Designation: D2369 − 10 (Reapproved 2015)´1

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 U.S. Department of Defense.

ε1 NOTE—Paragraph 9.3.2 was editorially corrected in June 2015.

1. Scope 1.7 This test method may not be applicable to all types of
coatings. Other procedures may be substituted with mutual
1.1 This test method describes a procedure for the determi-
agreement between the producer and the user.
nation of the weight percent volatile content of solventborne
and waterborne coatings. Test specimens are heated at 110 6 NOTE 3—If unusual decomposition or degradation of the specimen
5°C for 60 min. occurs during heating, the actual time and temperature used to cure the
coating in practice may be substituted for the time and temperature
NOTE 1—The coatings used in these round-robin studies represented specified in this test method, subject to mutual agreement between the
air-dried, air-dried oxidizing, heat-cured baking systems, and also in- producer and the user. The U.S. EPA Reference Method 24 specifies 110
cluded multicomponent paint systems. 6 5°C for 1 h for coatings.
NOTE 4—Practice D3960 for Determining Volatile Organic Compound
1.2 Sixty minutes at 110 6 5°C is a general purpose test (VOC) Content of Paints and Related Coatings describes procedures and
method based on the precision obtained with both solventborne calculations and provides guidance on selecting test methods to determine
and waterborne coatings (see Section 9). VOC content of solventborne and waterborne coatings.
1.8 The values stated in SI units are to be regarded as
1.3 This test method is viable for coatings wherein one or
standard. No other units of measurement are included in this
more parts may, at ambient conditions, contain liquid coreac-
standard.
tants that are volatile until a chemical reaction has occurred
with another component of the multi-package system. 1.9 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
NOTE 2—Committee D01 has run round-robin studies on volatiles of responsibility of the user of this standard to establish appro-
multicomponent paint systems. The only change in procedure is to premix priate safety and health practices and determine the applica-
the weighed components in the correct proportions and allow the
specimens to stand at room temperature for 1 h prior to placing them into bility of regulatory limitations prior to use.
the oven.
2. Referenced Documents
1.4 Test Method D5095 for Determination of the Nonvola-
tile Content in Silanes, Siloxanes and Silane-Siloxane Blends 2.1 ASTM Standards:2
Used in Masonry Water Repellent Treatments is the standard D1193 Specification for Reagent Water
method for nonvolatile content of these types of materials. D3925 Practice for Sampling Liquid Paints and Related
Pigmented Coatings
1.5 Test Methods D5403 for Volatile Content of Radiation D3960 Practice for Determining Volatile Organic Compound
Curable Materials is the standard method for determining (VOC) Content of Paints and Related Coatings
nonvolatile content of radiation curable coatings, inks and D5095 Test Method for Determination of the Nonvolatile
adhesives. Content in Silanes, Siloxanes and Silane-Siloxane Blends
1.6 Test Method D6419 for Volatile Content of Sheet-Fed Used in Masonry Water Repellent Treatments
and Coldset Web Offset Printing Inks is the method of choice D5403 Test Methods for Volatile Content of Radiation Cur-
for these types of printing inks. able Materials
D6419 Test Method for Volatile Content of Sheet-Fed and
Coldset Web Offset Printing Inks
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 June 1, 2015. Published June 2015. Originally contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
approved in 1965. Last previous edition approved in 2010 as D2369 – 10ε1. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D2369-10R15E01. the ASTM website.

