ASTM D2369-24
(Test Method)Standard Test Method for Volatile Content of Coatings
Standard Test Method for Volatile Content of Coatings
SIGNIFICANCE AND USE
4.1 This test method is the procedure of choice for determining volatiles in coatings for the purpose of calculating the volatile organic content in coatings under specified test conditions. The weight percent solids content (nonvolatile matter) may be determined by difference. This information is useful to the paint producer and user and to environmental interests for determining the volatiles emitted by coatings.
SCOPE
1.1 This test method describes a procedure for the determination of the weight percent volatile content of solventborne and waterborne coatings. Test specimens are heated at 110 °C ± 5 °C for 60 min.
Note 1: The coatings used in these round-robin studies represented air-dried, air-dried oxidizing, heat-cured baking systems, and also included multicomponent paint systems.
1.2 Sixty minutes at 110 °C ± 5 °C is a general purpose test method based on the precision obtained with both solventborne and waterborne coatings (see Section 9).
1.3 This test method is viable for coatings wherein one or more parts may, at ambient conditions, contain liquid coreactants that are volatile until a chemical reaction has occurred with another component of the multi-package system.
Note 2: Committee D01 has run round-robin studies on volatiles of multicomponent paint systems. The only change in procedure is to premix the weighed components in the correct proportions and allow the specimens to stand at room temperature for 1 h prior to placing them into the oven.
1.4 Test Method D5095 for Determination of the Nonvolatile Content in Silanes, Siloxanes and Silane-Siloxane Blends Used in Masonry Water Repellent Treatments is the standard method for nonvolatile content of these types of materials.
1.5 Test Methods D5403 for Volatile Content of Radiation Curable Materials is the standard method for determining nonvolatile content of radiation curable coatings, inks and adhesives.
1.6 Test Method D6419 for Volatile Content of Sheet-Fed and Coldset Web Offset Printing Inks is the method of choice for these types of printing inks.
1.7 This test method may not be applicable to all types of coatings. Other procedures may be substituted with mutual agreement between the producer and the user.
Note 3: If unusual decomposition or degradation of the specimen occurs during heating, the actual time and temperature used to cure the coating in practice may be substituted for the time and temperature specified in this test method, subject to mutual agreement between the producer and the user. The U.S. EPA Reference Method 24 specifies 110 °C ± 5 °C for 1 h for coatings.
Note 4: Practice D3960 for Determining Volatile Organic Compound (VOC) Content of Paints and Related Coatings describes procedures and calculations and provides guidance on selecting test methods to determine VOC content of solventborne and waterborne coatings.
1.8 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.9 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.10 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
General Information
Relations
Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D2369 − 24
Standard Test Method for
Volatile Content of Coatings
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.
NOTE 3—If unusual decomposition or degradation of the specimen
1. Scope
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
producer and the user. The U.S. EPA Reference Method 24 specifies
and waterborne coatings. Test specimens are heated at 110 °C
110 °C 6 5 °C for 1 h for coatings.
6 5 °C for 60 min.
NOTE 4—Practice D3960 for Determining Volatile Organic Compound
(VOC) Content of Paints and Related Coatings describes procedures and
NOTE 1—The coatings used in these round-robin studies represented
calculations and provides guidance on selecting test methods to determine
air-dried, air-dried oxidizing, heat-cured baking systems, and also in-
VOC content of solventborne and waterborne coatings.
cluded multicomponent paint systems.
1.8 The values stated in SI units are to be regarded as
1.2 Sixty minutes at 110 °C 6 5 °C is a general purpose test
standard. No other units of measurement are included in this
method based on the precision obtained with both solventborne
standard.
and waterborne coatings (see Section 9).
1.9 This standard does not purport to address all of the
1.3 This test method is viable for coatings wherein one or
safety concerns, if any, associated with its use. It is the
more parts may, at ambient conditions, contain liquid coreac-
responsibility of the user of this standard to establish appro-
tants that are volatile until a chemical reaction has occurred
priate safety, health, and environmental practices and deter-
with another component of the multi-package system.
mine the applicability of regulatory limitations prior to use.
NOTE 2—Committee D01 has run round-robin studies on volatiles of
1.10 This international standard was developed in accor-
multicomponent paint systems. The only change in procedure is to premix
dance with internationally recognized principles on standard-
the weighed components in the correct proportions and allow the
ization established in the Decision on Principles for the
specimens to stand at room temperature for 1 h prior to placing them into
the oven.
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
1.4 Test Method D5095 for Determination of the Nonvola-
Barriers to Trade (TBT) Committee.
tile Content in Silanes, Siloxanes and Silane-Siloxane Blends
Used in Masonry Water Repellent Treatments is the standard
2. Referenced Documents
method for nonvolatile content of these types of materials.
2.1 ASTM Standards:
1.5 Test Methods D5403 for Volatile Content of Radiation
D1193 Specification for Reagent Water
Curable Materials is the standard method for determining
D3925 Practice for Sampling Liquid Paints and Related
nonvolatile content of radiation curable coatings, inks and
Pigmented Coatings
adhesives.
D3960 Practice for Determining Volatile Organic Compound
1.6 Test Method D6419 for Volatile Content of Sheet-Fed
(VOC) Content of Paints and Related Coatings
and Coldset Web Offset Printing Inks is the method of choice
D5095 Test Method for Determination of the Nonvolatile
for these types of printing inks.
Content in Silanes, Siloxanes and Silane-Siloxane Blends
Used in Masonry Water Repellent Treatments
1.7 This test method may not be applicable to all types of
D5403 Test Methods for Volatile Content of Radiation Cur-
coatings. Other procedures may be substituted with mutual
able Materials
agreement between the producer and the user.
D6419 Test Method for Volatile Content of Sheet-Fed and
Coldset Web Offset Printing Inks
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
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 Feb. 1, 2024. Published February 2024. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1965. Last previous edition approved in 2020 as D2369 – 20. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D2369-24. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D2369 − 24
E145 Specification for Gravity-Convection and Forced- 5.3.2 Time Constant: the time required for the oven to
Ventilation Ovens return to setpoint temperature after opening oven door. The
E177 Practice for Use of the Terms Precision and Bias in oven must recover to the setpoint temp of 110 °C within 5
ASTM Test Methods minutes of leaving oven door open for 30 seconds.
E180 Practice for Determining the Precision of ASTM 5.3.3 Air Exchanges: how often fresh laboratory air is
Methods for Analysis and Testing of Industrial and Spe- introduced into the oven chamber. The oven must operate at ≥
cialty Chemicals (Withdrawn 2009) 50 air exchanges per hour.
E691 Practice for Conducting an Interlaboratory Study to
5.4 Each specification should be certified by the oven
Determine the Precision of a Test Method
manufacturer, confirmed by the user, or tested by a qualified
2.2 Other Standards:
third party. Evaluation of oven specifications should be per-
EPA Reference Method 24 Determination of Volatile Matter
formed according to the procedures outlined in Specification
Content, Density, Volume Solids, and Weight Solids of
E145.
Surface Coatings
NOTE 5—Be sure the shelves are level and dampers are open.
5.5 Syringe, 1 mL without needle, but equipped with caps,
3. Summary of Test Method
capable of properly dispensing the coating under test, at a
3.1 A designated quantity of coating specimen is weighed sufficient rate so that the specimen can be dissolved in the
into an aluminum foil dish containing 3 mL of an appropriate
solvent.
solvent, dispersed, and heated in an oven at 110 °C 6 5 °C for
NOTE 6—Disposable syringes with caps are recommended.
60 min. The percent volatile is calculated from the loss in
5.6 Paper Clips.
weight.
6. Reagents
4. Significance and Use
6.1 Purity of Reagents—Reagent grade chemicals shall be
4.1 This test method is the procedure of choice for deter-
used in all tests. Unless otherwise indicated, it is intended that
mining volatiles in coatings for the purpose of calculating the
all reagents shall conform to the specifications of the Commit-
volatile organic content in coatings under specified test condi-
tee on Analytical Reagents of the American Chemical Society,
tions. The weight percent solids content (nonvolatile matter)
where such specifications are available. Other grades may be
may be determined by difference. This information is useful to
used, provided it is first ascertained that the reagent is of
the paint producer and user and to environmental interests for
sufficiently high purity to permit its use without lessening the
determining the volatiles emitted by coatings.
accuracy of the determination.
5. Apparatus
6.2 Purity of Water—Unless otherwise indicated, references
to water shall be understood to mean Type II of Specification
5.1 Analytical Balance, capable of weighing 60.1 mg.
D1193.
5.2 Aluminum Foil Dishes , 58 mm in diameter by 18 mm
6.3 Toluene, water or appropriate solvent.
high with a smooth (planar) bottom surface. Precondition the
dishes for 30 min in an oven at 110 °C 6 5 °C and store in a
7. Procedure
desiccator prior to use. Use tongs or rubber gloves, or both, to
handle the dishes.
7.1 Take a representative sample of the liquid coating (each
component) in accordance with Practice D3925. Mix thor-
5.3 Forced Draft Oven, Proper air flow and temperature
oughly by hand before taking specimens.
control are critical for good precision, while adequate air
exchange minimizes accumulation of flammable solvent va-
7.2 For multi-component coatings, weigh each component
pors. The forced draft oven must operate in accordance with
in the proper proportion into a container that can be capped.
the following specifications:
Mix the components together thoroughly by hand before
5.3.1 Temperature Uniformity: the consistency of heating
extracting specimens. Tightly close the container to prevent
throughout the oven chamber. The oven must achieve a
loss of volatile materials.
temperature uniformity of ≤ 4.0 °C at 110 °C and temperature
NOTE 7—Manufacturers often specify mix ratios by volume. To
controller stability of ≤ 1.0 °C. Temperature controller stability
minimize errors, prepare the mixture gravimetrically using the measured
is the difference between the load temperature and setpoint
density of each component to convert volume to mass. The calculated
temperature over time.
mass and prepared mass should differ by no more than 0.1 % relative.
7.3 Weigh the preconditioned aluminum foil dish (see 5.2)
and record the weight to the nearest 0.1 mg (W ). Use
The last approved version of this historical standard is referenced on
www.astm.org.
Available from U.S. Government Printing Office Superintendent of Documents,
732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http:// ACS Reagent Chemicals, Specifications and Procedures for Reagents and
www.access.gpo.gov. Standard-Grade Reference Materials, American Chemical Society, Washington,
Available from Fisher, Disposable Aluminum Dishes (code 08–732–106), DC. For suggestions on the testing of reagents not listed by the American Chemical
www.fishersci.com; McAlister Bicknell, Aluminum Weighing Dishes (code Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,
10676–0000), www.mbcoct.com; Cole-Parmer, Disposable Aluminum Weigh U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma-
Dishes (code EW-01017–44), www.coleparmer.com. copeial Convention, Inc. (USPC), Rockville, MD.
D2369 − 24
disposable (no talc) rubber or polyethylene gloves, tweezers or prescribed induction time according to Table 1 before placing
forceps to handle the dish. the dishes in the oven.
7.4 To facilitate dispersing or spreading the specimen, a
7.11 Heat the aluminum foil dishes containing the speci-
metal paper clip may be placed (partially unfolded) in the
mens in the forced draft oven (5.3) for 60 min at 110 °C 6
aluminum dish and weighed with the dish. If a paper clip is
5 °C.
used, it must remain with the dish throughout the remainder of
7.12 Remove each dish from the oven, place immediately in
the procedure.
a desiccator, cool to ambient temperature, weigh to the nearest
7.5 Add to the aluminum foil dish the appropriate type and
0.1 mg and record this weight (W ) for each specimen.
amount of solvent according to Table 1.
7.6 Draw the coating specimen into the syringe. Remove the
8. Calculation
syringe from the specimen and then pull the plunger tip up 6
8.1 Calculate the percent volatile matter, V, in the liquid
mm ( ⁄4 in.) in order to pull the specimen away from the neck
of the syringe. Wipe the outer surface of the syringe to remove coating as follows:
excess material and cap the syringe. Place the filled syringe on
V 5 100 2 @~~W 2 W !/S ! × 100# (1)
A 2 1 A
the scale and tare the scale. Use disposable (no talc) rubber or
where:
polyethylene gloves to handle the syringe.
V = % volatiles (first determination),
A
7.7 Remove the cap and dispense from the syringe into the
W = weight of dish,
dish the target specimen weight as specified in Table 1. If
W = weight of dish plus specimen after heating,
solvent is used in the dish add the specimen dropwise to the
S = specimen weight, and
A
solvent-containing dish. The paper clip may be used to help
V = % volatiles (duplicate determination, calculate in same
B
disperse the coating specimen in the solvent. If the material
manner as V ).
A
forms a lump that cannot be dispersed, discard the specimen
V 5 ~V 1V !/2 (2)
and prepare a new one. If no solvent is used (see Table 1, A B
Method E), spread out the specimen in the dish with the paper
8.2 Report V, the mean of the duplicate determination if
clip to cover the bottom of the dish completely with as uniform
relative percent difference is 1.5 % or less. If relative difference
thickness as possible.
between V and V is greater than 1.5 %, repeat the duplicate
A B
7.8 After dispensing the specimen, do not wipe the tip of the
determinations. The 1.5 % relative difference is not applicable
syringe. Remove the specimen from the neck of the syringe by
to Method E; see requirements in Table 2 and 9.5.
pulling up the plunger. Cap and place the syringe on the
8.3 The percent of nonvolatile matter, N, in the coating may
balance (that was tared with the syringe before the specimen
be calculated by difference as follows:
was dispensed) and record the weight to the nearest 0.1 mg as
the Specimen Weight (S ).
A N 5 ~N 1N !/2 (3)
A B
7.9 Repeat steps 7.3 – 7.8 to prepare a duplicate specimen
where:
for each sample.
N = 100 − V , and
A A
NOTE 8—Duplicate determinations must meet the relative percent
N = 100 − V .
B B
difference requirements detailed in 8.2.
N represents first determination and N represents duplicate
A B
7.10 For multi-component coatings, after the specimens are
determination.
prepared, allow them to sit at ambient conditions for a
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 ml ± 1 ml water (6.2) 3 ml ± 1 ml solvent (6.3) 3 ml ± 1 ml water (6.2) 3 ml ± 1 ml solvent none
(6.3)
A
Specimen Weight 0.3 g ± 0.1 g if expected result is =<40 % volatile (>=60 % non-volatile) see
0.5 g ± 0.1 g if expected result is >40 % volatile (<60 % non-volatile)
B B
Induction Time N/A N/A 1 hr (see ) 1 hr (see ) 24
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D2369 − 20 D2369 − 24
Standard Test Method for
Volatile Content of Coatings
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.
1. Scope
1.1 This test method describes a procedure for the determination of the weight percent volatile content of solventborne and
waterborne coatings. Test specimens are heated at 110 6 5°C for 110 °C 6 5 °C for 60 min.
NOTE 1—The coatings used in these round-robin studies represented air-dried, air-dried oxidizing, heat-cured baking systems, and also included
multicomponent paint systems.
1.2 Sixty minutes at 110 6 5°C110 °C 6 5 °C is a general purpose test method based on the precision obtained with both
solventborne and waterborne coatings (see Section 9).
1.3 This test method is viable for coatings wherein one or more parts may, at ambient conditions, contain liquid coreactants that
are volatile until a chemical reaction has occurred with another component of the multi-package system.
NOTE 2—Committee D01 has run round-robin studies on volatiles of multicomponent paint systems. The only change in procedure is to premix the
weighed components in the correct proportions and allow the specimens to stand at room temperature for 1 h prior to placing them into the oven.
1.4 Test Method D5095 for Determination of the Nonvolatile Content in Silanes, Siloxanes and Silane-Siloxane Blends Used in
Masonry Water Repellent Treatments is the standard method for nonvolatile content of these types of materials.
1.5 Test Methods D5403 for Volatile Content of Radiation Curable Materials is the standard method for determining nonvolatile
content of radiation curable coatings, inks and adhesives.
1.6 Test Method D6419 for Volatile Content of Sheet-Fed and Coldset Web Offset Printing Inks is the method of choice for these
types of printing inks.
1.7 This test method may not be applicable to all types of coatings. Other procedures may be substituted with mutual agreement
between the producer and the user.
NOTE 3—If unusual decomposition or degradation of the specimen occurs during heating, the actual time and temperature used to cure the coating in
practice may be substituted for the time and temperature specified in this test method, subject to mutual agreement between the producer and the user.
The U.S. EPA Reference Method 24 specifies 110 6 5°C 110 °C 6 5 °C for 1 h for coatings.
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
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.
Current edition approved June 1, 2020Feb. 1, 2024. Published July 2020February 2024. Originally approved in 1965. Last previous edition approved in 20152020 as
ε1
D2369 – 10 (2015)D2369 – 20. . DOI: 10.1520/D2369-20.10.1520/D2369-24.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D2369 − 24
NOTE 4—Practice D3960 for Determining Volatile Organic Compound (VOC) Content of Paints and Related Coatings describes procedures and
calculations and provides guidance on selecting test methods to determine VOC content of solventborne and waterborne coatings.
1.8 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.9 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of
regulatory limitations prior to use.
1.10 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
D1193 Specification for Reagent Water
D3925 Practice for Sampling Liquid Paints and Related Pigmented Coatings
D3960 Practice for Determining Volatile Organic Compound (VOC) Content of Paints and Related Coatings
D5095 Test Method for Determination of the Nonvolatile Content in Silanes, Siloxanes and Silane-Siloxane Blends Used in
Masonry Water Repellent Treatments
D5403 Test Methods for Volatile Content of Radiation Curable Materials
D6419 Test Method for Volatile Content of Sheet-Fed and Coldset Web Offset Printing Inks
E145 Specification for Gravity-Convection and Forced-Ventilation Ovens
E177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
E180 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial and Specialty Chemicals
(Withdrawn 2009)
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
2.2 Other Standards:
EPA Reference Method 24 Determination of Volatile Matter Content, Density, Volume Solids, and Weight Solids of Surface
Coatings
3. Summary of Test Method
3.1 A designated quantity of coating specimen is weighed into an aluminum foil dish containing 3 mL of an appropriate solvent,
dispersed, and heated in an oven at 110 6 5°C110 °C 6 5 °C for 60 min. The percent volatile is calculated from the loss in weight.
4. Significance and Use
4.1 This test method is the procedure of choice for determining volatiles in coatings for the purpose of calculating the volatile
organic content in coatings under specified test conditions. The weight percent solids content (nonvolatile matter) may be
determined by difference. This information is useful to the paint producer and user and to environmental interests for determining
the volatiles emitted by coatings.
5. Apparatus
5.1 Analytical Balance, capable of weighing 60.1 mg.
5.2 Aluminum Foil Dishes , 58 mm in diameter by 18 mm high with a smooth (planar) bottom surface. Precondition the dishes
for 30 min in an oven at 110 6 5°C110 °C 6 5 °C and store in a desiccator prior to use. Use tongs or rubber gloves, or both, to
handle the dishes.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
The last approved version of this historical standard is referenced on www.astm.org.
Available 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.
Available from Fisher, Disposable Aluminum Dishes (code 08–732–106), www.fishersci.com; McAlister Bicknell, Aluminum Weighing Dishes (code 10676–0000),
www.mbcoct.com; Cole-Parmer, Disposable Aluminum Weigh Dishes (code EW-01017–44), www.coleparmer.com.
D2369 − 24
5.3 Forced Draft Oven, Type IIA or Type IIB as specified in SpecificationProper air flow and temperature control are critical for
E145. The oven must be operating in accordance with Specification good precision, while adequate E145, since it is important to
have proper air flow and good temperature control to ensure good precision.air exchange minimizes accumulation of flammable
solvent vapors. The forced draft oven must operate in accordance with the following specifications:
NOTE 5—Be sure the shelves are level and dampers are open.
5.3.1 Temperature Uniformity: the consistency of heating throughout the oven chamber. The oven must achieve a temperature
uniformity of ≤ 4.0 °C at 110 °C and temperature controller stability of ≤ 1.0 °C. Temperature controller stability is the difference
between the load temperature and setpoint temperature over time.
5.3.2 Time Constant: the time required for the oven to return to setpoint temperature after opening oven door. The oven must
recover to the setpoint temp of 110 °C within 5 minutes of leaving oven door open for 30 seconds.
5.3.3 Air Exchanges: how often fresh laboratory air is introduced into the oven chamber. The oven must operate at ≥ 50 air
exchanges per hour.
5.4 Each specification should be certified by the oven manufacturer, confirmed by the user, or tested by a qualified third party.
Evaluation of oven specifications should be performed according to the procedures outlined in Specification E145.
NOTE 5—Be sure the shelves are level and dampers are open.
5.5 Syringe, 1-mL without 1 mL without needle, but equipped with caps, capable of properly dispensing the coating under test,
at a sufficient rate so that the specimen can be dissolved in the solvent.
NOTE 6—Disposable syringes with caps are recommended.
5.6 Paper Clips.
6. Reagents
6.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where
such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high
purity to permit its use without lessening the accuracy of the determination.
6.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean Type II of Specification D1193.
6.3 Toluene, water or appropriate solvent.
7. Procedure
7.1 Take a representative sample of the liquid coating (each component) in accordance with Practice D3925. Mix thoroughly by
hand before taking specimens.
7.2 For multi-component coatings, weigh each component in the proper proportion into a container that can be capped. Mix the
components together thoroughly by hand before extracting specimens. Tightly close the container to prevent loss of volatile
materials.
NOTE 7—Manufacturers often specify mix ratios by volume. To minimize errors, prepare the mixture gravimetrically using the measured density of each
ACS Reagent Chemicals, Specifications and Procedures for Reagents and Standard-Grade Reference Materials, American Chemical Society, Washington, DC. For
suggestions on the testing of reagents not listed by the American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and
the United States Pharmacopeia and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
D2369 − 24
component to convert volume to mass. The calculated mass and prepared mass should differ by no more than 0.1 % relative.
7.3 Weigh the preconditioned aluminum foil dish (see 5.2) and record the weight to the nearest 0.1 mg (W ). Use disposable (no
talc) rubber or polyethylene gloves, tweezers or forceps to handle the dish.
7.4 To facilitate dispersing or spreading the specimen, a metal paper clip may be placed (partially unfolded) in the aluminum dish
and weighed with the dish. If a paper clip is used, it must remain with the dish throughout the remainder of the procedure.
7.5 Add to the aluminum foil dish the appropriate type and amount of solvent according to Table 1.
7.6 Draw the coating specimen into the syringe. Remove the syringe from the specimen and then pull the plunger tip up 6 mm
( ⁄4 in.) in order to pull the specimen away from the neck of the syringe. Wipe the outer surface of the syringe to remove excess
material and cap the syringe. Place the filled syringe on the scale and tare the scale. Use disposable (no talc) rubber or polyethylene
gloves to handle the syringe.
7.7 Remove the cap and dispense from the syringe into the dish the target specimen weight as specified in Table 1. If solvent is
used in the dish add the specimen dropwise to the solvent-containing dish. The paper clip may be used to help 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, Method E), spread out the specimen in the dish with the paper clip to cover the bottom of the dish
completely with as uniform thickness as possible.
7.8 After dispensing the specimen, do not wipe the tip of the 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 was dispensed) and
record the weight to the nearest 0.1 mg as the Specimen Weight (S ).
A
7.9 Repeat steps 7.3 – 7.8 to prepare a duplicate specimen for each sample.
NOTE 8—Duplicate determinations must meet the relative percent difference requirements detailed in 8.2.
7.10 For multi-component coatings, after the specimens are prepared, allow them to sit at ambient conditions for a prescribed
induction time according to Table 1 before placing the dishes in the oven.
7.11 Heat the aluminum foil dishes containing the specimens in the forced draft oven (5.3) for 60 min at 110 6 5°C.110 °C 6
5 °C.
7.12 Remove each dish from the oven, place immediately in a desiccator, cool to ambient temperature, weigh to the nearest 0.1
mg and record this weight (W ) for each specimen.
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
Solvent Type and Amount 3 ml ± 1 ml water (6.2) 3 ml ± 1 ml solvent (6.3) 3 ml ± 1 ml water (6.2) 3 ml ± 1 ml solvent none
(6.3)
A
Specimen Weight 0.3 ± 0.1 g if expected result is =<40 % volatile (>=60 % non-volatile) see
0.5 ± 0.1 g if expected result is >40 % volatile (<60 % non-volatile)
A
Specimen Weight 0.3 g ± 0.1 g if expected result is =<40 % volatile (>=60 % non-volatile) see
0.5 g ± 0.1 g if expected result is >40 % volatile (<60 % non-volatile)
B B
Induction Time N/A N/A 1 hr (see ) 1 hr (see ) 24 hr
A
Specimen weight to be representative of how the product is used (the low
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