1、Designation: D2697 03 (Reapproved 2014)Standard Test Method forVolume Nonvolatile Matter in Clear or Pigmented Coatings1This standard is issued under the fixed designation D2697; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the
2、year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the U.S. Department of Defense.1. Scope1.1 This test method is beli
3、eved to be applicable to thedetermination of the volume of nonvolatile matter of a varietyof coatings. An interlaboratory study to establish the precisionof this test method included a water-reducible exterior latexpaint and three automotive coatings that included a solvent-reducible primer surfacer
4、, water reducible primer surfacer,water reducible enamel topcoat, and acrylic dispersion lacquertopcoat. Earlier collaborative studies included a gloss enamel,a flat wall paint, a gloss house enamel, an industrial bakingenamel, an interior latex paint, and an exterior latex paint.1.2 The values stat
5、ed in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.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 establish appro-priate safety an
6、d health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1475 Test Method For Density of Liquid Coatings, Inks,and Related ProductsD2369 Test Method for Volatile Content of CoatingsD3925 Practice for Sampling Liquid Paints
7、 and RelatedPigmented CoatingsD3980 Practice for Interlaboratory Testing of Paint andRelated Materials (Withdrawn 1998)33. Summary of Test Method3.1 The weight and volume of a stainless steel disk is to bedetermined; after the disk is coated with the material beingtested. The weight and volume of th
8、e disk plus dried coating isdetermined by weighing in air and then by weighing in a liquidof known density. The volume being equal to the quotient ofthe weight loss of the coated disk (due to the Archimedesbuoyancy effect) divided by the density of the liquid displaced.The liquid may be water, organ
9、ic liquid such as low-solvencymineral spirits or kerosine, or with special modifications notcovered specifically in this method, mercury. The choice ofliquid depends upon the nature of the coating tested.NOTE 1Distilled water is suitable for most paints. Exceptions arecoatings that contain ingredien
10、ts that are readily leached out of the dryfilm by the water and low-gloss coatings, the surface of which is poorlywet by water even with surfactant added. (Note 2) Low-solvencyhydrocarbon solvent (KB below 36) is also practical for most paints andis preferred by some workers.4It is considered to be
11、particularly good forpaint films not readily wet by water. Analogously, organic solvents mustnot be used if the coating to be tested contains ingredients that will bedissolved readily by the solvent. Lacquers containing monomeric plasti-cizers would be examples where hydrocarbon solvents should defi
12、nitelynot be used. Coatings formulated much above the CPVC present a specialproblem, where mercury might be the desired “suspending” liquid (Note3), and for solvent-reducible paints hydrocarbon solvent might be consid-ered the poorest (unless it is the objective to obtain values closer to“theoretica
13、l” spaces between pigment particles not filled with binder,becoming partially filled with solvent during the test).NOTE 2Concentration of surfactant must be kept very low or literaturevalues for the density of the water cannot be used.NOTE 3Details of the mercury displacement techniques can be found
14、in the literature.53.2 From the measured weights and volumes of the diskbefore and after coating, the weight and volume of the driedcoating film are calculated. Based on the density of the liquidcoating and the weight percent nonvolatile matter, the volumeof the liquid coating deposited on the coate
15、d disk is calculated.The volume of the dried coating divided by the volume ofliquid coating, multiplied by 100, provides the volume percentnonvolatile matter in the total liquid coating.1This test method is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings, Materials, and App
16、lications and is the direct responsibility ofSubcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.Current edition approved July 1, 2014. Published July 2014. Originally approvedin 1968. Last previous edition approved in 2008 as D2697 03 (2008). DOI:10.1520/D2697-03R14.2For referenc
17、ed ASTM standards, visit the ASTM website, 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.3The last approved version of this historical standard is referenced onwww
