1、Designation: D3960 05 (Reapproved 2013)Standard Practice forDetermining Volatile Organic Compound (VOC) Content ofPaints and Related Coatings1This standard is issued under the fixed designation D3960; the number immediately following the designation indicates the year oforiginal adoption or, in the
2、case of revision, the 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 Department of Defense.1. Scope1.1 This pr
3、actice measures the volatile organic compound(VOC) content of solventborne and waterborne paints andrelated coatings as determined from the quantity of materialreleased from a sample under specified bake conditions andsubtracting exempt volatile compounds and water if present.NOTE 1The regulatory de
4、finition, under the control of the U.S. EPA,can change. To ensure currency, contact the local air pollution controlagency.1.2 This practice provides a guide to the selection ofappropriate ASTM test methods for the determination of VOCcontent.1.3 Certain organic compounds that may be released underth
5、e specified bake conditions are not counted toward coatingVOC content because they do not participate appreciably inatmospheric photochemical reactions. Such negligibly photo-chemically reactive compounds are referred to, as exemptvolatile compounds in this practice.NOTE 2Information on the US EPAde
6、finition of VOC and a list of thecurrent US EPA approved exempt volatile compounds which have beenused in coatings, are provided in Appendix X3.1.4 VOC content is calculated as a function of (1) thevolume of coating less water and exempt volatile compounds,and (2) the volume of coating solids, and (
7、3) the weight ofcoating solids.1.5 The values stated in SI units are to be regarded asstandard.1.6 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 pr
8、actices 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 CoatingsD2697 Test Method for Volume Nonvolatile Matter in C
9、learor Pigmented CoatingsD2832 Guide for Determining Volatile and Nonvolatile Con-tent of Paint and Related CoatingsD3792 Test Method for Water Content of Coatings by DirectInjection Into a Gas ChromatographD3925 Practice for Sampling Liquid Paints and RelatedPigmented CoatingsD4017 Test Method for
10、Water in Paints and Paint Materialsby Karl Fischer MethodD4457 Test Method for Determination of Dichloromethaneand 1,1,1-Trichloroethane in Paints and Coatings byDirect Injection into a Gas ChromatographD5095 Test Method for Determination of the NonvolatileContent in Silanes, Siloxanes and Silane-Si
11、loxane BlendsUsed in Masonry Water Repellent TreatmentsD5201 Practice for Calculating Formulation Physical Con-stants of Paints and CoatingsD5403 Test Methods for Volatile Content of Radiation Cur-able MaterialsD6093 Test Method for Percent Volume Nonvolatile Matterin Clear or Pigmented Coatings Usi
12、ng a Helium GasPycnometerD6133 Test Method for Acetone, p-Chlorobenzotrifluoride,Methyl Acetate or t-Butyl Acetate Content of Solvent-borne and Waterborne Paints, Coatings, Resins, and RawMaterials by Direct Injection Into a Gas ChromatographD6419 Test Method for Volatile Content of Sheet-Fed andCol
13、dset Web Offset Printing Inks1This practice is under the jurisdiction of ASTM Committee D01 on Paint andRelated Coatings, Materials, and Applications and is the direct responsibility ofSubcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.Current edition approved Nov. 1, 2013. Publi
14、shed November 2013. Originallyapproved in 1981. Last previous edition approved in 2005 as D3960 05. DOI:10.1520/D3960-05R13.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, r
15、efer 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 States1D6438 Test Method for Acetone, Methyl Acetate, andParachlorobenzotrifluoride Content of Paints, and Coat-ings by Solid Phas
16、e Microextraction-Gas Chromatogra-phyD6886 Test Method for Determination of the IndividualVolatile Organic Compounds (VOCs) inAir-Dry Coatingsby Gas ChromatographyE180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty Chemicals (Withdrawn 200
17、9)32.2 Other Documents:EPAFederal Reference Method 24 Determination ofVola-tile Matter Content, Density, Volume Solids, and WeightSolids of Surface Coatings4EPA 450/3-84-019 U.S. Environmental Protection AgencyProcedures for Certifying Quantity of Organic CompoundEmitted by Paint, Ink, and Other Coa
18、tings43. Terminology3.1 Definitions:3.1.1 exempt volatile compound, norganic compoundsthat do not participate significantly in atmospheric photochemi-cal reactions.3.1.2 nonvolatile material, nthe solid material remainingafter volatiles have been removed from a coating underspecified test conditions
19、.3.1.3 volatile organic compound (VOC), nany organiccompound that participates in atmospheric photochemicalreactions.3.1.3.1 DiscussionInformation on the US EPA definitionof VOC and a list of the current US EPAand approved exemptvolatile compounds which have been used in coatings, areprovided in App
20、endix X3.3.1.4 volatile organic compound content (VOC content),nthe mass of VOC released from a coating under specifiedtest conditions.3.1.4.1 DiscussionVOC content is expressed in this prac-tice as a function of: (1) the coating volume less water andexempt volatile compounds, and (2) the volume of
21、coatingsolids and (3) the weight of coating solids.4. Summary of Practice4.1 Take a representative sample of the liquid coating inaccordance with Practice D3925. Mix thoroughly before takingspecimens for individual tests. If air bubbles becomeentrapped, stir by hand until the air has been removed.4.
