ASTM D6266-00a(2011)

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)

SIGNIFICANCE AND USE
This test method provides basic engineering data that may be used to determine the amount of VOC delivered to the inlet of a VOC control device. The procedure is useful for establishing the quantity of VOC that is evolved from the coating in the flash zone or bake oven and available to be incinerated, although the same procedure can be followed when other forms of VOC abatement are used.
The total amount of VOC removed from the process by the VOC control device is a function of the amount available as given by this test method combined with the VOC removal efficiency of the control device.
SCOPE
1.1 This test method describes the determination of the amount of volatile organic compound (VOC) released from applied waterborne automotive coatings that is available for delivery to a VOC control device. The determination is accomplished by measuring the weight loss of a freshly coated test panel subject to evaporation or drying and by analysis of the VOC or water content in the coating.
1.2 This test method is applicable to the VOC released from application and baking operations after the paint has been applied in a simulation of a production process, or in an actual production facility.
1.3 Symbols and calculations from several other methods that determine VOC: Practice D3960, EPA 450/3-88-018 and EPA 450/3-84-019 have been incorporated into this test method. The majority of symbols and calculations used in this test method are unique because this test method deals uniquely with differences in weight of applied paint samples that have been subject to drying, curing or solvent addition.
Note 1—Training and knowledge of the product being evaluated are essential for obtaining meaningful data from this test method. It is recommended that several practice runs be performed, and the laboratories repeatability evaluated before performing this test on the test samples.
1.4 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of whoever uses this standard to consult and establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to its use.

General Information

• Status: Historical
• Publication Date: 31-May-2011
• ICS: 43.040.60 - Bodies and body components
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.21 - Chemical Analysis of Paints and Paint Materials

Relations

• Replaces: ASTM D6266-00a(2005) - 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)
• Effective Date: 01-Jun-2011

Standards Content (Sample)

