Designation:D3960–04
Standard Practice for
Determining Volatile Organic Compound(VOC)Content of Paints and Related Coatings1
This standard is issued under thefixed designation D3960;the number immediately following the designation indicates the year of original adoption or,in the case of revision,the year of last revision.A number in parentheses indicates the year of last reapproval.A superscript 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.Scope
1.1This practice measures the volatile organic compound (VOC)content of solventborne and waterborne paints and related coatings as determined from the quantity of material released from a sample under specified bake conditions and subtracting exempt volatile compounds and water if present. N OTE1—The regulatory definition,under the control of the U.S.EPA, can change.To ensure currency,contact the local air pollution control agency.
1.2This practice provides a guide to the selection of appropriate ASTM test methods for the determination of VOC content.
1.3Certain organic compounds that may be released under the specified bake conditions are not classified as VOC,as they do not participate in atmospheric photochemical reactions. Such nonphotochemically reactive compounds are referred to as exempt volatile compounds in this practice.
N OTE2—A list of the current US EPA approved exempt volatile compounds is found in Appendix X3,paragraph X3.1.1.1.
1.4VOC content is calculated as a function of(1)the volume of coating less water and exempt volatile compounds, and(2)the volume of coating solids,and(3)the weight of coating solids.
2.Referenced Documents
2.1ASTM Standards:2
D1475Test Method for Density of Liquid Coatings,Inks, and Related Products
D2369Test Method for V olatile Content of Coatings D2697Test Method for V olume Nonvolatile Matter in Clear or Pigmented Coatings
D2832Guide for Determining V olatile and Nonvolatile Content of Paint and Related Coatings
D3792Test Method for Water Content of Coatings by Direct Injection into a Gas Chromatograph
D3925Practice for Sampling Liquid Paints and Related Pigmented Coatings
D4017Test Method for Water in Paints and Paint Materials by Karl Fischer Method
D4457Test Method for Determination of Dichloromethane and1,1,1-Trichloroethane in Paints and Coatings by Direct Injection into a Gas Chromatograph
D5095Test Method for Determination of the Nonvolatile Content in Silanes,Siloxanes and Silane-Siloxa
ne Blends Used in Masonry Water Repellent Treatments
D5201Practice for Calculating Formulation Physical Con-stants of Paints and Coatings
D5403Test Methods for V olatile Content of Radiation Curable Materials
D6093Test Method for Percent V olume Nonvolatile Matter in Clear or Pigmented Coatings Using a Helium Gas Pycnometer
D6133Test Method for Acetone p-Chlorobenzotrifluoride, Methyl Acetate or t-Butyl Acetate Content of Solvent-Reducible and Water-Reducible Paints,Coatings,Resins, and Raw Materials by Direct Injection into a Gas Chro-matograph
D6419Test Method for V olatile Content of Non-Heatset Web Offset Printing Inks
D6438Test Method for Acetone,Methyl Acetate,and Parachlorobenzotrifluoride Content of Paints and Coatings by Solid Phase Microextraction-Gas Chromatography
D6886Test Method for Speciation of the V olatile Organic Compounds(VOCs)in Low VOC Content Waterborne Air-Dry Coatings by Gas Chromatography
E180Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial and Spe-cialty Chemicals
2.2Other Documents:
1This practice is under the jurisdiction of ASTM Committee D01on Paint and
Related Coatings,Materials,and Applications and is the direct responsibility of
Subcommittee D01.21on Chemical Analysis of Paints and Paint Materials.
Current edition approved Mar.1,2004.Published March2004.Originally
approved in1981.Last previous edition approved in2002as D3960–02.
2For referenced ASTM standards,visit the ASTM website,,or
contact ASTM Customer Service at For Annual Book of ASTM
Standards volume information,refer to the standard’s Document Summary page on
the ASTM website.
1
Copyright©ASTM International,100Barr Harbor Drive,PO Box C700,West Conshohocken,PA19428-2959,United States.
EPA Federal Reference Method 24—Determination of V olatile Matter Content,Density,V olume Solids,and Weight Solids of Surface Coatings 3
EPA 450/3-84-019,U.S.Environmental Protection Agency Procedures for Certifying Quantity of Organic Compound Emitted by Paint,Ink,and Other Coatings 3
EPA 450/3-83-013R,U.S.Environmental Protection Agency Glossary for Air Pollution Control of Industrial Coatings Operations 33.Terminology 3.1Definitions:
3.1.1exempt volatile compound —organic compounds that do not participate significantly in atmospheric photochemical reactions.