22、2 The volatile content, density, water content, volumesolids and exempt solvent content of the coating are deter-mined in accordance with designated methods and instructions.For multicomponent coatings, the components are first mixedin the appropriate ratios and the applicable values determinedon th
23、e mixture. These values are combined using specifiedequations to calculate the VOC content of the coating.NOTE 3In Reference Method 24 the U.S. EPA defines a waterbornecoating as any coating with more than 5 % water by weight in its volatilefraction, and requires/allows water determination for water
24、borne coatingsonly.5. Significance and Use5.1 This practice discusses applicable ASTM test methodsused in the determination of the VOC content of paints andrelated coatings and provides equations for calculating theVOC content expressed as the mass of VOC: (1) per unitvolume of coating less water an
25、d exempt volatile compounds,and (2) per unit volume of coating solids and (3) per unit massof coating solids.5.2 Volatile organic compound content is used to comparethe amount of VOC released from different coatings used forthe same application, that is, to coat the same area to the samedry film thi
26、ckness (assuming the same application efficiency).5.3 VOC content data are required by various regulatoryagencies.5.4 Only the expression of VOC content as a function of thevolume of coating solids gives a linear measure of thedifference in VOC released from different coatings used for thesame appli
27、cation.NOTE 4Thus assuming the same transfer efficiency, a coating withVOC content of 3 lb of VOC/gal of solids would release12 the VOC thatwould a coating with 6 lb of VOC/gal of solids.5.5 When VOC content is expressed as a function of thevolume of coating less water and exempt solvents, the value
28、sobtained do not account for differences in the volume solidscontent of the coatings being compared: this expression,therefore, does not provide a linear measure of the difference inVOC emitted from different coatings used for the sameapplication.NOTE 5Thus, a coating with VOC content of 3 lb of VOC
29、/gal lesswater and exempt volatile compounds would release about 85 % lessVOCthan a coating with 6 lb of VOC/gal less water and exempt volatilecompounds.6. Nonvolatile and Volatile Content6.1 Guide D2832 includes suggested time/temperature dry-ing schedules for the determination of the nonvolatile a
30、ndvolatile content of various types of coatings.NOTE 6For regulatory compliance testing, follow the method andconditions specified in the applicable regulation. Federal ReferenceMethod 24 specifies the use of Test Method D2369.6.2 Test Method D2369 includes a specific drying scheduleand sample weigh
31、t, and heating1hat1106 5C for thedetermination of the weight percent volatile content of solvent-borne and waterborne coatings.6.2.1 For multicomponent coatings, Test Method D2369specifies the components should be mixed first, then thevolatile content should be determined on the mixture. Testspecime
32、ns are held in the aluminum dish for at least 1 h beforebaking.3The last approved version of this historical standard is referenced onwww.astm.org.4Available from U.S. Government Printing Office Superintendent of Documents,732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http:/www.acces
33、s.gpo.gov.D3960 05 (2013)2NOTE 7Other induction periods are used. See U.S. EPA ReferenceMethod 24.6.2.2 The nonvolatile content of silanes, siloxanes, andsilane/siloxane blends used in masonry water repellent treat-ments is defined using Test Method D5095. In this standard,applicable to both solvent
34、 and water reducible materials, thetest specimen, containing an added catalyst, is allowed to standat room temperature for 1 h prior to heating in an oven at 1106 5C for 60 min.NOTE 8In VOC determinations, for 6.2.2 only, the density and watercontent (if applicable) are measured on the test material
35、 without the addedcatalyst.6.2.3 The nonvolatile content of radiation curable coatings,inks, and adhesives is defined using Test Methods D5403.These materials contain volatile reactive components thatbecome nonvolatile after radiation curing. Test Method A isapplicable to radiation curable materials
