1、Designation: D 2697 03Standard Test Method forVolume Nonvolatile Matter in Clear or Pigmented Coatings1This standard is issued under the fixed designation D 2697; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last rev
2、ision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1 This test method is believed to be applicabl
3、e 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, water reducible pr
4、imer 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 stated in SI units are t
5、o 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 and health practices a
6、nd determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 1475 Test Method for Density of Liquid Coatings, Inks,and Related ProductsD 2369 Test Method for Volatile Content of CoatingsD 3925 Practice for Sampling Liquid Paints and RelatedPigme
7、nted CoatingsD 3980 Practice for Interlaboratory Testing of Paint andRelated Materials33. 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 the disk plus dried coating isdeter
8、mined 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, organic liquid such as low-solvencymin
9、eral 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 ingredients that are readily leached out o
10、f 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 particularly good forpaint films
11、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 definitelynot be used. Coatings formu
12、lated 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“theoretical” spaces between pigment particl
13、es not filled with binder,becoming partially filled with solvent during the test).NOTE 2Concentration of surfactant must be kept very low or litera-ture values for the density of the water cannot be used.NOTE 3Details of the mercury displacement techniques can be foundin the literature.53.2 From the
14、 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 coated disk is calculated.The volume
15、 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 Applications and is the direct res
16、ponsibility ofSubcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.Current edition approved Dec. 1, 2003. Published January 2004. Originallyapproved in 1968. Last previous edition approved in 1986 as D 2697 86 (1998).2For referenced ASTM standards, visit the ASTM website, www.astm.
17、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.3Withdrawn.4Bissey, J. E., Offcial Digest, Federation of Paint and Varnish Production Clubs,Vol 35, 1963, p. 1072, and Ashton,
18、 H. E., Materials Research and Standards, Vol 1,1961, p. 549.5Cole, R. J., Journal, Oil Colour Chemists Assn., Vol. 45, 1962, p. 776.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.4. Significance and Use4.1 This test method is inten
19、ded 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 covered at a specified dry film thicknessper unit volume) obtainable with different coating products.4.2 For various reasons th
20、e 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 by a solution of resin in solvent maybe the same, greater, or less than the total volume of theseparate ingredients: such c
21、ontraction 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 solvent.4.3 The spatial configuration of the pigment particles andthe degree to which the spaces between the pigment particl
22、esare 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 significantly greater thantheoretical due to the increase in unfilled voids betweenpigment particles. The use of volume nonvolatile
23、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 Disk, preferably stainless steel, 60 mm (238 in.) indiameter and 22 gage (0.65 mm) in thickness with a small holenear the c
24、ircumference. 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. The 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 o
25、f 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 of these tubesare described in the annex.5.3 Counterweight, to be placed on the balance stirrup afterhanger bow and pan are
26、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 beaker under the balance stirrupwithout jamming the pan damper in the floor of the balance. Acork or neoprene ring is suitab
27、le 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 if 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 d
28、isk 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 to the liquid will help toensure rapid and thorough wetting of the disk. Be careful thatno air bubbles form on the disk or wi
29、re. 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 subsequent weighings when the disk iscoated.6.3 Record the temperature of the liquid. Obtain the densityof the liquid at the tempera
30、ture 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 millilitres 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 a
31、t temperature of test, g/mL.7. Procedure7.1 Take a representative sample of the liquid coating inaccordance with Practice D 3925. Mix thoroughly beforetaking specimens for the individual tests.7.2 Determine the weight nonvolatile of the liquid coatingby drying1hat1106 5C in accordance with Test Meth
32、odD 2369.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 accordance with Test Method D 1475.7.4 Dip the disk in the liquid coating and allow the liquid tocome up on the wire a dis
33、tance 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 edge of the disk.NOTE 6In some cases the paint or varnish may be of such consistencythat the amount of solid matter remaini
34、ng 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 operatorto obtain a more desirable volume of solid matter. However, extra caremust be observed to prevent trapping of air at the p
35、oint 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 statement is available.7.5 When beads or drips stop forming, hang the disk in theoven for1hat110C (Note 5). Remove and cool. Weig
36、h 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. Calculations8.1 Calculate the volume of the coated disk, H, in millilitres,as follows:H 5 w32 w4!/D (2)6CRC Press, Inc.
37、, West Palm Beach, FL, 1986.D2697032where: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 Calculate the volume of the dried coating, F, in millili-tres, as follows:F 5 H 2 G (3)8.3 Calculate the volume of wet coating, V,
38、 in millilitres,from which the dried coating was obtained, as follows:V 5 w32 w1!/w 3r! (4)where:w = nonvolatile matter in1gofwetcoating, g, andr = density of liquid coating material.8.4 Calculate the percent volume nonvolatile content in aliquid coating as follows:F/V! 3 100 (5)NOTE 7The displaceme
39、nt 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 Precision (In accordance with Practice D 3980)In aninterlaboratory study of this test method in which one operatorin each of
40、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 %, thepooled within-laboratory standard deviation was found to be0.444 % with 17 degrees of freedom (DF) and the pooledbetween-labora
41、tories 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 duplicate result from one laboratory on a thirdsample. Based on these standard deviations the followingcriteria should be
42、used for judging the acceptability of resultsat the 95 % confidence level:9.1.1 RepeatabilityTwo results, each the mean of dupli-cates, obtained by the same operator on different days shouldbe considered suspect if they differ by more than 1.32 %absolute at volume nonvolatile contents of 24 to 35 %.
43、9.1.2 ReproducibilityTwo results, each the mean of dupli-cates, obtained by operators in different laboratories should beconsidered suspect if they differ by more than 3.59 % absoluteat the same levels.9.2 BiasBias cannot be determined because there are noaccepted standards for volume nonvolatile ma
44、tter of clear orpigmented coatings.10. Keywords10.1 volume nonvolatile contentANNEX(Mandatory Information)A1. Aluminum TubesA1.1 Aluminum tubes,7uncoated, plain with no cap orliner, #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 tub
45、ing. 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 and return the tube to a round condition. Remove thetube from the pipe and press 1 in. wide strip at an end of thetube
46、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 this standard. Users of this standard are expressly advised that determination of the validity of any such patent right
47、s, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for r
48、evision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing y
49、ou 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 through the ASTM website(www.astm.org).7The sole source of supply of the tubes manufactured by Teledyne known to thecommittee
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