the force application, ete. Xin accordance with Annex Self Alignment Adhesion Tester Type Self Aligmnent Adhesion Tester Type re oF the maximum, 8 Calculation and Interpretation of Results 8.1 If instructed by the manufacturer, use the instrument calibration factors to convert the indicated force for each test into the actual force applied. 8.2 Either use the calibration chart supplied by the manu- facturer or compute the relative stess applied to each coating sample as follows: {Tecan Keech (WEG Equipments Blericos S.A.) punt fe License Agent No at eproduton utd ‘itp iphtmiS.convipxofferdbasic 36