3.1.2nonvolatile material —the solid material remaining after volatiles have been removed from a coating under specified test conditions.
3.1.3volatile organic compound (VOC)—any organic com-pound that participates in atmospheric photochemical reac-tions.
3.1.3.1Discussion —The definition of VOC adopted by the U.S.EPA and a list of exempt volatile compounds are included in Appendix X3.
3.1.4volatile organic compound content (VOC content)—the mass of VOC released from a coating under specified test conditions.
3.1.
4.1Discussion —VOC content is expressed in this prac-tice as a function of:(1)the coating volume less water and exempt volatile compounds,and (2)the volume of coating solids and (3)the weight of coating solids.
4.Summary of Practice
4.1Take a representative sample of the liquid coating in accordance with Practice D 392
5.Mix thoroughly before taking specimens for individual tests.If air bubbles become entrapped,stir by hand until the air has been removed.
4.2The volatile content,density,water content,volume solids and exempt solvent content of the coating are deter-mined in accordance with designated methods and instructions.For multicomponent coatings,the components are first mixed in the appropriate ratios and the applicable values determined on the mixture.These values are combined using specified equations to calculate the VOC content of the coating.
N OTE 3—In Reference Method 24,the U.S.EPA defines a waterborne coating as any coating with more than 5%water by weight in its volatile fraction,and requires/allows water determination for waterborne coatings only.
5.Significance and Use
5.1This practice discusses applicable ASTM test methods used in the determination of the VOC content of paints and related coatings and provides equations for calculating the VOC content expressed as the mass of VOC:(1)per unit
volume of coating less water and exempt volatile compounds,and (2)per unit volume of coating solids and (3)per unit mass of coating solids.
5.2V olatile organic compound content is used to compare the amount of VOC released from different coatings used for the same application,that is,to coat the same area to the same dry film thickness (assuming the same application efficiency).5.3VOC content data are required by various regulatory agencies.
5.4Only the expression of VOC content as a function of the volume of coating solids gives a linear measure of the difference in VOC released from different coatings used for the same application.
N OTE 4—Thus assuming the same transfer efficiency,a coating with VOC content of 3lb of VOC/gal of solids would release 1⁄2the VOC that would a coating with 6lb of VOC/gal of solids.
5.5When VOC content is expressed as a function of the volume of coating less water and exempt solvents,the values obtained do not account for differences in the volume solids content of the coatings being compared:this expression,therefore,does not provide a linear measure of the difference in VOC emitted from different coatings used for the same application.
N OTE 5—Thus,a coating with VOC content of 3lb of VOC/gal less water and exempt volatile compounds would release about 85%less VOC than a coating with 6lb of VOC/gal less water and exempt volatile compounds.
6.Nonvolatile and Volatile Content
6.1Guide D 2832includes suggested time/temperature dry-ing schedules for the determination of the nonvolatile and volatile content of various types of coatings.
N OTE 6—For regulatory compliance testing,follow the method and conditions specified in the applicable regulation.Federal Reference Method 24specifies the use of Test Method D 2369.
6.2Test Method D 2369includes a specific drying schedule and sample weight,and heating 1h at 11065°C for the determination of the weight percent volatile content of solvent-borne and waterborne coatings.
6.2.1For multicomponent coatings,Test Method D 2369specifies the components should be mixed first,then the volatile content should be determined on the mixture.Test specimens are held in the aluminum dish for at least 1h before baking.
N OTE 7—Other induction periods are used.See U.S.EPA Reference Method 24.
6.2.2The nonvolatile content of silanes,siloxanes,and silane/siloxane blends used in masonry water repellent treat-ments is defined using Test Method D 5095.In this standard,applicable to both solvent and water reducible materials,the test specimen,containing an added catalyst,is allowed to stand at room temperature for 1h prior to heating in an oven at 110°65°C for 60min.
N OTE 8—In VOC determinations,for 6.2.2only,the density and water content (if applicable)are measured on the test material without the added catalyst.
3
Available from the Superintendent of Documents,U.S.Government Printing Office,Washington,DC
20402.