36、 that are essentially100 % reactive but may contain traces (no more than 3 %) ofvolatile materials as impurities or introduced by the inclusionof various additives. Test Method B is applicable to allradiation curable materials but must be used for materials thatcontain volatile solvents intentionall
37、y introduced to controlapplication viscosity and that are intended to be removed fromthe material to cure.6.2.4 The volatile content of sheet-fed and coldset weboffset printing inks is defined using Test Method D6419. Thisstandard is based on Test Method D2369, but has tightercontrols for specimen w
38、eight and oven temperature. Interlabo-ratory studies have shown this necessary to improve theprecision of test results for these inks. It also allows the use ofink knives or taper knives for transferring the specimen to thealuminum dish from the sample container.6.2.5 Test Method D6886 is a direct g
39、as chromatographicmethod for the determination of individual and total volatileorganic compounds in low VOC content waterborne latexair-dry coatings. This method is intended primarily for analysisof waterborne coatings in which the material VOC content isbelow 5 weight percent. It is the only method
40、 for the speciationof VOCs in low VOC content waterborne latex air-dry coat-ings. This method provides a direct determination of weightpercent VOC content, in contrast to the indirect determination(total volatiles minus water) of weight percent VOC ofwaterborne coatings presented in Practice D3960.7
41、. Water Content7.1 To determine the water content of coatings two testmethods are available:7.1.1 In Test Method D3792, a paint specimen is dilutedwith dimethyl formamide, an internal standard (2-propanol) isadded, and an aliquot of the mixture is injected directly into agas chromatograph.7.1.2 Test
42、 Method D4017 offers three options for determin-ing water content by Karl Fischer titration.7.1.2.1 A specimen is dissolved in pyridine or anothersuitable solvent and titrated in the presence of a buffer, 1-ethylpiperidine. The use of newer non-pyridine titration reagents isalso allowed.7.1.2.2 The
43、water in a latex paint is first extracted intoanhydrous methanol, then an aliquot of the methanol extract istitrated with non-pyridine reagent in methanol solvent (seeAppendix X1 of Test Method D4017).7.1.2.3 The specimen is dispersed in methanol solvent usinga homogenizer accessory, then directly t
44、itrated with non-pyridine reagent (see Appendix X2 of Test Method D4017).7.1.3 With multicomponent coatings, the components arefirst mixed in the appropriate ratios, then water content isdetermined using Test Methods D3792 or D4017.8. Density8.1 The density of the paint or coating at 25C is determin
45、edin accordance with Test Method D1475. Although both thepycnometer and weight-per-gallon cup are covered by the testmethod, and the former is more accurate and precise, theweight-per-gallon cup is recommended because of its speedand ease of use.8.2 With multicomponent coatings, first mix the compo-
46、nents in appropriate ratios in sufficient quantity to determinethe weight-per-gallon using Test Method D1475.9. Exempt Volatile Compounds9.1 In Test Method D4457 an internal standard (1-propanol)is added to the test specimen, and then the specimen is injecteddirectly into a gas chromatograph.9.2 In
47、Test Method D6133 an internal standard is added tothe whole paint, and the mixture injected directly into the gaschromatograph.9.3 In Test Method D6438 an internal standard is added towhole paint, followed by solid phase microextraction (SPME)headspace sampling and subsequent injection into a gas ch
48、ro-matograph.9.4 With multicomponent coatings, the exempt volatilecompound content is determined on the mixture of the com-ponents.10. Calculation of VOC Content10.1 In this practice VOC content is expressed in threeways: (1) as the mass of VOC per unit volume of the coatingless water and exempt vol
49、atile compounds, (2) as the mass ofVOC per unit volume of coating solids, and (3) the mass ofVOC per unit mass of coatings solids. The following equationsshould be used to calculate VOC content and may be used forcoatings both “as supplied” and “as applied” (see Note 8).NOTE 9For compliance with VOC regulations, the VOC contentshould be calculated after any thinning or dilution (“as applied”).Instructions for VOC calculations of such diluted coatings are available inEPA 450/3-84-019.10.2 VOC Content Expressed as the Mass of VOC per UnitVolume of Coating Less Wa