ASTM D6266-00a(2005)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:D6266–00a(Reapproved2005)
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 2. Referenced Documents
1.1 This test method describes the determination of the 2.1 ASTM Standards:
amount of volatile organic compound (VOC) released from D343 Specification for 2–Wthoxyethyl Acetate (95 %
applied waterborne automotive coatings that is available for Grade)
delivery to a VOC control device. The determination is D1186 Test Methods for Nondestructive Measurement of
accomplished by measuring the weight loss of a freshly coated Dry Film Thickness of Nonmagnetic Coatings Applied to
test panel subject to evaporation or drying and by analysis of a Ferrous Base
the VOC or water content in the coating. D1193 Specification for Reagent Water
1.2 This test method is applicable to theVOC released from D1475 Test Method For Density of Liquid Coatings, Inks,
application and baking operations after the paint has been and Related Products
applied in a simulation of a production process, or in an actual D2369 Test Method for Volatile Content of Coatings
production facility. D2697 TestMethodforVolumeNonvolatileMatterinClear
1.3 Symbols and calculations from several other methods or Pigmented Coatings
that determine VOC: Practice D3960, EPA 450/3-88-018 and D3960 Practice for Determining Volatile Organic Com-
EPA 450/3-84-019 have been incorporated into this test pound (VOC) Content of Paints and Related Coatings
method. The majority of symbols and calculations used in this D4017 Test Method for Water in Paints and Paint Materials
test method are unique because this test method deals uniquely by Karl Fischer Method
with differences in weight of applied paint samples that have E145 Specification for Gravity-Convection and Forced-
been subject to drying, curing or solvent addition. Ventilation Ovens
E691 Practice for Conducting an Interlaboratory Study to
NOTE 1—Training and knowledge of the product being evaluated are
Determine the Precision of a Test Method
essential for obtaining meaningful data from this test method. It is
2.2 U.S. EPA Standards:
recommendedthatseveralpracticerunsbeperformed,andthelaboratories
EPA 450/3-88-018 (Dated December, 1988) Environmental
repeatability evaluated before performing this test on the test samples.
Protection Agency Protocol for Determining the Daily
1.4 The values stated in SI units are to be regarded as the
Volatile Organic Compound Emission Rate ofAutomobile
standard. The values given in parentheses are for information
and Light Duty Truck Topcoat Operations. This protocol
only.
describes procedures for determining VOC emission re-
1.5 This standard does not purport to address all of the
duction credit in abatement processes.
safety concerns, if any, associated with its use. It is the
EPA Federal Reference Method 24 - (Ref. 40CFR, part 60,
responsibility of whoever uses this standard to consult and
Appendix A) Determination of Volatile Matter Content,
establish appropriate safety and health practices and deter-
mine the applicability of regulatory limitations prior to its use.
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
This test method is under the jurisdiction of ASTM Committee D01 on Paint the ASTM website.
and Related Coatings, Materials, andApplications and is the direct responsibility of Withdrawn. The last approved version of this historical standard is referenced
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials. on www.astm.org.
Current edition approved July 1, 2005. Published August 2005. Originally AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
approved in 1998. Last previous edition approved in 2000 as D6266 – 00a. DOI: 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
10.1520/D6266-00AR05. www.access.gpo.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D6266–00a (2005)
Other grades may be used, provided it is ascertained that the reagent is of
WaterContent,Density,VolumeSolidsandWeightSolids,
sufficiently high purity to permit its use without lessening the accuracy of
of Surface Coatings.
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 ThisproceduremeasuresthelossofVOCfromafreshly
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)analyzingasampleoftheappliedcoatingforVOCorwater
5.3 Laboratory Spray Booth, for application of the test
content, or both, by gas chromatography (GC), or Karl Fisher,
coating, with air flow representative of production conditions.
or both, before and after various steps in a process, and (c)
5.4 Spray Application Equipment, selected to represent that
calculating the VOC directly or after subtracting the water
used in a production process or sufficiently similar that the
content. With these analyses, it is possible to relate the VOC
equipment will produce comparable performance.
loss to the volume of solids deposited on the test panel at each
5.5 Film Thickness Gage, for measuring dry paint thickness
step of a process. The information obtained is used to deter-
on metal surfaces (see Test Methods D1186).
mine the amount of VOC available for removal by the VOC
5.6 Laboratory Force-Draft Bake Oven, Type-IIA or Type
control device at each step of a process (see Fig. 1).
