ASTM D6266-00a(2017)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D6266 − 00a (Reapproved 2017)
Standard Test Method for
Determining the Amount of Volatile Organic Compound
(VOC) Released From Waterborne Automotive Coatings and
Available for Removal in a VOC Control Device
(Abatement)
This standard is issued under the fixed designation D6266; 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.
1. Scope ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
1.1 This test method describes the determination of the
mendations issued by the World Trade Organization Technical
amount of volatile organic compound (VOC) released from
Barriers to Trade (TBT) Committee.
applied waterborne automotive coatings that is available for
delivery to a VOC control device. The determination is
2. Referenced Documents
accomplished by measuring the weight loss of a freshly coated
2.1 ASTM Standards:
test panel subject to evaporation or drying and by analysis of
D343 Specification for 2-Ethoxyethyl Acetate (95% Grade)
the VOC or water content in the coating.
(Withdrawn 1980)
1.2 This test method is applicable to the VOC released from
D1186 Test Methods for Nondestructive Measurement of
application and baking operations after the paint has been
Dry Film Thickness of Nonmagnetic Coatings Applied to
applied in a simulation of a production process, or in an actual
a Ferrous Base (Withdrawn 2006)
production facility.
D1193 Specification for Reagent Water
1.3 Symbols and calculations from several other methods
D1475 Test Method For Density of Liquid Coatings, Inks,
that determine VOC: Practice D3960, EPA 450/3-88-018 and
and Related Products
EPA 450/3-84-019 have been incorporated into this test
D2369 Test Method for Volatile Content of Coatings
method. The majority of symbols and calculations used in this
D2697 Test Method for Volume Nonvolatile Matter in Clear
test method are unique because this test method deals uniquely
or Pigmented Coatings
with differences in weight of applied paint samples that have
D3960 Practice for Determining Volatile Organic Compound
been subject to drying, curing or solvent addition.
(VOC) Content of Paints and Related Coatings
NOTE 1—Training and knowledge of the product being evaluated are
D4017 Test Method for Water in Paints and Paint Materials
essential for obtaining meaningful data from this test method. It is
by Karl Fischer Method
recommended that several practice runs be performed, and the laboratories
E145 Specification for Gravity-Convection and Forced-
repeatability evaluated before performing this test on the test samples.
Ventilation Ovens
1.4 The values stated in SI units are to be regarded as the
E691 Practice for Conducting an Interlaboratory Study to
standard. The values given in parentheses are for information
Determine the Precision of a Test Method
only.
2.2 U.S. EPA Standards:
1.5 This standard does not purport to address all of the
EPA 450/3-88-018 (Dated December, 1988) Environmental
safety concerns, if any, associated with its use. It is the
Protection Agency Protocol for Determining the Daily
responsibility of whoever uses this standard to consult and
Volatile Organic Compound Emission Rate of Automobile
establish appropriate safety and health practices and deter-
and Light Duty Truck Topcoat Operations. This protocol
mine the applicability of regulatory limitations prior to its use.
1.6 This international standard was developed in accor-
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
dance with internationally recognized principles on standard-
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
This test method is under the jurisdiction of ASTM Committee D01 on Paint the ASTM website.
and Related Coatings, Materials, and Applications and is the direct responsibility of The last approved version of this historical standard is referenced on
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials. www.astm.org.
Current edition approved July 1, 2017. Published July 2017. Originally approved Available from U.S. Government Printing Office Superintendent of Documents,
in 1998. Last previous edition approved in 2011 as D6266 – 00a (2011). DOI: 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
10.1520/D6266-00AR17. www.access.gpo.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D6266 − 00a (2017)
describes procedures for determining VOC emission re- 5. Apparatus and Materials for the Analyses
duction credit in abatement processes. NOTE 2—Purity of Reagents—Reagent grade chemicals shall be used in
all tests. Unless otherwise indicated, it is intended that all reagents shall
EPA Federal Reference Method 24 - (Ref. 40CFR, part 60,
conform to the specification of the Committee on Analytical Reagents of
Appendix A) Determination of Volatile Matter Content,
the American Chemical Society, where such specifications are available.
Water Content, Density, Volume Solids and Weight Solids,
Other grades may be used, provided it is ascertained that the reagent is of
of Surface Coatings.
sufficiently high purity to permit its use without lessening the accuracy of
the determination. The references to purity of water, unless otherwise
EPA 450/3-84-019 Procedures for Certifying Quantity of
indicated, shall be understood to mean Type II reagent grade water
Organic Compound Emitted by Paint, Ink, and Other
conforming to Specification D1193.