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

1
 D2369 − 10 (2015)´1
E145 Specification for Gravity-Convection and Forced- 6. Reagents
Ventilation Ovens 6.1 Purity of Reagents—Reagent grade chemicals shall be
E177 Practice for Use of the Terms Precision and Bias in used in all tests. Unless otherwise indicated, it is intended that
ASTM Test Methods all reagents shall conform to the specifications of the Commit-
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 Chemicals (Withdrawn 2009)3 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
3.1 A designated quantity of coating specimen is weighed 7. Procedure
into an aluminum foil dish containing 3 mL of an appropriate 7.1 Take a representative sample of the liquid coating (each
solvent, dispersed, and heated in an oven at 110 6 5°C for 60 component) in accordance with Practice D3925. Mix thor-
min. The percent volatile is calculated from the loss in weight. oughly by hand before taking specimens.
4. Significance and Use 7.2 For multi-component coatings, weigh each component
in the proper proportion into a container that can be capped.
4.1 This test method is the procedure of choice for deter- Mix the components together thoroughly by hand before
mining volatiles in coatings for the purpose of calculating the extracting specimens. Tightly close the container to prevent
volatile organic content in coatings under specified test condi- loss of volatile materials.
tions. The weight percent solids content (nonvolatile matter)
may be determined by difference. This information is useful to 7.3 Weigh the preconditioned aluminum foil dish (see 5.2)
the paint producer and user and to environmental interests for and record the weight to the nearest 0.1 mg (W1). Use
determining the volatiles emitted by coatings. disposable (no talc) rubber or polyethylene gloves, tweezers or
forceps to handle the dish.
5. Apparatus 7.4 To facilitate dispersing or spreading the specimen, a
5.1 Analytical Balance, capable of weighing 60.1 mg. metal paper clip may be placed (partially unfolded) in the
aluminum dish and weighed with the dish. If a paper clip is
5.2 Aluminum Foil Dishes5, 58 mm in diameter by 18 mm used, it must remain with the dish throughout the remainder of
high with a smooth (planar) bottom surface. Precondition the the procedure.
dishes for 30 min in an oven at 110 6 5°C and store in a
desiccator prior to use. Use tongs or rubber gloves, or both, to 7.5 Add to the aluminum foil dish the appropriate type and
handle the dishes. amount of solvent according to Table 1.
5.3 Forced Draft Oven, Type IIA or Type IIB as specified in 7.6 Draw the coating specimen into the syringe. Remove the
Specification E145. The oven must be operating in accordance syringe from the specimen and then pull the plunger tip up 6
with Specification E145, since it is important to have proper air mm (1⁄4 in.) in order to pull the specimen away from the neck
flow and good temperature control to ensure good precision. of the syringe. Wipe the outer surface of the syringe to remove
excess material and cap the syringe. Place the filled syringe on
NOTE 5—Be sure the shelves are level and dampers are open. the scale and tare the scale. Use disposable (no talc) rubber or
5.4 Syringe, 1-mL without needle, but equipped with caps, polyethylene gloves to handle the syringe.
capable of properly dispensing the coating under test, at a
7.7 Remove the cap and dispense from the syringe into the
sufficient rate so that the specimen can be dissolved in the
dish the target specimen weight as specified in Table 1. If
solvent.
solvent is used in the dish add the specimen dropwise to the
NOTE 6—Disposable syringes with caps are recommended. solvent-containing dish. The paper clip may be used to help
5.5 Paper Clips. disperse the coating specimen in the solvent. If the material
forms a lump that cannot be dispersed, discard the specimen
and prepare a new one. If no solvent is used (see Table 1,
3
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 (2015)´1
TABLE 1 Summary of Methods
Method A – Method B – Method C – Method D – Method E –
Coating Type One Component One Component Multi-Component Multi-Component Multi-Component
Waterborne Solventborne Waterborne Solventborne >90 % Solids
Solvent Type and Amount 3 ± 1 ml water (6.2) 3 ± 1 ml solvent (6.3) 3 ± 1 ml water (6.2) 3 ± 1 ml solvent (6.3) none

Specimen Weight 0.3 ± 0.1 g if expected result is =<40 % volatile (>=60 % non-volatile) seeA
0.5 ± 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) × 3.14 × [Dish Diameter2 (mm2)/4] × 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.

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

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 D2369 − 10 (2015)´1
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.

Two results, each the mean of duplicate determinations 9.5.1 Repeatability Limit (r)—Two test results, each the
obtained by the same operator on different days, should be mean of duplicate determinations, obtained within one labora-
considered suspect if they vary by more than 1.74 % relative. tory shall be judged not equivalent if they differ by more than
9.3.2 Reproducibility for Solventborne Multicomponent Sys- the “r” value for that material; “r” is the interval representing
tems: the critical difference between two test results for the same
Coefficient of variation 1.46 % material, obtained by the same operator using the same
Degrees of freedom 5 equipment on the same day in the same laboratory.
Factor (based on 95 % confidence level) 3.64
Precision 5.31 % 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 9.5.2 Reproducibility Limit (R)—Two test results, each the
considered suspect if they vary by more than 5.31 % relative. mean of duplicate determinations, between different laborato-
9.3.3 Repeatability for Waterborne Multicomponent Sys- ries 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 0.53 % the critical difference between two test results for the same
Degrees of freedom 6 material, obtained by different operators using different equip-
Factor (based on 95 % confidence level) 3.46
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 % and 9.5.2 would have an approximate 95 % probability of
Degrees of freedom 5 being correct.
Factor (based on 95 % confidence level) 3.64
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:
A – Two component amine cured epoxy clear coating
9.4 Bias—Since there is no accepted standard for volatile
B – Two component amine cured epoxy pigmented coating
content in coatings, bias cannot be determined.
C – Two component urethane pigmented coating
9.5 Precision for Multi-Component, >90 % Solids D – Two component urethane waterproofing membrane
Systems—The precision of this test was expanded to include coating
data and analysis from Method E based on an interlaboratory E – Two component amine cured epoxy/acrylate highway
study conducted in 2009. Each of eight laboratories tested five marking coating
different materials, all multi-component, >90 % solids systems.
Every “test result” represents the mean of duplicate determi- 9.6 Bias—At the time of the study, there was no accepted
nations. Every laboratory reported three replicate test results reference material or method suitable for determining the bias
for the analysis. Practice E691 was followed for the design and for this test method, therefore no statement on bias is being
analysis of the data; the details are given in ASTM Research made.
Report RR:D01-1152.8
10. Keywords
8
10.1 multicomponent paints; nonvolatile determination;
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D01-1152. Contact ASTM Customer VOC baking temperature; VOC in paints; volatile determina-
Service at [email protected]. tion; volatiles

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 D2369 − 10 (2015)´1
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