IIB, as specified in Specification E145.
5.7 Wide-Mouth Glass Jars, with TFE-fluorocarbon-lined
4. Significance and Use
caps or polypropylene copolymer bottles, one for each sample.
4.1 This test method provides basic engineering data that
5.8 Smooth Aluminum Foil, (grade may vary).
may be used to determine the amount of VOC delivered to the
5.9 Ultrasonic Cleaner unit, with 0.95 L (1 qt) capacity
inlet of a VOC control device. The procedure is useful for
minimum.
establishing the quantity of VOC that is evolved from the
5.10 Laboratory Scale Paint Shaker (violent agitation) 3.8
coating in the flash zone or bake oven and available to be
L (1-gal) capacity.
incinerated, although the same procedure can be followed
5.11 Wood tongue Depressor or Tweezers, if desired to roll
when other forms of VOC abatement are used.
foil.
4.2 The total amount of VOC removed from the process by
Apparatus and Reagents for GC Analysis:
theVOCcontroldeviceisafunctionoftheamountavailableas
5.12 Gas Chromatograph, equipped with a flame ionization
given by this test method combined with the VOC removal
detector,electronicreportingintegrator,capillarysplitinjection
efficiency of the control device.
port, and autosampler (where available).
5. Apparatus and Materials for the Analyses
5.13 Chromatographic Syringe, (10.0 µL).
5.14 Analytical Balance, accurate to 0.1mg is needed, for
NOTE 2—PurityofReagents—Reagentgradechemicalsshallbeusedin
this method.
all tests. Unless otherwise indicated, it is intended that all reagents shall
5.15 Sealable Vials, (20 mL) scintillation.
conform to the specification of the Committee on Analytical Reagents of
the American Chemical Society, where such specifications are available. 5.16 Medicine Droppers.
FIG. 1 Test Panel Processing
D6266–00a (2005)
5.17 Analytical Column—capillary, (30 meter) (0.25 mm) 7.1.1 With the information obtained, establish test param-
inside diameter, eters that represent the range of conditions found in the plant.
5.17.1 film thickness, fused silica DB-5 or equivalent. Specific application parameters need not duplicate exact pro-
5.18 Autosampler Vials. duction conditions as long as the above parameters are con-
5.19 Pipet, Volumetric. trolled for this test.
5.20 Volumetric Flask, for calibration standard and internal 7.2 Identify all locations in the process sequence in which
standard solutions. flash zone/oven effluent is vented directly to a VOC control
5.21 Bottles, with good sealing caps for standard solutions. device.Thenumberoflocationswillaffectthenumberofpanel
5.22 SolventsStandards,expectedtobefoundinthecoating weightmeasurementstakenandthenumberofpanelsthatneed
to be tested. to be tested.
5.23 Tetrahydrofuran (THF)—HPLC grade, uninhibited.
5.24 Cyclohexanol—98 % or appropriate grade reagent. 8. Procedures
5.25 Water.
8.1 Parameters to Evaluate and General Method to Collect
5.26 Acetone—HPLC grade.
Samples:
5.27 Methanol—HPLC grade.
8.1.1 Parameters to be evaluated are as follows:
5.28 Dimethylformamide (DMF)—HPLC grade.
(1) Determination of water content by Karl FisherTitration
5.29 Chromatography Gases—Helium of 99.9995 % purity
(KF) or
or higher. Hydrogen of 99.9995 % minimum purity.Air, “dry”
(2) Determination of organic solvent content by gas chro-
quality, free of hydrocarbons.
matography (GC), or both, and
(3) Determination of volatiles and nonvolatiles (% NV)
Apparatus and Reagents for KF Analysis:
during flash/baking operations.
5.30 40-mL Volatile Organic Analysis (VOA) Vials, with
8.2 Use of Panels and Foil:
TFE-fluorocarbon lined caps.
8.2.1 For each location identified in 7.2, prepare test panels
5.31 Methanol—Low water grade (<0.008 % by K.F.)
in duplicate as a minimum or as agreed upon between the
5.32 Karl Fisher Titrator, or equivalent coulometric.
involved parties.