Coatings
Sample Preparation:
3. Summary of Test Method
2 2
5.1 Thin Steel Panels, with an area of 310 cm (48 in. ) or
3.1 This procedure measures the loss of VOC from a freshly
smaller.
coated surface by; (a) determining the difference in weight of
5.2 Laboratory Balance, with accuracy to 0.001 g (mini-
a coated test panel before and after various steps in a process,
mum).
(b) analyzing a sample of the applied coating for VOC or water
content, or both, by gas chromatography (GC), or Karl Fisher,
5.3 Laboratory Spray Booth, for application of the test
or both, before and after various steps in a process, and (c)
coating, with air flow representative of production conditions.
calculating the VOC directly or after subtracting the water
5.4 Spray Application Equipment, selected to represent that
content. With these analyses, it is possible to relate the VOC
used in a production process or sufficiently similar that the
loss to the volume of solids deposited on the test panel at each
equipment will produce comparable performance.
step of a process. The information obtained is used to deter-
mine the amount of VOC available for removal by the VOC
5.5 Film Thickness Gage, for measuring dry paint thickness
control device at each step of a process (see Fig. 1). on metal surfaces (see Test Methods D1186).
5.6 Laboratory Force-Draft Bake Oven, Type-IIA or Type
4. Significance and Use
IIB, as specified in Specification E145.
4.1 This test method provides basic engineering data that
5.7 Wide-Mouth Glass Jars, with TFE-fluorocarbon-lined
may be used to determine the amount of VOC delivered to the
caps or polypropylene copolymer bottles, one for each sample.
inlet of a VOC control device. The procedure is useful for
establishing the quantity of VOC that is evolved from the 5.8 Smooth Aluminum Foil, (grade may vary).
coating in the flash zone or bake oven and available to be
5.9 Ultrasonic Cleaner unit, with 0.95 L (1 qt) capacity
incinerated, although the same procedure can be followed
minimum.
when other forms of VOC abatement are used.
5.10 Laboratory Scale Paint Shaker (violent agitation) 3.8
4.2 The total amount of VOC removed from the process by
L (1-gal) capacity.
the VOC control device is a function of the amount available as
5.11 Wood tongue Depressor or Tweezers, if desired to roll
given by this test method combined with the VOC removal
efficiency of the control device. foil.
FIG. 1 Test Panel Processing
D6266 − 00a (2017)
Apparatus and Reagents for GC Analysis: 5.42 Toluene, minimum technical grade,
5.12 Gas Chromatograph, equipped with a flame ionization
5.43 Ethoxyethyl Acetate, minimum technical grade, Speci-
detector, electronic reporting integrator, capillary split injection fication D343.
port, and autosampler (where available).
6. Coating Materials
5.13 Chromatographic Syringe, (10.0 µL).
6.1 The coating materials used are to be in the “as applied
5.14 Analytical Balance, accurate to 0.1mg is needed, for
condition,” for example, representative of the specific formu-
this method.
lation used in the coating process to be evaluated.
5.15 Sealable Vials, (20 mL) scintillation.
5.16 Medicine Droppers.
7. Conditions
5.17 Analytical Column—capillary, (30 meter) (0.25 mm)
7.1 Prior to beginning the test, determine the following
inside diameter,
conditions that represent the production process:
5.17.1 film thickness, fused silica DB-5 or equivalent.
(1) Dry film thickness,
(2) Process sequence flash times,
5.18 Autosampler Vials.
(3) Air flow,
5.19 Pipet, Volumetric.
(4) Percent solids content after dehydration, and
5.20 Volumetric Flask, for calibration standard and internal
(5) Temperature and humidity conditions for each signifi-
standard solutions.
cant step of the process.
7.1.1 With the information obtained, establish test param-
5.21 Bottles, with good sealing caps for standard solutions.
eters that represent the range of conditions found in the plant.
5.22 Solvents Standards, expected to be found in the coating
Specific application parameters need not duplicate exact pro-
to be tested.
duction conditions as long as the above parameters are con-
5.23 Tetrahydrofuran (THF)—HPLC grade, uninhibited.
trolled for this test.
5.24 Cyclohexanol—98 % or appropriate grade reagent.
7.2 Identify all locations in the process sequence in which
flash zone/oven effluent is vented directly to a VOC control
5.25 Water.
device. The number of locations will affect the number of panel
5.26 Acetone—HPLC grade.
weight measurements taken and the number of panels that need
5.27 Methanol—HPLC grade.
to be tested.
