1、Designation: D 2369 07Standard Test Method forVolatile Content of Coatings1This standard is issued under the fixed designation D 2369; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in parenthes
2、es 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 describes a procedure for the determi-nation of the wei
3、ght percent volatile content of solventborneand waterborne coatings. Test specimens are heated at 110 65C for 60 min.NOTE 1The coatings used in these round-robin studies representedair-dried, air-dried oxidizing, heat-cured baking systems, and also in-cluded multicomponent paint systems.1.2 Sixty mi
4、nutes at 110 6 5C is a general purpose testmethod based on the precision obtained with both solventborneand waterborne coatings (see Section 9).1.3 This test method is viable for coatings wherein one ormore parts may, at ambient conditions, contain liquid coreac-tants that are volatile until a chemi
5、cal reaction has occurredwith another component of the multi-package system.NOTE 2Committee D01 has run round-robin studies on volatiles ofmulticomponent paint systems. The only change in procedure is to premixthe weighed components in the correct proportions and allow thespecimens to stand at room
6、temperature for 1 h prior to placing them intothe oven.1.4 Test Method D 5095 for Determination of the Nonvola-tile Content in Silanes, Siloxanes and Silane-Siloxane BlendsUsed in Masonry Water Repellent Treatments is the standardmethod for nonvolatile content of these types of materials.1.5 Test Me
7、thods D 5403 for Volatile Content of RadiationCurable Materials is the standard method for determiningnonvolatile content of radiation curable coatings, inks andadhesives.1.6 Test Method D 6419 for Volatile Content of Sheet-Fedand Coldset Web Offset Printing Inks is the method of choicefor these typ
8、es of printing inks.1.7 This test method may not be applicable to all types ofcoatings. Other procedures may be substituted with mutualagreement between the producer and the user.NOTE 3If unusual decomposition or degradation of the specimenoccurs during heating, the actual time and temperature used
9、to cure thecoating in practice may be substituted for the time and temperaturespecified in this test method, subject to mutual agreement between theproducer and the user. The U.S. EPA Reference Method 24 specifies 1106 5C for 1 h for coatings.NOTE 4Practice D 3960 for Determining Volatile Organic Co
10、mpound(VOC) Content of Paints and Related Coatings describes procedures andcalculations and provides guidance on selecting test methods to determineVOC content of solventborne and waterborne coatings.1.8 The values stated in SI units are to be regarded as thestandard. The values given in parentheses
11、 are for informationonly.1.9 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 and determine the applica-bility of regulatory limitations pri
12、or to use.2. Referenced Documents2.1 ASTM Standards:2D 1193 Specification for Reagent WaterD 3925 Practice for Sampling Liquid Paints and RelatedPigmented CoatingsD 3960 Practice for Determining Volatile Organic Com-pound (VOC) Content of Paints and Related CoatingsD 5095 Test Method for Determinati
13、on of the NonvolatileContent in Silanes, Siloxanes and Silane-Siloxane BlendsUsed in Masonry Water Repellent TreatmentsD 5403 Test Methods for Volatile Content of RadiationCurable MaterialsD 6419 Test Method for Volatile Content of Sheet-Fed andColdset Web Offset Printing InksE 145 Specification for
14、 Gravity-Convection and Forced-Ventilation OvensE 180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty Chemicals1This test method is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings, Materials, and Applications and i
15、s the direct responsibility ofSubcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.Current edition approved July 1, 2007. Published August 2007. Originallyapproved in 1965. Last previous edition approved in 2004 as D 2369 04.2For referenced ASTM standards, visit the ASTM website, w
16、ww.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.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.2.2
17、 Other Standards:EPAReference Method 24 Determination of Volatile MatterContent, Density, Volume Solids, and Weight Solids ofSurface Coatings33. Summary of Test Method3.1 A designated quantity of coating specimen is weighedinto an aluminum foil dish containing 3 mL of an appropriatesolvent, disperse
18、d, and heated in an oven at 110 6 5C for 60min. The percent volatile is calculated from the loss in weight.4. Significance and Use4.1 This test method is the procedure of choice for deter-mining volatiles in coatings for the purpose of calculating thevolatile organic content in coatings under specif