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 (Reapproved 2011)
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
2.1 ASTM Standards:
1.1 This test method describes the determination of the
D343 Specification for 2-Ethoxyethyl Acetate (95% Grade)
amount of volatile organic compound (VOC) released from
(Withdrawn 1980)
applied waterborne automotive coatings that is available for
D1186 Test Methods for Nondestructive Measurement of
delivery to a VOC control device. The determination is
Dry Film Thickness of Nonmagnetic Coatings Applied to
accomplished by measuring the weight loss of a freshly coated
a Ferrous Base (Withdrawn 2006)
test panel subject to evaporation or drying and by analysis of
D1193 Specification for Reagent Water
the VOC or water content in the coating.
D1475 Test Method For Density of Liquid Coatings, Inks,
1.2 This test method is applicable to theVOC released from
and Related Products
application and baking operations after the paint has been
D2369 Test Method for Volatile Content of Coatings
applied in a simulation of a production process, or in an actual
D2697 Test Method for Volume Nonvolatile Matter in Clear
production facility.
or Pigmented Coatings
D3960 PracticeforDeterminingVolatileOrganicCompound
1.3 Symbols and calculations from several other methods
(VOC) Content of Paints and Related Coatings
that determine VOC: Practice D3960, EPA 450/3-88-018 and
D4017 Test Method for Water in Paints and Paint Materials
EPA 450/3-84-019 have been incorporated into this test
by Karl Fischer Method
method. The majority of symbols and calculations used in this
E145 Specification for Gravity-Convection and Forced-
test method are unique because this test method deals uniquely
Ventilation Ovens
with differences in weight of applied paint samples that have
E691 Practice for Conducting an Interlaboratory Study to
been subject to drying, curing or solvent addition.
Determine the Precision of a Test Method
NOTE 1—Training and knowledge of the product being evaluated are
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-
duction credit in abatement processes.
1.5 This standard does not purport to address all of the
EPA Federal Reference Method 24 - (Ref. 40CFR, part 60,
safety concerns, if any, associated with its use. It is the
Appendix A) Determination of Volatile Matter Content,
responsibility of whoever uses this standard to consult and
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 [e-mail]. 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 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 June 1, 2011. Published June 2011. Originally AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
approved in 1998. Last previous edition approved in 2005 as D6266 – 00a (2005). 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
DOI: 10.1520/D6266-00AR11. www.access.gpo.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D6266 − 00a (2011)
sufficiently high purity to permit its use without lessening the accuracy of
WaterContent,Density,VolumeSolidsandWeightSolids,
the determination. The references to purity of water, unless otherwise
of Surface Coatings.
indicated, shall be understood to mean Type II reagent grade water
EPA 450/3-84-019 Procedures for Certifying Quantity of
conforming to Specification D1193.
Organic Compound Emitted by Paint, Ink, and Other
Coatings Sample Preparation:
2 2
5.1 Thin Steel Panels, with an area of 310 cm (48 in.)or
3. Summary of Test Method
smaller.
3.1 ThisproceduremeasuresthelossofVOCfromafreshly
5.2 Laboratory Balance, with accuracy to 0.001 g (mini-
coated surface by; (a) determining the difference in weight of
mum).
a coated test panel before and after various steps in a process,
(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
step of a process. The information obtained is used to deter-
5.5 Film Thickness Gage, for measuring dry paint thickness
mine the amount of VOC available for removal by the VOC
on metal surfaces (see Test Methods D1186).
control device at each step of a process (see Fig. 1).
5.6 Laboratory Force-Draft Bake Oven, Type-IIA or Type
IIB, as specified in Specification E145.
4. Significance and Use
4.1 This test method provides basic engineering data that 5.7 Wide-Mouth Glass Jars, with TFE-fluorocarbon-lined
caps or polypropylene copolymer bottles, one for each sample.
may be used to determine the amount of VOC delivered to the
inlet of a VOC control device. The procedure is useful for
5.8 Smooth Aluminum Foil, (grade may vary).
establishing the quantity of VOC that is evolved from the
5.9 Ultrasonic Cleaner unit, with 0.95 L (1 qt) capacity
coating in the flash zone or bake oven and available to be
minimum.
incinerated, although the same procedure can be followed
when other forms of VOC abatement are used.
5.10 Laboratory Scale Paint Shaker (violent agitation) 3.8
L (1-gal) capacity.
4.2 The total amount of VOC removed from the process by
theVOCcontroldeviceisafunctionoftheamountavailableas
5.11 Wood tongue Depressor or Tweezers, if desired to roll
given by this test method combined with the VOC removal
foil.
efficiency of the control device.
Apparatus and Reagents for GC Analysis:
5. Apparatus and Materials for the Analyses
5.12 Gas Chromatograph, equipped with a flame ionization
NOTE2—PurityofReagents—Reagentgradechemicalsshallbeusedin
all tests. Unless otherwise indicated, it is intended that all reagents shall detector,electronicreportingintegrator,capillarysplitinjection
conform to the specification of the Committee on Analytical Reagents of
port, and autosampler (where available).
the American Chemical Society, where such specifications are available.
