1、Designation: D2369 10Standard 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 number in parentheses
2、 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 Department of Defense.1. Scope1.1 This test method describes a procedure for the determi-nation of the weight
3、 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 minut
4、es 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 chemical
5、 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 tem
6、perature 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 the standardmethod for nonvolatile content of these types of materials.1.5 Test Method
7、s 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 Sheet-Fedand Coldset Web Offset Printing Inks is the method of choicefor these types of
8、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 to cur
9、e 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 D3960 for Determining Volatile Organic Compound(
10、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 are fo
11、r 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 prior to u
12、se.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD3925 Practice for Sampling Liquid Paints and RelatedPigmented CoatingsD3960 Practice for Determining Volatile Organic Com-pound (VOC) Content of Paints and Related CoatingsD5095 Test Method for Determination of the N
13、onvolatileContent in Silanes, Siloxanes and Silane-Siloxane BlendsUsed in Masonry Water Repellent TreatmentsD5403 Test Methods for Volatile Content of RadiationCurable MaterialsD6419 Test Method for Volatile Content of Sheet-Fed andColdset Web Offset Printing InksE145 Specification for Gravity-Conve
14、ction and Forced-Ventilation OvensE177 Practice for Use of the Terms Precision and Bias inASTM Test Methods1This 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 An
15、alysis of Paints and Paint Materials.Current edition approved July 1, 2010. Published September 2010. Originallyapproved in 1965. Last previous edition approved in 2007 as D2369 07. DOI:10.1520/D2369-10.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Ser
16、vice 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.E180 Practice for Determining the Precision
17、 of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty Chemicals3E691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method2.2 Other Standards:EPAReference Method 24 Determination of Volatile MatterContent, Density, Volume Solids, and Weight Solid
18、s 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 oven at 110 6 5C for 60min. The percent volatile is calculated from the loss in weight.4. Significanc
19、e 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. The weight percent solids content (nonvolatile matter)may be determined by difference. This informa
20、tion 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 Aluminum Foil Dishes5, 58 mm in diameter by 18 mmhigh with a smooth (planar) bottom surface. Precondition t
21、hedishes 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 inSpecification E145. The oven must be operating in accordancewith Specification E145, since it is import
22、ant 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,capable of properly dispensing the coating under test, at asufficient rate so that the specimen can be di
23、ssolved 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 indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytica
24、l 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 its use without lessening theaccuracy of the determination.6.2 Purity of WaterUnless otherwise indic
25、ated, 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 (eachcomponent) in accordance with Practice D3925. Mix thor-oughly by hand before taking specimens.7.2 For m
26、ulti-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 container to preventloss of volatile materials.7.3 Weigh the preconditioned aluminum foil dish (see 5
27、.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 specimen, ametal paper clip may be placed (partially unfolded) in thealuminum dish and weighed with the dish
28、. 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 Draw the coating specimen into the syringe. Remove thesyringe from the specimen and then pull the plung
29、er 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 onthe scale and tare the scale. Use disposable (no talc) rubber orpolyethylene gloves to handle the syri
30、nge.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 dish. The paper clip may be used to helpdisperse the coating specimen in the solvent. If the materialf
31、orms 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 the paperclip to cover the bottom of the dish completely with as uniformthickness as possible.7.8 After dispensing the specimen, do
32、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 specimen3Withdrawn. The last approved version of this historical standard is referencedon www.astm.org.4Avail
33、able 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), ; Cole-Parme
34、r, 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, BDH Ltd.
35、, Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.D2369 102was 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 sa
36、mple.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.7.11 Heat the aluminum foil dishes containing the speci-mens in the forced draft oven (5.3) for 60
37、 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. Calculation8.1 Calculate the percent volatile matter, V, in the liquidcoating as follows:VA5 100 2 W22 W1!/
38、SA! 3 100 (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 insame manner as VA).V 5 VA1 VB!/2 (2)8.2 Report V, the mean of the duplicate determination ifrelativ
39、e 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 applicabeto Method E.8.3 The percent of nonvolatile matter, N, in the coating maybe calculated by difference as follows:N 5 NA1
40、 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 tests at 60 min at 110 6 5Care based on an interlaboratory study7in which 1 operator ineach of 15 laboratories analyzed in duplicate
41、 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 statistically in accordance with Practice E180.The within-laboratory coefficient of variation was fo
42、und 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 acceptability of results at the 95 % confidence level.9.1.1 RepeatabilityTwo results, each the mean
43、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 dupli-cate determinations, obtained by operators in different labora-tories should be considered susp
44、ect 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 eachof five laboratories analyzed in duplicate on two different days,four samples of commercially supp
45、lied 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 of variation 0.5 %Degrees of freedom 6Factor (based on 95 % confidence level) 3.46Precision 1.74
46、%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 % relative.7Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D01-10
47、26.TABLE 1 Summary of MethodsCoating TypeMethod A One ComponentWaterborneMethod B One ComponentSolventborneMethod 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
48、 ml solvent (6.3) noneSpecimen Weight 0.3 6 0.1 g if expected result is =60 % non-volatile)0.5 6 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
49、eight laboratories tested fivedifferent materials, 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 D011152.89.5.1 Repeatability Limit (r)Two test results, each themean of duplicate determinations, obtained within one labora-tory shall be judged not e