5.28 Dimethylformamide (DMF)—HPLC grade.
8. Procedures
5.29 Chromatography Gases—Helium of 99.9995 % purity
8.1 Parameters to Evaluate and General Method to Collect
or higher. Hydrogen of 99.9995 % minimum purity. Air, “dry”
Samples:
quality, free of hydrocarbons.
8.1.1 Parameters to be evaluated are as follows:
Apparatus and Reagents for KF Analysis:
(1) Determination of water content by Karl Fisher Titration
(KF) or
5.30 40-mL Volatile Organic Analysis (VOA) Vials, with
(2) Determination of organic solvent content by gas chro-
TFE-fluorocarbon lined caps.
matography (GC), or both, and
5.31 Methanol—Low water grade (<0.008 % by K.F.)
(3) Determination of volatiles and nonvolatiles (% NV)
5.32 Karl Fisher Titrator, or equivalent coulometric.
during flash/baking operations.
5.33 Reagents, appropriate for titrator.
8.2 Use of Panels and Foil:
8.2.1 For each location identified in 7.2, prepare test panels
5.34 Associated Glassware, for the tests (pipetes, volumet-
in duplicate as a minimum or as agreed upon between the
ric flasks, etc).
involved parties.
5.35 Water, for calibration of the test instrument.
NOTE 3—Thin steel panels 101.6 by 304.8 mm (4 by 12 in.) are
Apparatus and Reagents for Solids Density (Test Methods
preferred. If spray area is limited, smaller panels such as 101.6 by 152.4
mm (4 by 6 in.) can be used. Foils should be 13 mm ( ⁄2 in.) larger in size
D2369, D1475, D2697; EPA Federal Reference Method 24):
than the area to be sprayed for easiness in handling.
5.36 Syringe, 5 mL.
8.2.2 Specified time at which the samples need to be
5.37 Weighing or Bottle with eye dropper.
collected. The following is suggested as a guideline throughout
5.38 Test Tube, with new cork stopper. the rest of this procedure:
(1) Immediately after paint application, (Sample A)
5.39 Aluminum Foil Dish, 58 mm (2.3 in.) in diameter by 18
(2) Entrance to Dehydration Ovens, (Sample B)
mm (0.71 in.) high with a smooth bottom surface.
(3) Exit of Dehydration Oven, (Sample C)
5.40 Laboratory Force-Draft Bake Oven Type IIA or Type-
Where only the dehydration oven is exhausted to the VOC
IIB, as specified in Specification E145.
Control Device for example calculations in Section 11.
5.41 Analytical Balance, with accuracy to 0.1 mg. 8.2.3 Preparation of Samples:
D6266 − 00a (2017)
8.2.3.1 Dry and label sufficient sheets of foil (i=1, ., n) for 8.5.2.2 Fill a 5.0-mL disposable syringe with a well mixed
each test (A ; B ; C ) to constant weight to remove residual representative portion of the methanol from one of the glass
i i i
moisture. sample jars. Perform this step in a low humidity room or
8.2.3.2 Record each foil weight (F ; F ; F ). chamber.
Ai Bi Ci
8.2.4 Wrap or secure foils on panels so some area (mini- 8.5.2.3 Weigh and transfer enough of each sample into the
Karl Fischer titration vessels so that at least 10 mL of KF
mum of ⁄2 in. (13 mm) per side) remains unpainted for the
future handling. reagent will be required to reach the endpoint. Repeat for each
sample and all blank vials.
8.2.5 Weigh jars and lids prior to spraying. Record the data.
Record each jar and lid weight (J ; J ; J ). 8.5.3 Calculation of % Water in the Paint Sample on a
Ai Bi Ci
Wt./Wt. Basis:
8.2.6 Prepare as a minimum one additional steel panel per
8.5.3.1 Determine the weight of sample paint on the foil P
spray out (for film thickness verification) to be sprayed with the
i
as follows:
foiled panels. All panels can be sprayed simultaneously.
Alternatively, the spraying could be broken into families of
P 5 K 2 F 1J (1)
~ !
i i i i
various panels for each one of the requested tests for % NV,
where:
KF, and GC.
i = foil i,
NOTE 4—“Trip blanks” are analyzed for all parameters of interest. Trip
K = weight of jar, lid, foil and paint (4.1.1),
i
blanks are often prepared by the laboratory and submitted to the sampling
F = weight of foil (8.2.3.2), and
i
team when bottle ware is delivered. The trip blank accompanies all of the
J = weight of jar and lid (8.2.5).
i
project samples through all custody changes in possession, coolers, and
refrigerators. Trip blanks are not opened by the sampling team. The trip
8.5.3.2 Determine the weight of methanol used for Sample
blanks provide information with respect t
...