ASTM D6266-00a

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D6266–00a
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 D 6266; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope D 343 Specification for 2–Ethoxyethyl Acetate (95 %)
Grade
1.1 This test method describes the determination of the
D 1186 Test Methods for Nondestructive Measurement of
amount of volatile organic compound (VOC) released from
Dry Film Thickness of Non-magnetic CoatingsApplied to
applied waterborne automotive coatings that is available for
a Ferrous Base
delivery to a VOC control device. The determination is
D 1193 Specification for Reagent Water
accomplished by measuring the weight loss of a freshly coated
D 1475 Test Method for Density of Liquid Coatings, Inks,
test panel subject to evaporation or drying and by analysis of
and Related Products
the VOC or water content in the coating.
D 2369 Test Method for Volatile Content of Coatings
1.2 This test method is applicable to theVOC released from
D 2697 Test Method for Volume Nonvolatile Matter in
application and baking operations after the paint has been
Clear or Pigmented Coatings
applied in a simulation of a production process, or in an actual
D 3960 Practice for Determining Volatile Organic com-
production facility.
pound (VOC) Content of Paints and Related Coatings
1.3 Symbols and calculations from several other methods
D 4017 Test Method forWater in Paints and Paint Materials
that determine VOC: Practice D 3960, EPA 450/3-88-018 and
by Karl Fisher Method
EPA 450/3-84-019 have been incorporated into this test
E 145 Specification for Gravity-Convention and Forced-
method. The majority of symbols and calculations used in this
Ventilation Ovens
test method are unique because this test method deals uniquely
E 691 Practice for Conducting an Interlaboratory Study to
with differences in weight of applied paint samples that have
Determine the Precision of a Test Method
been subject to drying, curing or solvent addition.
2.2 U.S. EPA Standards:
NOTE 1—Training and knowledge of the product being evaluated are
EPA450/3-88-018 (Dated December, 1988). Environmental
essential for obtaining meaningful data from this test method. It is
Protection Agency Protocol for Determining the Daily
recommendedthatseveralpracticerunsbeperformed,andthelaboratories
Volatile Organic Compound Emission Rate ofAutomobile
repeatability evaluated before performing this test on the test samples.
and Light Duty Truck Topcoat Operations. This protocol
1.4 The values stated in SI units are to be regarded as the
describes procedures for determining VOC emission re-
standard. The values given in parentheses are for information
duction credit in abatement processes.
only.
EPA Federal Reference Method 24 - (Ref. 40CFR, part 60,
1.5 This standard does not purport to address all of the
Appendix A). Determination of Volatile Matter Content,
safety concerns, if any, associated with its use. It is the
Water Content, Density, Volume Solids, of Surface Coat-
responsibility of whoever uses this standard to consult and
ings.
establish appropriate safety and health practices and deter-
EPA 450/3-84-019 Procedures for Certifying Quantity of
mine the applicability of regulatory limitations prior to its use.
Organic Compound Emitted by Paint, Ink, and Other
Coatings
2. Referenced Documents
2.1 ASTM Standards:
Discontinued l980; see l979 Annual Book of ASTM Standards, Part 29.
Annual Book of ASTM Standards, Vol 06.01.
1 4
This test method is under the jurisdiction of ASTM Committee D01 on Paint Annual Book of ASTM Standards, Vol 11.01.
and Related Coatings, Materials, andApplications and is the direct responsibility of Annual Book of ASTM Standards, Vol 14.04.
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials. Annual Book of ASTM Standards, Vol 14.02.
Current edition approved May 10, 2000. Published August 2000. Originally Available from the Superintendent of Documents, U.S. Government Printing
published as D 6266 – 98. Last previous edition D 6266 – 00. Office, Washington, DC 20402.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D6266–00a
3. Summary of Test Method 5.11 Wood tongue Depressor or Tweezers, if desired to roll
foil.
3.1 This procedure measures the loss ofVOC from a freshly
coated surface by; (a) determining the difference in weight of
Apparatus and Reagents for GC Analysis:
a coated test panel before and after various steps in a process,
(b) analyzing a sample of the applied coating forVOC or water
5.12 Gas Chromatograph, equipped with a flame ionization
content, or both, by gas chromatography (GC), or Karl Fisher,
detector,electronicreportingintegrator,capillarysplitinjection
or both, before and after various steps in a process, and (c)
port, and autosampler (where available).
calculating the VOC directly or after subtracting the water
5.13 Chromatographic Syringe, (10.0 µL).
content. With these analyses, it is possible to relate the VOC
5.14 Analytical Balance, accurate to 0.1mg is needed, for
loss to the volume of solids deposited on the test panel at each
this method.
step of a process. The information obtained is used to deter-
5.15 Sealable Vials, (20 mL) scintillation.
mine the amount of VOC available for removal by the VOC
5.16 Medicine Droppers.
control device at each step of a process (see Fig. 1).