Other grades may be used, provided it is ascertained that the reagent is of 5.13 Chromatographic Syringe, (10.0 µL).
FIG. 1 Test Panel Processing
D6266 − 00a (2011)
5.14 Analytical Balance, accurate to 0.1mg is needed, for 6. Coating Materials
this method.
6.1 The coating materials used are to be in the “as applied
5.15 Sealable Vials, (20 mL) scintillation. condition,” for example, representative of the specific formu-
lation used in the coating process to be evaluated.
5.16 Medicine Droppers.
5.17 Analytical Column—capillary, (30 meter) (0.25 mm)
7. Conditions
inside diameter,
7.1 Prior to beginning the test, determine the following
5.17.1 film thickness, fused silica DB-5 or equivalent.
conditions that represent the production process:
5.18 Autosampler Vials.
(1) Dry film thickness,
(2) Process sequence flash times,
5.19 Pipet, Volumetric.
(3) Air flow,
5.20 Volumetric Flask, for calibration standard and internal
(4) Percent solids content after dehydration, and
standard solutions.
(5) Temperature and humidity conditions for each signifi-
cant step of the process.
5.21 Bottles, with good sealing caps for standard solutions.
7.1.1 With the information obtained, establish test param-
5.22 SolventsStandards,expectedtobefoundinthecoating
eters that represent the range of conditions found in the plant.
to be tested.
Specific application parameters need not duplicate exact pro-
5.23 Tetrahydrofuran (THF)—HPLC grade, uninhibited. duction conditions as long as the above parameters are con-
trolled for this test.
5.24 Cyclohexanol—98 % or appropriate grade reagent.
7.2 Identify all locations in the process sequence in which
5.25 Water.
flash zone/oven effluent is vented directly to a VOC control
5.26 Acetone—HPLC grade.
device.Thenumberoflocationswillaffectthenumberofpanel
weightmeasurementstakenandthenumberofpanelsthatneed
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
or higher. Hydrogen of 99.9995 % minimum purity.Air, “dry”
8.1 Parameters to Evaluate and General Method to Collect
quality, free of hydrocarbons.
Samples:
8.1.1 Parameters to be evaluated are as follows:
Apparatus and Reagents for KF Analysis:
(1) Determination of water content by Karl FisherTitration
5.30 40-mL Volatile Organic Analysis (VOA) Vials, with
(KF) or
TFE-fluorocarbon lined caps.
(2) Determination of organic solvent content by gas chro-
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:
5.34 Associated Glassware, for the tests (pipetes, volumet- 8.2.1 For each location identified in 7.2, prepare test panels
ric flasks, etc). in duplicate as a minimum or as agreed upon between the
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
D2369, D1475, D2697; EPA Federal Reference Method 24):
mm (4 by 6 in.) can be used. Foils should be 13 mm ( ⁄2 in.) larger in size
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
the rest of this procedure:
5.38 Test Tube, with new cork stopper.
(1) Immediately after paint application, (Sample A)
5.39 AluminumFoilDish,58mm(2.3in.)indiameterby18
(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.
8.2.3 Preparation of Samples:
5.41 Analytical Balance, with accuracy to 0.1 mg.
8.2.3.1 Dry and label sufficient sheets of foil (i=1, ., n) for
5.42 Toluene, minimum technical grade,
each test (A; B; C) to constant weight to remove residual
i i i
moisture.
5.43 Ethoxyethyl Acetate, minimum technical grade, Speci-
fication D343. 8.2.3.2 Record each foil weight (F ; F ; F ).
Ai Bi Ci
D6266 − 00a (2011)
8.2.4 Wrap or secure foils on panels so some area (mini- 8.5.2 Sample Analysis:
mum of ⁄2 in. (13 mm) per side) remains unpainted for the 8.5.2.1 Follow the procedure for KFTitration in accordance
future handling. with Test Method D4017.
8.2.5 Weigh jars and lids prior to spraying. Record the data. 8.5.2.2 Fill a 5.0-mL disposable syringe with a well mixed
Record each jar and lid weight (J ; J ; J ). representative portion of the methanol from one of the glass
Ai Bi Ci
8.2.6 Prepare as a minimum one additional steel panel per sample jars. Perform this step in a low humidity room or
sprayout(forfilmthicknessverification)tobesprayedwiththe chamber.
foiled panels. All panels can be sprayed simultaneously. 8.5.2.3 Weigh and transfer enough of each sample into the
Alternatively, the spraying could be broken into families of Karl Fischer titration vessels so that at least 10 mL of KF
various panels for each one of the requested tests for % NV, reagent will be required to reach the endpoint. Repeat for each
KF, and GC. sample and all blank vials.
8.5.3 Calculation of % Water in the Paint Sample on a
NOTE 4—“Trip blanks” are analyzed for all parameters of interest. Trip
Wt./Wt. Basis:
blanks are often prepared by the laboratory and submitted to the sampling
8.5.3.1 Determine the weight of sample paint on the foil P
team when bottle ware is delivered. The trip blank accompanies all of the
i
project samples through all custody changes in possession, coolers, and
as follows:
refrigerators. Trip blanks are not opened by the sampling team. The trip
P 5 K 2 F 1J (1)
~ !
i i i i
blanks provide information with respect to contamination that is “picked-
up” during sample packaging, shipping and storage.
where:
NOTE 5—The “field blank” is a portion of the sampling matrix that is
carried through the entire analytical scheme. The field blank is treated i = foil i,
exactly as the actual sample is treated. For example, the field blank vial is K = weight of jar, lid, foil and paint (4.1.1),
i
opened and closed when the corresponding sample vial is opened and
F = weight of foil (8.2.3.2), and
i
closed. It is important that the volume/weight of the field blanks be the
J = weight of jar and lid (8.2.5).
i
same
...