6.2.3The nonvolatile content of radiation curable coatings, inks,and adhesives is defined using Test Methods D5403. These materials contain volatile reactive components that become nonvolatile after radiation curing.Test Method A is applicable to radiation curable materials that are essentially 100%reactive but may contain traces(no more than3%)of volatile materials as impurities or introduced
by the inclusion of various additives.Test Method B is applicable to all radiation curable materials but must be used for materials that contain volatile solvents intentionally introduced to control application viscosity and that are intended to be removed from the material to cure.
6.2.4The volatile content of sheet-fed and coldset web offset printing inks is defined using Test Method D6419.This standard is based on Test Method D2369,but has tighter controls for specimen weight and oven temperature.Interlabo-ratory studies have shown this necessary to improve the precision of test results for these inks.It also allows the use of ink knives or taper knives for transferring the specimen to the aluminum dish from the sample container.
6.2.5Test Method D6886is a direct gas chromatographic method for the determination of individual and total volatile organic compounds in low VOC content waterborne latex air-dry coatings.This method is intended primarily for analysis of waterborne coatings in which the material VOC content is below5weight percent.It is the only method for the speciation of VOCs in low VOC content waterborne latex air-dry coat-ings.This method provides a direct determination of weight percent VOC content,in contrast to the indirect determination (total volatiles minus water)of weight percent VOC of waterborne coatings presented in Practice D3960.
7.Water Content
7.1To determine the water content of coatings two test methods are available:
7.1.1In Test Method D3792,a paint specimen is diluted with dimethyl formamide,an internal standard(2-propanol)is added,and an aliquot of the mixture is injected directly into a gas chromatograph.
7.1.2Test Method D4017offers three options for determin-ing water content by Karl Fischer titration.
7.1.2.1A specimen is dissolved in pyridine or another suitable solvent and titrated in the presence of a buffer,1-ethyl piperidine.The use of newer non-pyridine titration reagents is also allowed.
7.1.2.2The water in a latex paint isfirst extracted into anhydrous methanol,then an aliquot of the methanol extract is titrated with non-pyridine reagent in methanol solvent(see Appendix X1of Test Method D4017).
7.1.2.3The specimen is dispersed in methanol solvent using
a homogenizer accessory,then directly titrated with non-pyridine reagent(see Appendix X2of Test Method D4017).
7.1.3With multicomponent coatings,the components are first mixed in the appropriate ratios,then water content is determined using Test Methods D3792or D4017.
8.Density
8.1The density of the paint or coating at25°C is determined in accordance with Test Method D1475.Although both the pycnometer and weight-per-gallon cup are covered by the test method,and the former is more accurate and precise,the weight-per-gallon cup is recommended because of its speed and ease of use.
8.2With multicomponent coatings,first mix the compo-nents in appropriate ratios in sufficient quantity to determine the weight-per-gallon using Test Method D1475.
9.Exempt Volatile Compounds
9.1In Test Method D4457an internal standard(1-propanol)is added to the test specimen,and then the specimen is injected directly into a gas chromatograph.
9.2In Test Method D6133an internal standard is added to the whole paint,and the mixture injected directly into the gas chromatograph.
9.3In Test Method D6438an internal standard is added to whole paint,followed by solid phase microextraction(SPME) headspace sampling and subsequent injection into a gas chro-matograph.
9.4With multicomponent coatings,the exempt volatile compound content is determined on the mixture of the com-ponents.
10.Calculation of VOC Content
10.1In this practice VOC content is expressed in three ways:(1)as the mass of VOC per unit volume of the coating less water and exempt volatile compounds,(2)as the mass of VOC per unit volume of coating solids,and(3)the mass of VOC per unit mass of coatings solids.The following equations should be used to calculate VOC content and may be used for coatings both“as supplied”and“as applied”(see Note8).
N OTE9—For compliance with VOC regulations,the VOC content should be calculated after any thinning or dilution(“as applied”). Instructions for VOC calculations of such diluted coatings are available in EPA450/3-84-019.
10.2VOC Content Expressed as the Mass of VOC per Unit Volume of Coating Less Water and Exempt Volatile Com-pounds:
10.2.1General Expression:
@~weight percent of total volatiles less water less(1) VOC5
exempt volatile compounds!~density of coating!#
@100%2~volume percent of water!
2~volume percent of exempt volatile compounds!#
or
VOC5
~W o!~D c!
100%2V w2V ex(2) 5
~W v2W w2W ex!~D c!
