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Designation: D2369 – 10

Standard Test Method for

Volatile Content of Coatings1
This standard is issued under the fixed designation D2369; 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 (´) 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 NOTE 3—If unusual decomposition or degradation of the specimen

occurs during heating, the actual time and temperature used to cure the
1.1 This test method describes a procedure for the determi- coating in practice may be substituted for the time and temperature
nation of the weight percent volatile content of solventborne specified in this test method, subject to mutual agreement between the
and waterborne coatings. Test specimens are heated at 110 6 producer and the user. The U.S. EPA Reference Method 24 specifies 110
5°C for 60 min. 6 5°C for 1 h for coatings.
NOTE 4—Practice D3960 for Determining Volatile Organic Compound
NOTE 1—The coatings used in these round-robin studies represented (VOC) Content of Paints and Related Coatings describes procedures and
air-dried, air-dried oxidizing, heat-cured baking systems, and also in- calculations and provides guidance on selecting test methods to determine
cluded multicomponent paint systems. VOC content of solventborne and waterborne coatings.
1.2 Sixty minutes at 110 6 5°C is a general purpose test 1.8 The values stated in SI units are to be regarded as the
method based on the precision obtained with both solventborne standard. The values given in parentheses are for information
and waterborne coatings (see Section 9). only.
1.3 This test method is viable for coatings wherein one or 1.9 This standard does not purport to address all of the
more parts may, at ambient conditions, contain liquid coreac- safety concerns, if any, associated with its use. It is the
tants that are volatile until a chemical reaction has occurred responsibility of the user of this standard to establish appro-
with another component of the multi-package system. priate safety and health practices and determine the applica-
NOTE 2—Committee D01 has run round-robin studies on volatiles of bility of regulatory limitations prior to use.
multicomponent paint systems. The only change in procedure is to premix
the weighed components in the correct proportions and allow the 2. Referenced Documents
specimens to stand at room temperature for 1 h prior to placing them into 2.1 ASTM Standards:2
the oven. D1193 Specification for Reagent Water
1.4 Test Method D5095 for Determination of the Nonvola- D3925 Practice for Sampling Liquid Paints and Related
tile Content in Silanes, Siloxanes and Silane-Siloxane Blends Pigmented Coatings
Used in Masonry Water Repellent Treatments is the standard D3960 Practice for Determining Volatile Organic Com-
method for nonvolatile content of these types of materials. pound (VOC) Content of Paints and Related Coatings
1.5 Test Methods D5403 for Volatile Content of Radiation D5095 Test Method for Determination of the Nonvolatile
Curable Materials is the standard method for determining Content in Silanes, Siloxanes and Silane-Siloxane Blends
nonvolatile content of radiation curable coatings, inks and Used in Masonry Water Repellent Treatments
adhesives. D5403 Test Methods for Volatile Content of Radiation
1.6 Test Method D6419 for Volatile Content of Sheet-Fed Curable Materials
and Coldset Web Offset Printing Inks is the method of choice D6419 Test Method for Volatile Content of Sheet-Fed and
for these types of printing inks. Coldset Web Offset Printing Inks
1.7 This test method may not be applicable to all types of E145 Specification for Gravity-Convection and Forced-
coatings. Other procedures may be substituted with mutual Ventilation Ovens
agreement between the producer and the user. E177 Practice for Use of the Terms Precision and Bias in
ASTM Test Methods
1
This test method is under the jurisdiction of ASTM Committee D01 on Paint
and Related Coatings, Materials, and Applications and is the direct responsibility of
2
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved July 1, 2010. Published September 2010. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1965. Last previous edition approved in 2007 as D2369 – 07. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D2369-10. the ASTM website.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

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 D2369 – 10
E180 Practice for Determining the Precision of ASTM tee on Analytical Reagents of the American Chemical Society,
Methods for Analysis and Testing of Industrial and Spe- where such specifications are available.6 Other grades may be
cialty Chemicals3 used, provided it is first ascertained that the reagent is of
E691 Practice for Conducting an Interlaboratory Study to sufficiently high purity to permit its use without lessening the
Determine the Precision of a Test Method accuracy of the determination.
2.2 Other Standards: 6.2 Purity of Water—Unless otherwise indicated, references
EPA Reference Method 24 Determination of Volatile Matter to water shall be understood to mean Type II of Specification
Content, Density, Volume Solids, and Weight Solids of D1193.
Surface Coatings 4 6.3 Toluene, water or appropriate solvent.