18、.astm.org.4Bissey, J. E., Offcial Digest, Federation of Paint and Varnish Production Clubs,Vol 35, 1963, p. 1072, and Ashton, H. E., Materials Research and Standards, Vol 1,1961, p. 549.5Cole, R. J., Journal, Oil Colour Chemists Assn., Vol. 45, 1962, p. 776.Copyright ASTM International, 100 Barr Har
19、bor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States14. Significance and Use4.1 This test method is intended to provide a measure of thevolume of dry coating obtainable from a given volume ofliquid coating. This value is useful for comparing the coverage(square feet of surface cov
20、ered at a specified dry film thicknessper unit volume) obtainable with different coating products.4.2 For various reasons the value obtained may not be equalto that predicted from simple additivity of the weights andvolumes of the raw materials in a formulation. One reason isthat the volume occupied
21、 by a solution of resin in solvent maybe the same, greater, or less than the total volume of theseparate ingredients: such contraction or expansion in resinsolutions is governed by a number of factors, one of which isthe extent and direction of spread between solubility param-eters of the resin and
22、solvent.4.3 The spatial configuration of the pigment particles andthe degree to which the spaces between the pigment particlesare filled with the binder also affect the volume of a dry coatingformulation. Above the critical pigment volume concentration,the apparent volume of the dry film is signific
23、antly greater thantheoretical due to the increase in unfilled voids betweenpigment particles. The use of volume nonvolatile matter valuesin such instances should be carefully considered as the in-creased volume is largely due to air trapped in these voids.5. Apparatus5.1 Analytical Balance.5.2 Steel
24、 Disk, preferably stainless steel, 60 mm (238 in.) indiameter and 22 gage (0.65 mm) in thickness with a small holenear the circumference. A fine wire, such as Chromel A, 28gage (0.32 mm), is attached through the hole and made theappropriate length for subsequent suspension of the disk in aliquid. Th
25、e wire should have a small loop on the upper end sothe disk and wire can be hung by this loop on the balance.NOTE 4Instead of steel disks, some analysts use aluminum tubes. Inthe round-robin results, essentially no difference was found in theprecision obtained by both methods. Source and dimensions
26、of these tubesare described in the annex.5.3 Counterweight, to be placed on the balance stirrup afterhanger bow and pan are removed.5.4 Beaker, 1-LFor easier manipulation during the weigh-ing of disk in liquid it is advisable to cut the beaker to a heightof115mm(412 in.).5.5 Support for holding the
27、beaker under the balance stirrupwithout jamming the pan damper in the floor of the balance. Acork or neoprene ring is suitable when a single-pan balance isused.5.6 Weight per Gallon Cup, acrometer, or other suitablemeans for determining the density of the coating material andthe suspending liquids i
28、f not known.6. Volume Determination of Uncoated Disks6.1 Dry the disk in an oven at 110 6 5C for 10 min. Cooland weigh the disk in air.6.2 Weigh the disk in the liquid to be used for suspension ofthe coated disk. If water is used as the suspending liquid, a fewdrops of wetting agent (Note 2) added t
29、o the liquid will help toensure rapid and thorough wetting of the disk. Be careful thatno air bubbles form on the disk or wire. Mark the level ofliquid in the 1-L beaker necessary for complete immersion ofthe disk which should be at least 20 mm (34 in.) above the disk.Maintain this level in subseque
30、nt weighings when the disk iscoated.6.3 Record the temperature of the liquid. Obtain the densityof the liquid at the temperature used, from a table, such as isfound for pure water in Handbook of Chemistry and Physics,6or determine it to 0.001 g/mL.6.4 Calculate the volume of the disk, G, in millilit
31、res asfollows:G 5 w12 w2!/D (1)where:w1= weight of disk in air, gw2= weight of disk in liquid, g, andD = density of liquid at temperature of test, g/mL.7. Procedure7.1 Take a representative sample of the liquid coating inaccordance with Practice D3925. Mix thoroughly before takingspecimens for the i
32、ndividual tests.7.2 Determine the weight nonvolatile of the liquid coatingby drying1hat1106 5C in accordance with Test MethodD2369.NOTE 5If this method does not apply, then the method used should beagreed upon between producer and user.7.3 Determine to 0.001 g/mL the density of the liquidcoating in