100%2~W w!~D c/D w!2~W ex!~D c/D ex!
where:
VOC=VOC content in g/L of coating less water and exempt volatile compound(see Note9),
W o=weight of organic volatiles,%(W v−W w−W ex), W v=weight of total volatiles,%(100%−weight% nonvolatiles,see Test Method D2369),
W w=weight of water,%(see Test Methods D3792or D
4017),
W ex=weight of exempt volatile compound,%(see
3.1.3.1,Note11,and Test Methods D4457,
D6133,and D6438),
V w=volume of water,%(W w)(D c/D w),
V ex=volume of exempt volatile compound,%(see
3.1.3.1,Note11),=(W ex)(D c/D ex),
D c=density of coating,g/L,at25°C,(see Test Method
D1475),
D w=density of water,g/L,at25°C,(0.9973103),and D ex=density of exempt volatile compound g/L,at25°C,
(see Test Method D1475).
N OTE10—To convert from g/L to lb/gal,multiply the result(VOC content)by8.345310−3(lb/gal/g/L).To convert g/L to kg/L,divide the result by103.
N OTE11—See X2.1and X2.2for comments on coatings containing one or more exempt volatile compounds.
10.2.2Solventborne Coatings—Calculate the VOC content in grams of VOC per litre of coating less water and exempt volatile compounds using the appropriate equation:
10.2.2.1For solventborne coatings that do not contain water or exempt volatile compounds:
VOC5~W v!~D c!
100%(3)
10.2.2.2For solventborne coatings that contain an exempt volatile compound but do not contain water(see section3.1.3.1 and Note2):
VOC5editorial hand
~W v2W ex!~D c!
100%2~W ex!~D c/D ex!
(4)
10.2.2.3For solventborne coatings that contain water but do not contain exempt volatile compounds(see3.1.3.1and Note 2):
VOC5
~W v2W w!~D c!
100%2W w!~D c/D w!
(5)
10.2.2.4For solventborne coatings that contain both an exempt volatile compound and water,use Eq1and Eq2in 10.2.1(see3.1.3.1and Note2).
10.2.3Waterborne Coatings—Calculate the VOC content in grams of VOC per litre of coating less water and exempt volatile compound using the appropriate equation.
10.2.3.1For waterborne coatings that contain no exempt volatile compounds,use Eq5in10.2.2.3(see3.1.3.1and Note 2).
10.2.3.2For waterborne coatings that contain exempt vola-tile compounds,use Eq1and Eq2in10.2.1(see3.1.3.1and Note2).
10.3VOC Content Expressed in Terms of the Mass of VOC per Unit Volume of Coating Solids(Nonvolatiles):
10.3.1Calculate the VOC content in grams of VOC per litre of coating solids according to the following equation:
VOC m5
~W o!~D c!
V n(6)
where:
VOC m=VOC content in g/L of coating solids,
W o=W v−W w−W ex(terms defined as in10.2.1), and
V n=volume of nonvolatile content of the liquid coating,%(see Test Methods D6093and
D2697,and Note12and Note13).
N OTE12—The EPA Reference Method24does not include an analyti-
cal method for determining V
n
,but states that the value be calculated from the coating manufacturer’s formulation.
N OTE13—An expression for calculating formula V
n
from the coating formulation is included in X2.3,Eq X2.1.
10.4VOC Content Expressed in Terms of the Mass of VOC per Unit Mass of Coating Solids(Nonvolatiles):
10.4.1Calculate the VOC content in grams of VOC per gram of coating solids according to the following equations:
VOC b5
W o
W S(7) where:
VOC b=VOC content in g/g of coating solids,
W o=W v–W w–W ex(terms defined as in10.2.1,and
W S=weight of solids,%.
N OTE14—The calculated VOC is expressed as weight of VOC/weight of solids.This may be“lb VOC per lb solids”or“Kg of VOC per Kg of solids.”
11.Keywords
11.1test precision;VOC;VOC calculations;VOC content; VOC content of
paint
APPENDIXES
(Nonmandatory Information)
X1.AUTOMOTIVE COATINGS SUPPLIERS ROUND ROBIN
X1.1A round robin was conducted at the laboratories of automotive coatings suppliers for determination of VOC using Practice D 3960.The analysts involved were persons experi-enced in running all the test methods involved in VOC determination.The data was analyzed statistically in accor-dance with Practice E 180.As was suspected from previous round robins conducted to evaluate Practice D 3960(which involved some laboratories not familiar with these test meth-ods),when well experienced analysts conduct the tests,the precision data is much improved.
