4 the Dison en Princes or the Trae (rT Commie, Aly Designation: D7541 - 11 (Reapproved 2015) Standard Practice for Estimating Critical Surface Tensions’ “This standud is sued unde the Ged designation D7S41; he mums imnedsely follwing the designation indicts the ear of xia ain oye eve eon the ent of as sevson. A nar pence dicts he yar Of lst ape A ‘Speer pice (e) ites eal change since the ast ison 0: ap ONAL 1. Scope 1.1. This practice covers procedures for estimating values of the critica surface tension of surfaces by observing the wetting and dewetting of a series of liquids (usually organic solvents) applied to the surface in question 1.2 Another technique, measurement of the contact angles, 6, of a series of test liquids and plotting cos 0 versus surface tension (Zisman plots), provides data that allow the dotermi nation of more exact values for critical surface tension. 1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in th standard. 1.4 This standand does not purport to address all of the safety concems, if any, associated with its use. It is the responsibility of the user of this standard to establish appro priate safety and health practices and determine the applica bility of regulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards? 1D2578 Test Method for Wetting Tension of Polyethylene and Polypropylene Films 22 Nordtest Standards: NT_poly 176 Spreading Surface Tension by the Applied Droplet Method. 3. Terminology 3.1 Definitions: 3.1.1 critical surface tension, n—the surface tension of a hypothetical liquid that would just spontaneously spread if applied as a drop to the surface in question; any liguid with a Related Coatings Nate, snd Appian andi the dec esponsiy of Subctemite BDL. on Pye Proeres of Appi Pit Fin CCoreet dion approved Jane 1. 2015. Pabbed one 2015. Orsay sgproved in 2009 La preoas ein apo i 20112 DISA =. DOE 152000751- 11815, oe refececed ASTM snd, vs the ASTM website. ww sim og. oF ortat ASTM Cantor Serie a service @ arm ey Far Annual Boo of ASTM Stunden volume infomoion, refer tothe sands Dacarem Siiay fog OF the ASTM nebo "Fee Nordes stands, ee wo: nodicinaovation nets cn or coist Notes, Tekin 1, FIN-0250 Espoo, Fan surface tension lower than the critical surface tension will spread spontancously. 4. Summary of Pract 4.1 In this practice, a series of liquids of gradually increas- ing surface tension are applied to a surface in the form of drops, narrow strips, or spots. Drops may be applied using a dropper, syringe or other device capable of producing indi- vidoal drops. Liquid strips or spots are applied to the surface by swabbing with saturated cotton swabs or by another type of applicator, such as one that is similar to a marker pen. In the ‘ease of the drop, the observer determines whether the drop slays in place or spreads, Inthe case of the liquid strip or spot, the question is whether the liquid stays in place or dewets and crawls. In each case, the break point between wetting and ‘dewetting provides the ertieal surface tension 5. Significance and Use 5.1 Knowledge of the critical surface tension of substrates, primers and other coatings is useful for explaining or predict ing wetibility by paints and other coatings applied to those surrfaces. Surfaces with low critical surface tensions usually are prone to sufler defeets such as crawling, picture framing, cratering and loss of adhesion when painted. Low or irregular values, o both, often are indicative of contamination that could reduce adhesion. Surfaces with high critical surface tensions are easy to wel and usually provide an excellent platform for painting 5.2 The swab, marking pen and draw-down tests all simu Jate the application of a film 5.3 The swab and marking pen techniques are simple and rapid and are particularly useful for testing in the fleld or on curved, irregular or porous surfaces where contact angles cannot be measured. The drop test does not work well on such surfaces and the draw-down method requites a flat specimen that is relatively large 54 The estimation of critical surface tension bas been useful in characterizing surfaces before and after cleaning processes such as power washes and solvent wipes in order to ‘evaluate the efficiency of the cleaning. 