1、Designation: D2369 10 (Reapproved 2015)1Standard Test Method forVolatile Content of Coatings1This standard is issued under the fixed designation D2369; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A nu
2、mber 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.1NOTEParagraph 9.3.2 was editorially corrected in June 2015.1.
3、Scope1.1 This test method describes a procedure for the determi-nation of the weight 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-c
4、ured baking systems, and also in-cluded multicomponent paint systems.1.2 Sixty minutes 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, a
5、t ambient conditions, contain liquid coreac-tants that are volatile until a chemical 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 weigh
6、ed components in the correct proportions and allow thespecimens to stand at room temperature for 1 h prior to placing them intothe oven.1.4 Test Method D5095 for Determination of the Nonvola-tile Content in Silanes, Siloxanes and Silane-Siloxane BlendsUsed in Masonry Water Repellent Treatments is th
7、e standardmethod for nonvolatile content of these types of materials.1.5 Test Methods D5403 for Volatile Content of RadiationCurable Materials is the standard method for determiningnonvolatile content of radiation curable coatings, inks andadhesives.1.6 Test Method D6419 for Volatile Content of Shee
8、t-Fedand Coldset Web Offset Printing Inks is the method of choicefor these types 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 degradati
9、on of the specimenoccurs during heating, the actual time and temperature used 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
10、for 1 h for coatings.NOTE 4Practice D3960 for Determining Volatile Organic Compound(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 i
11、n SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.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 hea
12、lth practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD3925 Practice for Sampling Liquid Paints and RelatedPigmented CoatingsD3960 Practice for DeterminingVolatile Organic Compound(VOC) Co
13、ntent of Paints and Related CoatingsD5095 Test Method for Determination of the NonvolatileContent in Silanes, Siloxanes and Silane-Siloxane BlendsUsed in Masonry Water Repellent TreatmentsD5403 Test Methods for Volatile Content of Radiation Cur-able MaterialsD6419 Test Method for Volatile Content of
14、 Sheet-Fed andColdset Web Offset Printing Inks1This test method is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings, Materials, and Applications and is the direct responsibility ofSubcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.Current edition approved
15、 June 1, 2015. Published June 2015. Originallyapproved in 1965. Last previous edition approved in 2010 as D2369 101. DOI:10.1520/D2369-10R15E01.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards v
16、olume information, refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1E145 Specification for Gravity-Convection and Forced-Ventilation OvensE177 Practice for Use of the Term
17、s Precision and Bias inASTM Test MethodsE180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty Chemicals (Withdrawn 2009)3E691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method2.2 Other Standards:EPA
18、Reference Method 24 Determination of Volatile MatterContent, Density, Volume Solids, and Weight Solids ofSurface Coatings43. Summary of Test Method3.1 A designated quantity of coating specimen is weighedinto an aluminum foil dish containing 3 mL of an appropriatesolvent, dispersed, and heated in an
19、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 specified test condi-tions
20、. 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 weighing 60.1 mg.5.2 Alumin
21、um Foil Dishes5, 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 IIB as specified inSp
22、ecification E145. The oven must be operating in accordancewith Specification E145, since it is important to have proper airflow 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 equipped with caps,capa
23、ble 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. Unless otherwise indicate
24、d, 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.6Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit
25、 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 SpecificationD1193.6.3 Toluene, water or appropriate solvent.7. Procedure7.1 Take a representative sample of the liquid coating (eachco
26、mponent) in accordance with Practice D3925. 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 specimens. Tightly close the
27、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 or spreading the specime
28、n, 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 according to Table 1.7.6 Dr
29、aw 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 removeexcess material and cap the syringe. Place the filled syringe ont
30、he 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 dropwise to thesolvent-containing d
31、ish. 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 1,3The last approved version of this historical standard is referenced onwww.astm.org
32、.4Available from U.S. Government Printing Office Superintendent of Documents,732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http:/www.access.gpo.gov.5Available from Fisher, Disposable Aluminum Dishes (code 08732106),; McAlister Bicknell, Aluminum Weighing Dishes (code106760000), ; Col
33、e-Parmer, Disposable Aluminum WeighDishes (code EW-0101744), .6Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, B
34、DH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.D2369 10 (2015)12Method E), spread out the specimen in the dish with the paperclip to cover the bottom of the dish completely with as uniformthickness as p
35、ossible.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 the syringe before the specimenwas dispensed) and record the weight to the nearest 0.1
36、 mg asthe Specimen Weight (SA).7.9 Repeat steps 7.3 7.8 to prepare a duplicate specimenfor each sample.7.10 For multi-component coatings, after the specimens areprepared, allow them to sit at ambient conditions for aprescribed induction time according to Table 1 before placingthe dishes in the oven.
37、7.11 Heat the aluminum foil dishes containing the speci-mens in the forced draft oven (5.3) for 60 min at 110 6 5C.7.12 Remove each dish from the oven, place immediately ina desiccator, cool to ambient temperature, weigh to the nearest0.1 mg and record this weight (W2) for each specimen.8. Calculati
38、on8.1 Calculate the percent volatile matter, V, in the liquidcoating as follows:VA5 100 2 W22 W1!/SA! 3100# (1)where:VA= % volatiles (first determination),W1= weight of dish,W2= weight of dish plus specimen after heating,SA= specimen weight, andVB= % volatiles (duplicate determination, calculate in
39、samemanner as VA).V 5 VA1VB!/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 duplicatedeterminations. The 1.5 % relative difference is not applicableto Method E.8.3 The
40、percent of nonvolatile matter, N, in the coating maybe calculated by difference as follows:N 5 NA1NB!/2 (3)where:NA= 100 VA, andNB= 100 VB.NArepresents first determination and NBrepresents duplicatedetermination.9. Precision and Bias9.1 The precision estimated for tests at 60 min at 110 6 5Care base
41、d on an interlaboratory study7in 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. The resultswere analyzed sta
42、tistically in accordance with Practice E180.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 should be used for judgingthe acc
43、eptability 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 results, each the mean of dupl
44、i-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 in which one operator in eacho
45、f 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 E180.9.3.1 Repeatability for Solventborne Multicomponent Sys-tems:Coefficient
46、of variation 0.5 %Degrees of freedom 6Factor (based on 95 % confidence level) 3.46Precision 1.74 %7Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D01-1026. ContactASTM CustomerService at serviceastm.org.TABLE 1 Summary of Method
47、sCoating TypeMethod A One ComponentWaterborneMethod B One ComponentSolventborneMethod C Multi-ComponentWaterborneMethod D Multi-ComponentSolventborneMethod E Multi-Component90 % SolidsSolvent Type and Amount 31mlwater(6.2) 31mlsolvent (6.3) 31mlwater(6.2) 31mlsolvent (6.3) noneSpecimen Weight 0.3 0.
48、1 g if expected result is =60 % non-volatile)0.5 0.1 g if expected result is 40 % volatile (90 % SolidsSystemsThe precision of this test was expanded to includedata and analysis from Method E based on an interlaboratorystudy conducted in 2009. Each of eight laboratories tested fivedifferent material
49、s, all multi-component, 90 % solids systems.Every “test result” represents the mean of duplicate determi-nations. Every laboratory reported three replicate test resultsfor the analysis. Practice E691 was followed for the design andanalysis of the data; the details are given in ASTM ResearchReport RR:D01-1152.89.5.1 Repeatability Limit (r)Two test results, each themean of duplicate determinations, obtained within one labora-tory shall be judged not equivalent if they differ by mo