5.17 Analytical Column—capillary, (30 meter) (0.25 mm)
inside diameter,
4. Significance and Use
5.17.1 film thickness, fused silica DB-5 or equivalent.
4.1 This test method provides basic engineering data that
5.18 Autosampler Vials.
may be used to determine the amount of VOC delivered to the
5.19 Pipet Volumetric.
inlet of a VOC control device. The procedure is useful for
5.20 Volumetric Flask, for calibration standard and internal
establishing the quantity of VOC that is evolved from the
standard solutions.
coating in the flash zone or bake oven and available to be
5.21 Bottles, with good sealing caps for standard solutions.
incinerated, although the same procedure can be followed
5.22 SolventsStandards,expectedtobefoundinthecoating
when other forms of VOC abatement are used.
to be tested.
4.2 The total amount of VOC removed from the process by
5.23 Tetrahydrofuran (THF)—HPLC grade, uninhibited.
theVOCcontroldeviceisafunctionoftheamountavailableas
5.24 Cyclohexanol—98 % or appropriate grade reagent.
given by this test method combined with the VOC removal
5.25 Water.
efficiency of the control device.
5.26 Acetone—HPLC grade.
5.27 Methanol—HPLC grade.
5. Apparatus and Materials for the Analyses
5.28 Dimethylformamide (DMF)—HPLC grade.
NOTE 2—PurityofReagents—Reagentgradechemicalsshallbeusedin
5.29 Chromatography Gases—Helium of 99.9995 % purity
all tests. Unless otherwise indicated, it is intended that all reagents shall
or higher. Hydrogen of 99.9995 % minimum purity.Air, “dry”
conform to the specification of the Committee on Analytical Reagents of
quality, free of hydrocarbons.
the American Chemical Society, where such specifications are available.
Other grades may be used, provided it is ascertained that the reagent is of
sufficiently high purity to permit its use without lessening the accuracy of
Apparatus and Reagents for KF Analysis:
the determination. The references to purity of water, unless otherwise
5.30 40-mL Volatile Organic Analysis (VOA) Vials, with
indicated, shall be understood to mean Type II reagent grade water
TFE-fluorocarbon lined caps.
conforming to Specification D 1193.
5.31 Methanol—Low water grade (<0.008 % by K.F.)
Sample Preparation:
5.32 Karl Fisher Titrator, or equivalent coulometric.
2 2
5.1 Thin Steel Panels, with an area of 310 cm (48 in.)or
5.33 Reagents, appropriate for titrator.
smaller.
5.34 Associated Glassware, for the tests (pipetes, volumet-
5.2 Laboratory Balance, with accuracy to 0.001 g (mini-
ric flasks, etc).
mum).
5.35 Water, for calibration of the test instrument.
5.3 Laboratory Spray Booth, for application of the test
coating, with air flow representative of production conditions.
Apparatus and Reagents for Solids Density (Test Methods
5.4 Spray Application Equipment, selected to represent that
D2369, D1475, D2697; EPA Federal Reference Method
used in a production process or sufficiently similar that the
24):
equipment will produce comparable performance.
5.36 Syringe, 5 mL.
5.5 Film Thickness Gage, for measuring dry paint thickness
5.37 Weighing or Bottle with eye dropper.
on metal surfaces (see Test Methods D 1186).
5.38 Test Tube, with new cork stopper.
5.6 Laboratory Force-Draft Bake Oven, Type-IIA or Type
5.39 AluminumFoilDish,58mm(2.3in.)indiameterby18
IIB, as specified in Specification E 145.
mm (0.71 in.) high with a smooth bottom surface.
5.7 Wide-Mouth Glass Jars, with TFE-fluorocarbon-lined
5.40 Laboratory Force-Draft Bake Oven Type IIA or Type-
caps or polypropylene copolymer bottles, one for each sample.
IIB, as specified in Specification E 145.
5.8 Smooth Aluminum Foil, (grade may vary).
5.41 Analytical Balance, with accuracy to 0.1 mg.
5.9 Ultrasonic Cleaner unit, with 0.95 L (1 qt) capacity
5.42 Toluene, minimum technical grade,
minimum.
5.10 Laboratory Scale Paint Shaker (violent agitation) 3.8 5.43 Ethoxyethyl Acetate, minimum technical grade, Speci-
L (1-gal) capacity. fication D 343.