33、accordance with Test Method D1475.7.4 Dip the disk in the liquid coating and allow the liquid tocome up on the wire a distance from 5 to 15 mm (14 to12 in.).Allow about 10 min for draining, and blot the coating materialoff the bottom edge of the disk so that beads or drops do not dryon the bottom ed
34、ge of the disk.NOTE 6In some cases the paint or varnish may be of such consistencythat the amount of solid matter remaining on the disk after drying is toosmall for an accurate volume determination. The use of a flat pan with asidewall about 10 mm in height in place of the disk enables the operatort
35、o obtain a more desirable volume of solid matter. However, extra caremust be observed to prevent trapping of air at the point where the sidewallmeets the bottom of the pan. In no case should bubbles be allowed to bepresent in cast films. This procedure has not been evaluated and noprecision statemen
36、t is available.7.5 When beads or drips stop forming, hang the disk in theoven for1hat110C (Note 5). Remove and cool. Weigh thecoated disk in air.7.6 Weigh the coated disk in the chosen medium in the samemanner as for the uncoated disk, recording the temperature ofthe liquid at the time of the test.8
37、. Calculations8.1 Calculate the volume of the coated disk, H, in millilitres,as follows:6CRC Press, Inc., West Palm Beach, FL, 1986.D2697 03 (2014)2H 5 w32 w4!/D (2)where:w3= weight of coated disk in air, g,w4= weight of coated disk in liquid, g, andD = density of liquid at temperature of test.8.2 C
38、alculate the volume of the dried coating, F,inmillilitres, as follows:F 5 H 2 G (3)8.3 Calculate the volume of wet coating, V, in millilitres,from which the dried coating was obtained, as follows:V 5 w32 w1!/w 3! (4)where:w = nonvolatile matter in1gofwetcoating, g, and = density of liquid coating ma
39、terial.8.4 Calculate the percent volume nonvolatile content in aliquid coating as follows:F/V! 3100 (5)NOTE 7The displacement liquid used should be reported with volumepercent nonvolatile results. The method of drying the films should also bestated if different from that specified.9. Precision9.1 Pr
40、ecision (In accordance with Practice D3980)In aninterlaboratory study of this test method in which one operatorin each of five laboratories analyzed in duplicate on two daysfour coatings (two solvent-reducible and two water-reducible)with nonvolatile contents ranging from 24 to 35 volume %, thepoole
41、d within-laboratory standard deviation was found to be0.444 % with 17 degrees of freedom (DF) and the pooledbetween-laboratories standard deviation 1.195 % with 16 DF,after discarding one days results from two laboratories on onesample, one days results from one laboratory on anothersample, and one
42、duplicate result from one laboratory on a thirdsample. Based on these standard deviations the followingcriteria should be used for judging the acceptability of resultsat the 95 % confidence level:9.1.1 RepeatabilityTwo results, each the mean ofduplicates, obtained by the same operator on different d
43、aysshould be considered suspect if they differ by more than 1.32 %absolute at volume nonvolatile contents of 24 to 35 %.9.1.2 ReproducibilityTwo results, each the mean ofduplicates, obtained by operators in different laboratoriesshould be considered suspect if they differ by more than 3.59 %absolute
44、 at the same levels.9.2 BiasBias cannot be determined because there are noaccepted standards for volume nonvolatile matter of clear orpigmented coatings.10. Keywords10.1 volume nonvolatile contentANNEX(Mandatory Information)A1. Aluminum TubesA1.1 Aluminum tubes,7uncoated, plain with no cap or liner,
45、#16 neck and orifice, 32 mm by 160 mm (114 by 614 in.).A1.2 Cut two 75 mm (3-in.) lengths of tube from thealuminum tubing. Make a 20 mm (34-in.) cut on the flattenedend of the tube about 6 mm (14 in.) from the end. Slip the tubeover a short length of 25 mm (1 in.) inside diameter electricalconduit a
46、nd return the tube to a round condition. Remove thetube from the pipe and press 1 in. wide strip at an end of thetube toward the center to serve as a hangar attachment.ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin t
47、his standard. Users of this standard are expressly advised that 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
48、be reviewed every five years andif not revised, either reapproved 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 there
49、sponsible technical committee, which you may attend. If you feel 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 reprints (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 thro