3. Summary of Test Method 7. Procedure

3.1 A designated quantity of coating specimen is weighed 7.1 Take a representative sample of the liquid coating (each
into an aluminum foil dish containing 3 mL of an appropriate component) in accordance with Practice D3925. Mix thor-
solvent, dispersed, and heated in an oven at 110 6 5°C for 60 oughly by hand before taking specimens.
min. The percent volatile is calculated from the loss in weight. 7.2 For multi-component coatings, weigh each component
in the proper proportion into a container that can be capped.
4. Significance and Use
Mix the components together thoroughly by hand before
4.1 This test method is the procedure of choice for deter- extracting specimens. Tightly close the container to prevent
mining volatiles in coatings for the purpose of calculating the loss of volatile materials.
volatile organic content in coatings under specified test condi- 7.3 Weigh the preconditioned aluminum foil dish (see 5.2)
tions. The weight percent solids content (nonvolatile matter) and record the weight to the nearest 0.1 mg (W1). Use
may be determined by difference. This information is useful to disposable (no talc) rubber or polyethylene gloves, tweezers or
the paint producer and user and to environmental interests for forceps to handle the dish.
determining the volatiles emitted by coatings. 7.4 To facilitate dispersing or spreading the specimen, a
metal paper clip may be placed (partially unfolded) in the
5. Apparatus aluminum dish and weighed with the dish. If a paper clip is
5.1 Analytical Balance, capable of weighing 60.1 mg. used, it must remain with the dish throughout the remainder of
5.2 Aluminum Foil Dishes5, 58 mm in diameter by 18 mm the procedure.
high with a smooth (planar) bottom surface. Precondition the 7.5 Add to the aluminum foil dish the appropriate type and
dishes for 30 min in an oven at 110 6 5°C and store in a amount of solvent according to Table 1.
desiccator prior to use. Use tongs or rubber gloves, or both, to 7.6 Draw the coating specimen into the syringe. Remove the
handle the dishes. syringe from the specimen and then pull the plunger tip up 6
5.3 Forced Draft Oven, Type IIA or Type IIB as specified in mm (1⁄4 in.) in order to pull the specimen away from the neck
Specification E145. The oven must be operating in accordance of the syringe. Wipe the outer surface of the syringe to remove
with Specification E145, since it is important to have proper air excess material and cap the syringe. Place the filled syringe on
flow and good temperature control to ensure good precision. the scale and tare the scale. Use disposable (no talc) rubber or
NOTE 5—Be sure the shelves are level and dampers are open. polyethylene gloves to handle the syringe.
7.7 Remove the cap and dispense from the syringe into the
5.4 Syringe, 1-mL without needle, but equipped with caps,
dish the target specimen weight as specified in Table 1. If
capable of properly dispensing the coating under test, at a
solvent is used in the dish add the specimen dropwise to the
sufficient rate so that the specimen can be dissolved in the
solvent-containing dish. The paper clip may be used to help
solvent.
disperse the coating specimen in the solvent. If the material
NOTE 6—Disposable syringes with caps are recommended. forms a lump that cannot be dispersed, discard the specimen
5.5 Paper Clips. and prepare a new one. If no solvent is used (see Table 1,
Method E), spread out the specimen in the dish with the paper
6. Reagents clip to cover the bottom of the dish completely with as uniform
6.1 Purity of Reagents—Reagent grade chemicals shall be thickness as possible.
used in all tests. Unless otherwise indicated, it is intended that 7.8 After dispensing the specimen, do not wipe the tip of the
all reagents shall conform to the specifications of the Commit- syringe. Remove the specimen from the neck of the syringe by
pulling up the plunger. Cap and place the syringe on the
balance (that was tared with the syringe before the specimen
3
Withdrawn. The last approved version of this historical standard is referenced
on www.astm.org.
4
Available from U.S. Government Printing Office Superintendent of Documents,
6
732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http:// Reagent Chemicals, American Chemical Society Specifications, American
www.access.gpo.gov. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
5
Available from Fisher, Disposable Aluminum Dishes (code 08–732–106), listed by the American Chemical Society, see Analar Standards for Laboratory
www.fishersci.com; McAlister Bicknell, Aluminum Weighing Dishes (code Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
10676–0000), www.mbcoct.com; Cole-Parmer, Disposable Aluminum Weigh and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Dishes (code EW-01017–44), www.coleparmer.com. MD.