5.33 Reagents, appropriate for titrator.
NOTE 3—Thin steel panels 101.6 by 304.8 mm (4 by 12 in.) are
5.34 Associated Glassware, for the tests (pipetes, volumet-
preferred. If spray area is limited, smaller panels such as 101.6 by 152.4
ric flasks, etc). 1
mm (4 by 6 in.) can be used. Foils should be 13 mm ( ⁄2 in.) larger in size
5.35 Water, for calibration of the test instrument.
than the area to be sprayed for easiness in handling.
8.2.2 Specified time at which the samples need to be
Apparatus and Reagents for Solids Density (Test Methods
collected.The following is suggested as a guideline throughout
D2369, D1475, D2697; EPA Federal Reference Method 24):
the rest of this procedure:
5.36 Syringe, 5 mL.
(1) Immediately after paint application, (Sample A)
5.37 Weighing or Bottle with eye dropper.
(2) Entrance to Dehydration Ovens, (Sample B)
5.38 Test Tube, with new cork stopper.
(3) Exit of Dehydration Oven, (Sample C)
5.39 AluminumFoilDish,58mm(2.3in.)indiameterby18
Where only the dehydration oven is exhausted to the VOC
mm (0.71 in.) high with a smooth bottom surface.
Control Device for example calculations in Section 11.
5.40 Laboratory Force-Draft Bake Oven Type IIA or Type-
8.2.3 Preparation of Samples:
IIB, as specified in Specification E145.
8.2.3.1 Dry and label sufficient sheets of foil (i=1, ., n) for
5.41 Analytical Balance, with accuracy to 0.1 mg.
each test (A; B; C) to constant weight to remove residual
i i i
5.42 Toluene, minimum technical grade,
moisture.
5.43 Ethoxyethyl Acetate, minimum technical grade, Speci-
8.2.3.2 Record each foil weight (F ; F ; F ).
Ai Bi Ci
fication D343.
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. Coating Materials
future handling.
6.1 The coating materials used are to be in the “as applied
8.2.5 Weigh jars and lids prior to spraying. Record the data.
condition,” for example, representative of the specific formu-
Record each jar and lid weight (J ; J ; J ).
Ai Bi Ci
lation used in the coating process to be evaluated.
8.2.6 Prepare as a minimum one additional steel panel per
sprayout(forfilmthicknessverification)tobesprayedwiththe
7. Conditions
foiled panels. All panels can be sprayed simultaneously.
7.1 Prior to beginning the test, determine the following
Alternatively, the spraying could be broken into families of
conditions that represent the production process:
various panels for each one of the requested tests for % NV,
(1) Dry film thickness,
KF, and GC.
(2) Process sequence flash times,
NOTE 4—“Trip blanks” are analyzed for all parameters of interest. Trip
(3) Air flow,
blanks are often prepared by the laboratory and submitted to the sampling
(4) Percent solids content after dehydration, and
team when bottle ware is delivered. The trip blank accompanies all of the
(5) Temperature and humidity conditions for each signifi-
project samples through all custody changes in possession, coolers, and
cant step of the process. refrigerators. Trip blanks are not opened by the sampling team. The trip
D6266–00a (2005)
blanks provide information with respect to contamination that is “picked-
8.5.3.2 Determine the weight of methanol used for Sample
up” during sample packaging, shipping and storage.
M.
i
NOTE 5—The “field blank” is a portion of the sampling matrix that is
M 5L –K (2)
i i i
carried through the entire analytical scheme. The field blank is treated
exactly as the actual sample is treated. For example, the field blank vial is
where:
opened and closed when the corresponding sample vial is opened and
i = foil i,
closed. It is important that the volume/weight of the field blanks be the
L = weight of jar, lid, foil, paint and methanol, and
i
same as that of the samples.
K = weight of jar, lid, foil and paint.
i
8.3 Spraying Samples:
8.5.3.3 Calculate the % water (corrected for % water in the
8.3.1 Apply basecoat using an automated device (preferred
field blank) in the paint sample on a weight/weight basis as
for consistency) to target film build simulating assembly plant follows:
processing conditions.
%H O ~wt./wt.!5 (3)
8.4 Collection of Samples:
@~% water in sample!3~M 1P !– ~% water in field blank!~M !
i i i
8.4.1 At the sampling points specified in 8.2.2, the foil
P
i
samples for KF and GC analyses need to be placed in jars with
a specified solvent (8.5 and 8.6). The samples for % NV just
where:
need to be weighed at the sampl
...