5.5 One or more of these techniques could be the basis of a _go/no-go quality control test where if a certain liquid wets, the Copyright by ASTRE et (al igs reserved): Mon Aug 6 10:1708 EDT 2018 Dowalade rind by Henry Paul KV Mark Corporton)pusuan 1 License Agere, Nofarher reproductions authorize,Gp 07541 - 11 (2015) TABLE 1 Test Liquids and Their Surface Tensions ae Sarat Tension J sox Dinet formanie 382 2epetaone 376 enany2-pyroaone 390 Diet sutoxice 80 Eijne cyantystin fea Femarido seo Water me surface is acceptable for painting, but if that liquid retracts and crawls, the surface is not acceptable. 5.6 Another gofno go test is possible where the test liquid is 4 paint and the surface is a substrate, primer or basecoat. A form of this test has been used for coatings for plastics. 6. Interferences 6.1 The specimen must be clean in order for results to be ‘meaningful. The surface must not be touched or rubbed 6.2 ‘The surface tensions of tes Liquids, especially those that are mixtures, are subject to change with time. Test liquid surface tensions should be confirmed before they arc firs used, measured periodically after that and whenever change is suspected. 6.3 Test liquids may become contaminated, in which case results with them will be meaningless, Test liquid surface tensions should be confirmed before they are first used, ‘measured periodically after that and whenever contamination is, suspected, 64 High ambient temperature may cause rapid evaporation ff test Liquids and make it difficult to determine whether retraction has occurred or shrinkage is due to evaporation, 7. Apparatus 7.1 Several of one of the following types of applicators 71.1 Cotton swab (small ball of cotton atthe end of a stick). 7.1.2 Marker pen type applicator 7.1.3 Dropper or svringe. 7.1.4 Other device withthe ability to apply a drop, strip, oF spot. 7.2 Drawdown Bar—only for draw-down test. 73 Instrument or devices for measuring temperature and humidity 8, Materials 8.1 Swab, drop and draw-down tests B11 Test liquids, 8.1.1.1 The original publication on the swab test’ specified the liquids in Table | (listed along with their surface tensions). This set of liquids has a large surface tension gap between 24 and 35 dynesiem. “Hawa, CM. 1 Coat Tech, 8 (50), 57 (1972 ‘Copyright by ASTI lt legs resened Mon Aug 6101705 EDT 2018 > Dovnloadedprined by 8.1.1.2 Test Method D257S specifies mixtures of formamide and ethylene glycol monomethyl ether (both reagent grade). Mixtures can be designed so as to produce any combination of surface fension values 8.1.1.3 The drop test publications’ * specify mixtures of ethanol and water, but do ot give details of the proportions. 8.1.1.4 Nordiest Method NT poly 176" includes a table of surface tensions for ethanoliwater mixtures at 23°C, which gives values ranging from 22 to 72 mN/m in 2 mN/m intervals. 8.1.1.5 Other liguids covering a range of surface tensions could be used. If possible, highly volatile solvents should be avoided as itis difficult to tell whether they are dewetting or just evaporating. 9. Preparation of Specimens 9.1 The areas tested shall not contain visible blemishes or defects and shall not be touched with the fingets or be allowed to be contaminated in any way. 9.2 Specimens may be cleaned, bearing in mind that the surface of the specimen may be affected by the cleaning process. Any cleaning method should be chosen only after considering how the process may alter the surface. Cleaning rust be clearly indicated in the report. 10, Procedure-Cotton Swab 10.1 Beginning wit the lowest surface tension liquid in the test series, saturate the cotton ball at the end of the stick and apply three uniform strips 0.5 to 1 em wide and 2 to 5 em long (o the test specimen. 10.2 Observe whether the liguid remains as an intact film, retracts (crawls) or completely beads up. Allow 3 seconds for retraction or beading to occur. Longer times may be used, but ‘evaporation of the liquid may cause retraction that appears to be dewetting, but is not 10.3 If the liquid strip does not retract or bead up within 3 seconds, repeat the procedure on an untested section of the specimen with a clean cotton swab and the next higher surface tension liquid. Ifthe strip does retractor bead in the initial test, a lower surface tension test liquid must be found and used, 104 Each of the liquids in the series is used to test the specimen until one of them clearly retracts. There are two different conventions for determining the end point and esti- mating the critical surface tension: 10.4.1 The critical surface tension of dewetting is taken as being intermediate between the surface tension value ofthe last Tiguid that wet the surface and the first one example, if a 34 mN/m liquid wets the sp mN/m liquid does not, the critical