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 D2369 – 10
TABLE 1 Summary of Methods
Method A – Method B – Method C – Method D – Method E –
Coating Type One Component One Component Mulit-Component Mulit-Component Mulit-Component
Waterborne Solventborne Waterborne Solventborne >90 % Solids
Solvent Type and Amount 3 6 1 ml water (6.2) 3 6 1 ml solvent (6.3) 3 6 1 ml water (6.2) 3 6 1 ml solvent (6.3) none

Specimen Weight 0.3 6 0.1 g if expected result is =<40 % volatile (>=60 % non-volatile) seeA
0.5 6 0.1 g if expected result is >40 % volatile (<60 % non-volatile)

Induction Time N/A N/A 1 hr (seeB) 1 hr (seeB) 24 hr

A
Specimen weight to be representative of how the product is used (the lowest thickness which the manufacturer’s literature recommends) where: Weight (g) = Thickness
(mm) 3 3.14 3 [Dish Diameter2(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 mm
diameter dish at a thickness of 0.5 mm calculates to 1.0 g.
B
Other induction periods are used. See EPA Reference Method 24.

was dispensed) and record the weight to the nearest 0.1 mg as 9. Precision and Bias
the Specimen Weight (SA). 9.1 The precision estimated for tests at 60 min at 110 6 5°C
7.9 Repeat steps 7.3-7.8 to prepare a duplicate specimen for are based on an interlaboratory study7 in which 1 operator in
each sample. each of 15 laboratories analyzed in duplicate on 2 different
7.10 For multi-component coatings, after the specimens are days 7 samples of waterborne paints and 8 samples of
prepared, allow them to sit at ambient conditions for a solventborne paints containing between 35 and 72 % volatile
prescribed induction time according to Table 1 before placing material. The paints were commercially supplied. The results
the dishes in the oven. were analyzed statistically in accordance with Practice E180.
7.11 Heat the aluminum foil dishes containing the speci- The within-laboratory coefficient of variation was found to be
mens in the forced draft oven (5.3) for 60 min at 110 6 5°C. 0.5 % relative at 213 df and the between-laboratories coeffi-
7.12 Remove each dish from the oven, place immediately in cient of variation was 1.7 % relative at 198 df. Based on these
a desiccator, cool to ambient temperature, weigh to the nearest coefficients, the following criteria should be used for judging
0.1 mg and record this weight (W2) for each specimen. the acceptability of results at the 95 % confidence level.
9.1.1 Repeatability—Two results, each the mean of dupli-
8. Calculation cate determinations, obtained by the same operator on different
8.1 Calculate the percent volatile matter, V, in the liquid days should be considered suspect if they differ by more than
coating as follows: 1.5 % relative.
VA 5 100 2 [~~W 2 2 W1!/SA! 3 100] (1) 9.1.2 Reproducibility—Two results, each the mean of dupli-
cate determinations, obtained by operators in different labora-
where: tories should be considered suspect if they differ by more than
VA = % volatiles (first determination), 4.7 % relative.
W1 = weight of dish, 9.2 Bias—Bias has not been determined.
W2 = weight of dish plus specimen after heating, 9.3 The precision results for multicomponent systems are
SA = specimen weight, and based on an interlaboratory study in which one operator in each
VB = % volatiles (duplicate determination, calculate in of five laboratories analyzed in duplicate on two different days,
same manner as VA). four samples of commercially supplied solventborne and
V 5 ~VA 1 VB!/2 (2) waterborne multicomponent systems. The results were ana-
8.2 Report V, the mean of the duplicate determination if lyzed statistically in accordance with Practice E180.
relative percent difference is 1.5 % or less. If relative difference 9.3.1 Repeatability for Solventborne Multicomponent Sys-
between VA and VB is greater than 1.5 %, repeat the duplicate tems:
determinations. The 1.5 % relative difference is not applicabe Coefficient of variation 0.5 %
Degrees of freedom 6
to Method E. Factor (based on 95 % confidence level) 3.46
8.3 The percent of nonvolatile matter, N, in the coating may Precision 1.74 %
be calculated by difference as follows:
Two results, each the mean of duplicate determinations
N 5 ~NA 1 NB!/2 (3) obtained by the same operator on different days, should be
considered suspect if they vary by more than 1.74 % relative.
where:
NA = 100 − VA, and
NB = 100 − VB.
NA represents first determination and NB represents duplicate 7
Supporting data have been filed at ASTM International Headquarters and may
determination. be obtained by requesting Research Report RR:D01-1026.