19、ied test condi-tions. The weight percent solids content (nonvolatile matter)may be determined by difference. This information is useful tothe paint producer and user and to environmental interests fordetermining the volatiles emitted by coatings.5. Apparatus5.1 Analytical Balance, capable of weighin
20、g 60.1 mg.5.2 Aluminum Foil Dishes, 58 mm in diameter by 18 mmhigh with a smooth (planar) bottom surface. Precondition thedishes for 30 min in an oven at 110 6 5C and store in adesiccator prior to use. Use tongs or rubber gloves, or both, tohandle the dishes.5.3 Forced Draft Oven, Type IIAor Type II
21、B as specified inSpecification E 145. The oven must be operating in accordancewith Specification E 145, since it is important to have properair flow and good temperature control to ensure good precision.NOTE 5Be sure the shelves are level and dampers are open.5.4 Syringe, 1-mL without needle, but eq
22、uipped with caps,capable of properly dispensing the coating under test, at asufficient rate so that the specimen can be dissolved in thesolvent.NOTE 6Disposable syringes with caps are recommended.5.5 Paper Clips.6. Reagents6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unle
23、ss otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.4Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently
24、high purity to permit its use without lessening theaccuracy of the determination.6.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean Type II of SpecificationD 1193.6.3 Toluene, water or appropriate solvent.7. Procedure7.1 Take a representative sample of the
25、liquid coating (eachcomponent) in accordance with Practice D 3925. Mix thor-oughly by hand before taking specimens.7.2 For multi-component coatings, weigh each componentin the proper proportion into a container that can be capped.Mix the components together thoroughly by hand beforeextracting specim
26、ens. Tightly close the container to preventloss of volatile materials.7.3 Weigh the preconditioned aluminum foil dish (see 5.2)and record the weight to the nearest 0.1 mg (W1). Usedisposable (no talc) rubber or polyethylene gloves, tweezers orforceps to handle the dish.7.4 To facilitate dispersing o
27、r spreading the specimen, ametal paper clip may be placed (partially unfolded) in thealuminum dish and weighed with the dish. If a paper clip isused, it must remain with the dish throughout the remainder ofthe procedure.7.5 Add to the aluminum foil dish the appropriate type andamount of solvent acco
28、rding to Table 1.7.6 Draw the coating specimen into the syringe. Remove thesyringe from the specimen and then pull the plunger tip up 6mm (14 in.) in order to pull the specimen away from the neckof the syringe. Wipe the outer surface of the syringe to remove3Available from U.S. Government Printing O
29、ffice Superintendent of Documents,732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http:/www.access.gpo.gov.4Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemic
30、al Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.TABLE 1 Summary of MethodsCoating TypeMethod A One ComponentWaterborneMethod B One ComponentSolv
31、entborneMethod C Mulit-ComponentWaterborneMethod D Mulit-ComponentSolventborneMethod E Mulit-Component90 % SolidsSolvent Type and Amount 3 6 1 ml water (6.2)36 1 ml solvent (6.3)36 1 ml water (6.2)36 1 ml solvent (6.3) noneSpecimen Weight 0.3 6 0.1 g if expected result is =60 % non-volatile)0.5 6 0.
32、1 g if expected result is 40 % volatile (60 % non-volatile)seeAInduction Time N/A N/A 1 hr (seeB) 1 hr (seeB)24hrASpecimen weight to be representative of how the product is used (the lowest thickness which the manufacturers literature recommends) where: Weight (g) = Thickness(mm) 3 3.14 3 Dish Diame
33、ter2(mm2)/4 3 Density (g/cc)/1000. For example: the appropriate specimen weight for a coating with a density of 1 g/cc placed in a 50 mmdiameter dish at a thickness of 0.5 mm calculates to 1.0 g.BOther induction periods are used. See EPA Reference Method 24.D2369072excess material and cap the syring
34、e. Place the filled syringe onthe scale and tare the scale. Use disposable (no talc) rubber orpolyethylene gloves to handle the syringe.7.7 Remove the cap and dispense from the syringe into thedish the target specimen weight as specified in Table 1.Ifsolvent is used in the dish add the specimen drop
35、wise to thesolvent-containing dish. The paper clip may be used to helpdisperse the coating specimen in the solvent. If the materialforms a lump that cannot be dispersed, discard the specimenand prepare a new one. If no solvent is used (see Table 1,Method E), spread out the specimen in the dish with