D6266–00a
FIG. 1 Test Panel Processing
D6266–00a
6. Coating Materials 8.2.4 Wrap or secure foils on panels so some area (mini-
mum of ⁄2 in. (13 mm) per side) remains unpainted for the
6.1 The coating materials used are to be in the “as applied
future handling.
condition”, for example, representative of the specific formu-
8.2.5 Weigh jars and lids prior to spraying. Record the data.
lation used in the coating process to be evaluated.
Record each jar and lid weight (J ; J ; J ).
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8.2.6 Prepare as a minimum one additional steel panel per
7. Conditions
sprayout(forfilmthicknessverification)tobesprayedwiththe
7.1 Prior to beginning the test, determine the following
foiled panels. All panels can be sprayed simultaneously.
conditions that represent the production process:
Alternatively, the spraying could be broken into families of
(1) Dry film thickness,
various panels for each one of the requested tests for % NV,
(2) Process sequence flash times,
KF, and GC.
(3) Air flow,
NOTE 4—“Trip blanks” are analyzed for all parameters of interest. Trip
(4) Percent solids content after dehydration, and
blanks are often prepared by the laboratory and submitted to the sampling
(5) Temperature and humidity conditions for each signifi-
team when bottle ware is delivered. The trip blank accompanies all of the
cant step of the process.
project samples through all custody changes in possession, coolers, and
refrigerators. Trip blanks are not opened by the sampling team. The trip
7.1.1 With the information obtained, establish test param-
blanks provide information with respect to contamination that is“ picked-
eters that represent the range of conditions found in the plant.
up” during sample packaging, shipping and storage.
Specific application parameters need not duplicate exact pro-
NOTE 5—The “field blank” is a portion of the sampling matrix that is
duction conditions as long as the above parameters are con-
carried through the entire analytical scheme. The field blank is treated
trolled for this test.
exactly as the actual sample is treated. For example, the field blank vial is
7.2 Identify all locations in the process sequence in which
opened and closed when the corresponding sample vial is opened and
flash zone/oven effluent is vented directly to a VOC control
closed. It is important that the volume/weight of the field blanks be the
device.Thenumberoflocationswillaffectthenumberofpanel same as that of the samples.
weightmeasurementstakenandthenumberofpanelsthatneed
8.3 Spraying Samples:
to be tested.
8.3.1 Apply basecoat using an automated device (preferred
for consistency) to target film build simulating assembly plant
8. Procedures
processing conditions.
8.1 Parameters to Evaluate and General Method to Collect
8.4 Collection of Samples:
Samples:
8.4.1 At the sampling points specified in 8.2.2, the foil
8.1.1 Parameters to be evaluated are as follows:
samples for KF and GC analyses need to be placed in jars with
(1) Determination of water content by Karl FisherTitration
a specified solvent (8.5 and 8.6). The samples for % NV just
(KF) or need to be weighed at the sampling point.Then, they are baked
(2) Determination of organic solvent content by gas chro- at final bake condition and re-weighed.
matography (GC), or both, and 8.4.2 Roll up foil paint side out for KF (8.5) and GC (8.6).
8.4.3 Place coated foil (8.4.1) immediately into a jar of size
(3) Determination of volatiles and nonvolatiles (% NV)
during flash/baking operations. depending upon foil size. Weigh jars, lids, and coated foils.
Record weights (K ; K ; K ) including field blanks (see
8.2 Use of Panels and Foil:
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8.2.6).
8.2.1 For each location identified in 7.2, prepare test panels
8.4.4 Fold foils paint side in for % NV (8.7).
in duplicate as a minimum or as agreed upon between the
8.5 Water Content by KF:
involved parties.
8.5.1 Water Content Solvent Preparation:
NOTE 3—Thin steel panels 101.6 by 304.8 mm (4 by 12 in.) are
8.5.1.1 Analyze a sample of the bulk methanol for water
preferred. If spray area is limited, smaller panels such as 101.6 by 152.4
content by the Karl Ficher Method in accordance with Test
mm (4 by 6 in.) can be used. Foils should be 13 mm ( ⁄2 in.) larger in size
Method D 4017 to check purity of reagent.
than the area to be sprayed for easiness in handling.
8.5.1.2 Fill each jar (as described in 8.4.1.1) with 30 mL of
8.2.2 Specified time at which the samples need to be
methanol. Foil should be completely submerged in methanol.
collected.The following is suggested as a guideline throughout
8.5.1.3 Reweigh jars, lids, coated foils and methanol and
the rest of this procedure:
record weights (L ; L ; L ).
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(1) Immediately after paint application, (Sample A)
8.5.1.4 Place the capped jars containing methanol and foil
(2) Entrance to Dehydration Ovens, (Sample B)
strips into an ultrasonic cleaning unit until sample is uniformly
(3) Exit of Dehydration Oven, (Sample C)
dispersed int
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