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 D2369 – 10
TABLE 2 ILS Summary for Method E – % Volatile Material (V)A
Repeatability Reproducibility
Repeatability Reproducibility
Material AverageB Standard Standard
Limit Limit
Deviation Deviation
V (%) sr sR r R
A 3.25 0.17 1.15 0.47 3.21
B 1.87 0.15 0.34 0.41 0.95
C 2.67 0.18 1.59 0.52 4.46
D 0.64 0.12 0.20 0.32 0.56
E 0.15 0.05 0.11 0.14 0.30
A
The differences in the precision between the different materials (types of coatings) tested in this study are not due to the specific chemistry or class of material but
are attributed to the specific formulations and components.
B
The average of the laboratories’ calculated averages.

9.3.2 Reproducibility for Solventborne Multicomponent Sys- tory shall be judged not equivalent if they differ by more than
tems: the “r” value for that material; “r” is the interval representing
Coefficient of variation 1.46 % the critical difference between two test results for the same
Degrees of freedom 5 material, obtained by the same operator using the same
Factor (based on 95 % confidence level) 3.46
Precision 5.31 %
equipment on the same day in the same laboratory.
9.5.1.1 Repeatability limits for each of the materials tested
Two results, each the mean of duplicate determinations
are listed in Table 2.
obtained by operators in different laboratories, should be
considered suspect if they vary by more than 5.31 % relative. 9.5.2 Reproducibility Limit (R)—Two test results, each the
9.3.3 Repeatability for Waterborne Multicomponent Sys- mean of duplicate determinations, between different laborato-
tems: ries shall be judged not equivalent if they differ by more than
the “R” value for that material; “R” is the interval representing
Coefficient of variation 0.53 %
Degrees of freedom 6 the critical difference between two test results for the same
Factor (based on 95 % confidence level) 3.46 material, obtained by different operators using different equip-
Precision 1.84 %
ment in different laboratories.
Two results, each the mean of duplicate determinations 9.5.2.1 Reproducibility limits for each of the metals tested
obtained by the same operator on different days, should be are listed in Table 2.
considered suspect if they vary by more than 1.84 % relative. 9.5.3 The above terms (repeatability limit and reproducibil-
9.3.4 Reproducibility for Waterborne Multicomponent Sys- ity limit) are used as specified in Practice E177.
tems:
9.5.4 Any judgment in accordance with statements 9.5.1
Coefficient of variation 0.94 %
Degrees of freedom 5
and 9.5.2 would have an approximate 95 % probability of
Factor (based on 95 % confidence level) 3.64 being correct.
Precision 3.43 % 9.5.5 The precision statement for Method E for Multi-
Two results, each the mean of duplicate determinations Component, >90 % Solids Systems was determined through
obtained by operators in different laboratories, should be statistical examination of 120 reported results, from eight
considered suspect if they vary by more then 3.43 % relative. laboratories, on five materials, which were identified as:
9.4 Bias—Since there is no accepted standard for volatile A – Two component amine cured epoxy clear coating
content in coatings, bias cannot be determined. B – Two component amine cured epoxy pigmented coating
9.5 Precision for Multi-Component, >90 % Solids
C – Two component urethane pigmented coating
Systems—The precision of this test was expanded to include
data and analysis from Method E based on an interlaboratory D – Two component urethane waterproofing membrane
study conducted in 2009. Each of eight laboratories tested five coating
different materials, all multi-component, >90 % solids systems. E – Two component amine cured epoxy/acrylate highway
Every “test result” represents the mean of duplicate determi- marking coating
nations. Every laboratory reported three replicate test results 9.6 Bias—At the time of the study, there was no accepted
for the analysis. Practice E691 was followed for the design and reference material or method suitable for determining the bias
analysis of the data; the details are given in ASTM Research for this test method, therefore no statement on bias is being
Report D01–1152.8 made.
9.5.1 Repeatability Limit (r)—Two test results, each the
mean of duplicate determinations, obtained within one labora- 10. Keywords
10.1 multicomponent paints; nonvolatile determination;
8
Supporting data have been filed at ASTM International Headquarters and may VOC baking temperature; VOC in paints; volatile determina-
be obtained by requesting Research Report RR:D01-1152. tion; volatiles

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 D2369 – 10
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