X1.2The interlaboratory study involved four laboratories
and six samples;four solventborne automotive topcoats and two waterborne automotive topcoats.One operator in each of the four laboratories analyzed the sample in duplicate on 2different days.The following duplicates,repeatability,and reproducibility coefficients of variation were obtained.
Automotive Topcoats Duplicates,%
Repeatability,%
(Within Laboratory)
Reproducibility,%
(Between Laboratory)
Solventborne 0.86 1.62 2.86Waterborne
3.94
5.29
9.75
X2.CALCULATION OF VOC CONTENT (SECTION 10)
X2.1Measurement of Exempt Volatile Compound Content —The value of the weight percent of exempt volatile compound,W ex ,used in the VOC expression in Eq 2and Eq 4and to determine W o for Eq 6,Eq 7,and Eq X2.2can be obtained using Test Method D 4457for methylene chloride and 1,1,1trichlor
oethane,and either Test Methods D 6133or D 6438for acetone,p-chlorobenzotrifluoride and methyl ac-etate.
X2.2Two or More Exempt Volatile Compounds —For solvent or waterborne coatings containing more than one exempt volalile compound,the values for W ex and (W ex )(D c /D ex )to be used in Eq 2and Eq 4,and to determine W o for Eq 6,Eq 7,and Eq X2.2(10.2.1,10.2.2.2,10.3.1,10.4.1,X2.4)are the summations of the values of W ex and (W ex )(D c /D ex )for each individual exempt volatile compound.For example,for a coating with three exempt volatile compounds use (W ex1+W ex2+W ex3)for W ex and use ((W ex1)(D c /D ex1+(W ex2)(D c /D ex2)+(W ex3)(D c /D ex3))for (W ex )(D c /D ex ).
X2.3Volume Nonvolatile Content —The volume percent nonvolatile content,V n ,in Eq 6(10.4.1)can be calculated from the summation of the individual contributions of each compo-nent in the coating formulation (“p”components)using the following equation (Eq X2.1and Eq X2.2):
V n 5
(
j 21
p
[~@V n #j !~V j /100%!#
(X2.1)
where:
(V n )j =volume of nonvolatile content of component “j,”%
[(100%)3(volume of nonvolatiles of “j”per unit volume of “j”)],and
V j
=volume of component “j”in the coating %[(100%)3(volume of “j”used)/(total volume of coating)].
N OTE X2.1—Instructions for calculating the value for the formula
percent volume solids (or formula volume percent nonvolatile)content of the coating are provided in Practice D 5201.
N OTE X2.2—Eq X2.1is meant to clarify the equation (II-4)currently in the EPA document EPA-450/3-84-019for the expression of calculated volume percent nonvolatile content,V n .
X2.4Amount of VOC in a Coating Expressed in Terms of Mass of VOC per Unit Volume of Coating Including Water and Exempt Volatile Compounds —The amount of volatile organic compounds in both solvent-and waterborne coatings can be expressed in terms of the mass of volatile organic compounds per unit volume of coating including water and exempt volatile compounds according to the following equation (Eq X2.2):
VOA 5~W o !~D c !
100%
(X2.2)
where:
VOA =Amount of volatile organic compounds in g/L of
coating including water and exempt volatile com-pounds,and
W o
=W v –W w –W ex (terms defined as in 10.2.1.N OTE X2.3—Calculation of the amount of volatile organic compound
based on the total volume of coating (including water and exempt volatile compounds),as illustrated in Eq X2.2,does not provide a measure of the amount of VOC that would be released from two coatings used for the same application (that is,to coat the same area to the same dry film thickness assuming the same application efficiency for each coating)when one or both of the coatings contain water or exempt solvents.These units do not identify which of the coatings will release the greater amount of VOC as they treat water and exempt volatile compounds as coating solids.These units,therefore,have not been used,recommended or accepted by U.S.EPA for demonstration of compliance with VOC content regulations as such calculations yield misleading results for coatings that contain water or exempt volatile compounds.
N OTE X2.4—The expression in X2.2is useful for the calculation of the mass of VOC released per unit of time (for example,the mass of VOC per unit of volume including water and exempt volatile compounds times
the
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