surface tension will be considered to be approximately 35 mN/m. 10.4.2 The critical surface tension is taken as the highest surface tension liquid that just wets the surface. Using this criterion, the critical surface tension in the example in 104.1 ‘would be considered to be approximately 34 mNin, *Hamen CS. Berean Coins 94, 838 (199) ‘atsen CNC Pent and Resin Tel 27,374 (1998) Henry Pal (KV Mi Copuraon pute to License Arerent. No farther reproductions ahora.Gp 07541 11 (2015) ———— i __aa_ 22 26 30 34 38 mN/m FIG. 1 Drops of Ditlerent Surface Tension Liquids on a Low Surface Tension Surface, Left to Right: Low to High Surface Tension Lig- ids; Spreading to Beacing AL, Procedure-Marker Pen Applicator 11.1 Begin with the marker pen with the lowest tension, surface 11.2 Press the applicator tip firmly on the comer of the specimen until the tip is fully ssturated with the ink 11.3 Lightly draw the pen across the specimen in three parallel passes. One of the pen manufacturers specifies only evaluating the last pass. 11.4 If the last ink strip remains wetted for 3 seconds or ‘more, repeat steps 1.2 and 11.3 on an untested portion of the specimen with the next higher surface tension marker pen. 11.5 Continue testing until the paint strip clearly retracts. As with the cotton swab test, there are two conventions for determining the end point and estimating the critical surface tension, See 10.4.1 and 10.4.2 for details. 12, Procedure-Drop Test 12.1 Beginning with the lowest surface tension test liquid, place a small drop of the test liquid om the test specimen 12.2 Observe whether the liquid spreads. If it does, apply a drop of the next higher surface tension liquid. 123 Continue with higher and higher surface tension lig- ids until a drop does not spread. 124 See 10.4.1 and 10.4.2 for the two conventions used in ‘estimating the critical surface tension from the observations, 125 An example is shown in Fig. |. The surface has a critical surface tension between 22 and 26 dynes/em. Liquids with surface tensions equal to or higher than 26 dynesfem do not wet the surface and, therefore, retain their droplet form, 13, Procedure-Draw-Down Test 13.1 A flat specimen, preferably on the order of 20 by 25 em is placed on and clamped to a work bench or table. 13.2 Several test liquid drops are placed across the top of the specimen with space between them. The liquids should range from low to high surface tension, increasing from left to right, A draw-down bar is placed above the drops and pulled down, The resultant draw-downs are quickly examined for wetting and dewetting behavior. 13.3 As with the other methods, there should be a break point between the draw-down strips that wet and those that ddewet and retract. 14, Report 14.1 The report shall contain the following information when applicable and available. 14.1.1 Date, time, and place of the measurement, 14.1.2 Description of the test specimen, 14.1.3 Whether specimen is as-received or whether cleaning has been done. Ifthe later, then describe the cleaning process. 14.1.4 ‘Temperature and humidity in the area of the test. 14.1.5 Identification of the test and applicator that were used. 14.1.6 If the drop test is used, indicate the drop size 14.1.7 Any deviations from the method, 14.1.8 Identification of which convention was used to esti- ‘mate the critical surface tension, 14.1.9 ‘The estimated value forthe critical surface tension in mN/m. 15. Keywords 15.1 critical surface tension; dewetting; surface contamina- tion; wettability; wetting ASTM btematona takes no poston respecting te vay of ay paler hts asserted connection wh any tem mentioned ‘nas stardars Userso Wis Sandra xpress seis a lemon One vay of ary su pat gh he sk of itingoment of such hts are erate own responsi is standards sublet ores at any tne byte responabie etic commits and mus be revi evry ve years and ‘unease, eos aapproved or ren YourConements re rod othe lr ovsion the stars for aston ean {and should be astecce te ASTM rtamatonal Hesaquara’ Your coments wl eave crcl cansioraton aa mec oe ‘make your ewe kncan fo he ASTM Commitee cn Standscs, a he naese sewn Con ‘Ts standards copyghted by ASTM Intmatona 100 Bar Harbor Dive, PO Box 6709, West Conshehocken, PA 19488-2950, Lunt Sites. ahigul reprints angle er mutple copes) of Mis standard may be Wea by cotacing AST a! the above aadrecs or at 610.832.9565 (hone), 6108820665 ff, oF service acim 79 (ena), 2” Uveugh the ASTAT wobste {invasin og). 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