36、the paperclip to cover the bottom of the dish completely with as uniformthickness as possible.7.8 After dispensing the specimen, do not wipe the tip of thesyringe. Remove the specimen from the neck of the syringe bypulling up the plunger. Cap and place the syringe on thebalance (that was tared with
37、the syringe before the specimenwas dispensed) and record the weight to the nearest 0.1 mg asthe Specimen Weight (SA).7.9 Repeat steps 7.3-7.8 to prepare a duplicate specimen foreach sample.7.10 For multi-component coatings, after the specimens areprepared, allow them to sit at ambient conditions for
38、 aprescribed induction time according to Table 1 before placingthe dishes in the oven.7.11 Heat the aluminum foil dishes containing the speci-mens in the forced draft oven (5.3) for 60 minutes at 1106 5C.7.12 Remove each dish from the oven, place immediately ina desiccator, cool to ambient temperatu
39、re, weigh to the nearest0.1 mg and record this weight (W2) for each specimen.8. Calculation8.1 Calculate the percent volatile matter, V, in the liquidcoating as follows:VA5 100 2 W22 W1!/SA! 3 100 (1)where:VA= % volatiles (first determination),W1= weight of dish,W2= weight of dish plus specimen afte
40、r heating,SA= specimen weight, andVB= % volatiles (duplicate determination, calculate insame manner as VA).V 5 VA1 VB!/2 (2)8.2 Report V, the mean of the duplicate determination ifrelative percent difference is 1.5 % or less. If relative differencebetween VAand VBis greater than 1.5 %, repeat the du
41、plicatedeterminations.8.3 The percent of nonvolatile matter, N, in the coating maybe calculated by difference as follows:N 5 NA1 NB!/2 (3)where:NA= 100 VA, andNB= 100 VB.NArepresents first determination and NBrepresents duplicatedetermination.9. Precision and Bias9.1 The precision estimated for test
42、s at 60 min at 1106 5Care based on an interlaboratory study5in which 1 operator ineach of 15 laboratories analyzed in duplicate on 2 differentdays 7 samples of waterborne paints and 8 samples ofsolventborne paints containing between 35 and 72 % volatilematerial. The paints were commercially supplied
43、. The resultswere analyzed statistically in accordance with Practice E 180.The within-laboratory coefficient of variation was found to be0.5 % relative at 213 df and the between-laboratories coeffi-cient of variation was 1.7 % relative at 198 df. Based on thesecoefficients, the following criteria sh
44、ould be used for judgingthe acceptability of results at the 95 % confidence level.9.1.1 RepeatabilityTwo results, each the mean of dupli-cate determinations, obtained by the same operator on differentdays should be considered suspect if they differ by more than1.5 % relative.9.1.2 ReproducibilityTwo
45、 results, each the mean of dupli-cate determinations, obtained by operators in different labora-tories should be considered suspect if they differ by more than4.7 % relative.9.2 BiasBias has not been determined.9.3 The precision results for multicomponent systems arebased on an interlaboratory study
46、 in which one operator in eachof five laboratories analyzed in duplicate on two different days,four samples of commercially supplied solventborne andwaterborne multicomponent systems. The results were ana-lyzed statistically in accordance with Practice E 180.9.3.1 Repeatability for Solventborne Mult
47、icomponent Sys-tems:Coefficient of variation 0.5 %Degrees of freedom 6Factor (based on 95 % confidence level) 3.46Precision 1.74 %Two results, each the mean of duplicate determinationsobtained by the same operator on different days, should beconsidered suspect if they vary by more than 1.74 % relati
48、ve.9.3.2 Reproducibility for Solventborne Multicomponent Sys-tems:Coefficient of variation 1.46 %Degrees of freedom 5Factor (based on 95 % confidence level) 3.46Precision 5.31 %Two results, each the mean of duplicate determinationsobtained by operators in different laboratories, should beconsidered
49、suspect if they vary by more than 5.31 % relative.9.3.3 Repeatability for Waterborne Multicomponent Sys-tems:Coefficient of variation 0.53 %Degrees of freedom 6Factor (based on 95 % confidence level) 3.46Precision 1.84 %Two results, each the mean of duplicate determinationsobtained by the same operator on different days, should beconsidered suspect if they vary by more than 1.84 % relative.5Supporting data are available from ASTM International Headquarters. RequestRR: D01-1026.D23690739.3.4 Reproducibility for Waterborne Multicomponent Sys-tems:
