Draft Uganda Standard: Standard Test Method For Volatile Content of Coatings

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DUS 2002

DRAFT UGANDA STANDARD


First Edition
2018-mm-dd

Standard Test Method for Volatile Content of Coatings

Reference number
DUS 2002: 2018

This Draft Uganda Standard, DUS 2002:2018, is based on ASTM D2369 – 10, Standard
Test Method for Volatile Content of Coatings, Copyright ASTM International, 100 Barr
Harbor Drive, West Conshohocken, PA 19428, USA, pursuant to license with ASTM
International. © UNBS 2018
D2369 – 10 DUS 2002: 2018

Compliance with this standard does not, of itself confer immunity from legal obligations

A Uganda Standard does not purport to include all necessary provisions of a contract. Users are
responsible for its correct application

© UNBS 2018

All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form
or by any means, electronic or mechanical, including photocopying and microfilm, without prior written permission
from UNBS.

Requests for permission to reproduce this document should be addressed to

The Executive Director


Uganda National Bureau of Standards
P.O. Box 6329
Kampala
Uganda
Tel: +256 417 333 250/1/2
Fax: + 256 414 286 123
E-mail: [email protected]
Web: www.unbs.go.ug

© UNBS 2018 – All rights reserved ii


D2369 – 10 DUS 2002: 2018

Foreword

Uganda National Bureau of Standards (UNBS) is a parastatal under the Ministry of Trade, Industry and
Cooperatives established under Cap 327, of the Laws of Uganda, as amended. UNBS is mandated to co-ordinate
the elaboration of standards and is
(a) a member of International Organisation for Standardisation (ISO) and

(b) a contact point for the WHO/FAO Codex Alimentarius Commission on Food Standards, and

(c) the National Enquiry Point on TBT Agreement of the World Trade Organisation (WTO).

The work of preparing Uganda Standards is carried out through Technical Committees. A Technical Committee is
established to deliberate on standards in a given field or area and consists of key stakeholders including
government, academia, consumer groups, private sector and other interested parties.
Draft Uganda Standards adopted by the Technical Committee are widely circulated to stakeholders and the
general public for comments. The committee reviews the comments before recommending the draft standards for
approval and declaration as Uganda Standards by the National Standards Council.

The committee responsible for this document is Technical Committee UNBS/TC5/SC2, Paints, Varnishes and
related products.

Wherever the words, “ASTM Standard" appear, they should be replaced by "Uganda Standard."

© UNBS 2018 – All rights reserved iii


DRAFT UGANDA STANDARD DUS 2002: 2018

Designation: D2369 – 10

This Draft Uganda Standard, DUS 2002:2018, is based on ASTM D2369 – 10, Standard Test Method for Volatile
Content of Coatings, Copyright ASTM International, 100 Barr Harbor Drive, West Conshohocken, PA 19428, USA,
pursuant to license with ASTM International

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 (ε) 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

1.1 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 ± 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 ± 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 ± 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

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 Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.
Current edition approved June 1, 2015. Published June 2015. Originally approved in 1965. Last previous edition approved in 2010 as D2369 – 10ε1. DOI:
10.1520/D2369-10R15E01.

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D2369 – 10 DUS 2002: 2018

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 and health practices and determine the applicability
of regulatory limitations prior to use.

2. Referenced Documents

2.1 ASTM Standards:2


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)3
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 4

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 ± 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 ±0.1 mg.


5.2 Aluminum Foil Dishes5 , 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 ± 5°C and store in a desiccator prior to use. Use tongs or rubber gloves, or both, to handle
the dishes.
5.3 Forced Draft Oven, Type IIA or Type IIB as specified in Specification E145. The oven must be operating in

2 For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [email protected]. For Annual Book of
ASTM Standards volume information, refer to the standard’s Document Summary page on the ASTM website.
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, 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401,
http://www.access.gpo.gov.
5 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.

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D2369 – 10 DUS 2002: 2018

accordance with Specification E145, since it is important to have proper air flow and good temperature control to ensure good
precision.
NOTE 5—Be sure the shelves are level and dampers are open.
5.4 Syringe, 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.
5.5 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.6 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.
7.3 Weigh the preconditioned aluminum foil dish (see 5.2) and record the weight to the nearest 0.1 mg (W 1). 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.

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) see A
0.5 ± 0.1 g if expected result is >40 % volatile (<60 % non-volatile)

Induction Time N/A N/A 1 hr (see B) 1 hr (see B) 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.

7.6 Draw the coating specimen into the syringe. Remove the syringe from the specimen and then pull the plunger tip up 6
mm (1/4 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

6 Reagent Chemicals, American Chemical Society Specifications, 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.

© UNBS 2018 – All rights reserved 9


D2369 – 10 DUS 2002: 2018

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.
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 ± 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 (W2) for each specimen.

8. Calculation

8.1 Calculate the percent volatile matter, V, in the liquid coating as follows:

where:
VA = % volatiles (first determination),
W1 = weight of dish,
W2 = weight of dish plus specimen after heating,
SA = specimen weight, and
VB = % volatiles (duplicate determination, calculate in same manner as VA).

8.2 Report V, the mean of the duplicate determination if relative percent difference is 1.5 % or less. If relative difference
between VA and VB is greater than 1.5 %, repeat the duplicate determinations. The 1.5 % relative difference is not applicable to
Method E.
8.3 The percent of nonvolatile matter, N, in the coating may be calculated by difference as follows:

where:
NA = 100 – VA, and
NB = 100 – VB.

NA represents first determination and NB represents duplicate determination.

9. Precision and Bias

9.1 The precision estimated for tests at 60 min at 110 ± 5°C are based on an interlaboratory study 7 in which 1 operator in
each of 15 laboratories analyzed in duplicate on 2 different days 7 samples of waterborne paints and 8 samples of
solventborne paints containing between 35 and 72 % volatile material. The paints were commercially supplied. The results
were analyzed statistically in accordance with Practice E180. The within-laboratory coefficient of variation was found to be
0.5 % relative at 213 df and the between-laboratories coefficient of variation was 1.7 % relative at 198 df. Based on these

7 Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D01-1026. Contact ASTM
Customer Service at [email protected].

© UNBS 2018 – All rights reserved 10


D2369 – 10 DUS 2002: 2018

coefficients, the following criteria should be used for judging the acceptability of results at the 95 % confidence level.
9.1.1 Repeatability—Two results, each the mean of duplicate determinations, obtained by the same operator on different
days should be considered suspect if they differ by more than 1.5 % relative.
9.1.2 Reproducibility—Two results, each the mean of duplicate determinations, obtained by operators in different
laboratories should be considered suspect if they differ by more than 4.7 % relative.
9.2 Bias—Bias has not been determined.
9.3 The precision results for multicomponent systems are based on an interlaboratory study in which one operator in each
of five laboratories analyzed in duplicate on two different days, four samples of commercially supplied solventborne and
waterborne multicomponent systems. The results were analyzed statistically in accordance with Practice E180.
9.3.1 Repeatability for Solventborne Multicomponent Systems:

Coefficient of variation 0.5 %


Degrees of freedom 6
Factor (based on 95 % confidence level) 3.46
Precision 1.74 %
Two results, each the mean of duplicate determinations obtained by the same operator on different days, should be
considered suspect if they vary by more than 1.74 % relative.

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 Systems:

Coefficient of variation 1.46 %


Degrees of freedom 5
Factor (based on 95 % confidence level) 3.64
Precision 5.31 %
Two results, each the mean of duplicate determinations obtained by operators in different laboratories, should be considered
suspect if they vary by more than 5.31 % relative.
9.3.3 Repeatability for Waterborne Multicomponent Systems:

Coefficient of variation 0.53 %


Degrees of freedom 6
Factor (based on 95 % confidence level) 3.46
Precision 1.84 %
Two results, each the mean of duplicate determinations obtained by the same operator on different days, should be
considered suspect if they vary by more than 1.84 % relative.
9.3.4 Reproducibility for Waterborne Multicomponent Systems:

Coefficient of variation 0.94 %


Degrees of freedom 5
Factor (based on 95 % confidence level) 3.64
Precision 3.43 %
Two results, each the mean of duplicate determinations obtained by operators in different laboratories, should be considered

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D2369 – 10 DUS 2002: 2018

suspect if they vary by more then 3.43 % relative.


9.4 Bias—Since there is no accepted standard for volatile content in coatings, bias cannot be determined.
9.5 Precision for Multi-Component, >90 % Solids Systems—The precision of this test was expanded to include data and
analysis from Method E based on an interlaboratory study conducted in 2009. Each of eight laboratories tested five different
materials, all multi-component, >90 % solids systems. Every “test result” represents the mean of duplicate determinations.
Every laboratory reported three replicate test results for the analysis. Practice E691 was followed for the design and analysis
of the data; the details are given in ASTM Research Report RR:D01-1152.8
9.5.1 Repeatability Limit (r)—Two test results, each the mean of duplicate determinations, obtained within one laboratory
shall be judged not equivalent if they differ by more than the “r” value for that material; “r” is the interval representing the
critical difference between two test results for the same material, obtained by the same operator using the same equipment on
the same day in the same laboratory.
9.5.1.1 Repeatability limits for each of the materials tested are listed in Table 2.
9.5.2 Reproducibility Limit (R)—Two test results, each the mean of duplicate determinations, between different laboratories
shall be judged not equivalent if they differ by more than the “R” value for that material; “R” is the interval representing the
critical difference between two test results for the same material, obtained by different operators using different equipment in
different laboratories.
9.5.2.1 Reproducibility limits for each of the metals tested are listed in Table 2.
9.5.3 The above terms (repeatability limit and reproducibility limit) are used as specified in Practice E177.
9.5.4 Any judgment in accordance with statements 9.5.1 and 9.5.2 would have an approximate 95 % probability of being
correct.
9.5.5 The precision statement for Method E for Multi-Component, >90 % Solids Systems was determined through
statistical examination of 120 reported results, from eight laboratories, on five materials, which were identified as:
A – Two component amine cured epoxy clear coating
B – Two component amine cured epoxy pigmented coating
C – Two component urethane pigmented coating
D – Two component urethane waterproofing membrane coating
E – Two component amine cured epoxy/acrylate highway marking coating
9.6 Bias—At the time of the study, there was no accepted reference material or method suitable for determining the bias for
this test method, therefore no statement on bias is being made.

10. Keywords

10.1 multicomponent paints; nonvolatile determination; VOC baking temperature; VOC in paints; volatile determination;
volatiles

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8 Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D01-1152. Contact ASTM
Customer Service at [email protected].

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D2369 – 10 DUS 2002: 2018

Certification marking

Products that conform to Uganda standards may be marked with Uganda National Bureau of Standards (UNBS)
Certification Mark shown in the figure below.

The use of the UNBS Certification Mark is governed by the Standards Act, and the Regulations made thereunder.
This mark can be used only by those licensed under the certification mark scheme operated by the Uganda
National Bureau of Standards and in conjunction with the relevant Uganda Standard. The presence of this mark on
a product or in relation to a product is an assurance that the goods comply with the requirements of that standard
under a system of supervision, control and testing in accordance with the certification mark scheme of the Uganda
National Bureau of Standards. UNBS marked products are continually checked by UNBS for conformity to that
standard.

Further particulars of the terms and conditions of licensing may be obtained from the Director, Uganda National
Bureau of Standards.

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D2369 – 10 DUS 2002: 2018

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