This document is not anASTM standard and is intended only to provide the user of anASTM 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:D6266–00a(Reapproved2005) Designation:D6266–00a(Reapproved2011)
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
1.1 This test method describes the determination of the amount of volatile organic compound (VOC) released from applied
waterborne automotive coatings that is available for delivery to a VOC control device. The determination is accomplished by
measuring the weight loss of a freshly coated test panel subject to evaporation or drying and by analysis of the VOC or water
content in the coating.
1.2 This test method is applicable to the VOC released from application and baking operations after the paint has been applied
in a simulation of a production process, or in an actual production facility.
1.3 Symbols and calculations from several other methods that determine VOC: Practice D3960, EPA 450/3-88-018 and EPA
450/3-84-019 have been incorporated into this test method. The majority of symbols and calculations used in this test method are
uniquebecausethistestmethoddealsuniquelywithdifferencesinweightofappliedpaintsamplesthathavebeensubjecttodrying,
curing or solvent addition.
NOTE 1—Training and knowledge of the product being evaluated are essential for obtaining meaningful data from this test method. It is recommended
that several practice runs be performed, and the laboratories repeatability evaluated before performing this test on the test samples.
1.4 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of whoever uses this standard to consult and establish appropriate safety and health practices and determine the applicability of
regulatory limitations prior to its use.
2. Referenced Documents
2.1 ASTM Standards:
D343 Specification for 2–Wthoxyethyl Acetate (95% Grade) Specification for 2-Ethoxyethyl Acetate (95% Grade)
D1186 Test Methods for Nondestructive Measurement of Dry Film Thickness of Nonmagnetic Coatings Applied to a Ferrous
Base
D1193 Specification for Reagent Water
D1475 Test Method For Density of Liquid Coatings, Inks, and Related Products
D2369 Test Method for Volatile Content of Coatings
D2697 Test Method for Volume Nonvolatile Matter in Clear or Pigmented Coatings
D3960 Practice for Determining Volatile Organic Compound (VOC) Content of Paints and Related Coatings
D4017 Test Method for Water in Paints and Paint Materials by Karl Fischer Method
E145 Specification for Gravity-Convection and Forced-Ventilation Ovens
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
2.2 U.S. EPA Standards:
EPA 450/3-88-018 (Dated December, 1988) Environmental Protection Agency Protocol for Determining the Daily Volatile
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 JulyJune 1, 2005.2011. Published August 2005.June 2011. Originally approved in 1998. Last previous edition approved in 20002005 as
D6266 – 00a (2005). DOI: 10.1520/D6266-00AR0511.
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at [e-mail]. ForAnnualBookofASTMStandards
volume information, refer to the standard’s Document Summary page on the ASTM website.
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D6266–00a (2011)
Organic Compound Emission Rate of Automobile and Light Duty Truck Topcoat Operations. This protocol describes
procedures for determining VOC emission reduction credit in abatement processes.
EPA Federal Reference Method 24 - (Ref. 40CFR, part 60, Appendix A) Determination of Volatile Matter Content, Water
Content, Density, Volume Solids and Weight Solids, of Surface Coatings.
EPA 450/3-84-019 Procedures for Certifying Quantity of Organic Compound Emitted by Paint, Ink, and Other Coatings
3. Summary of Test Method
3.1 This procedure measures the loss of VOC from a freshly coated surface by; (a) determining the difference in weight of a
coated test panel before and after various steps in a process, (b) analyzing a sample of the applied coating for VOC or water
content, or both, by gas chromatography (GC), or Karl Fisher, or both, before and after various steps in a process, and (c)
calculating the VOC directly or after subtracting the water content. With these analyses, it is possible to relate the VOC loss to
thevolumeofsolidsdepositedonthetestpanelateachstepofaprocess.Theinformationobtainedisusedtodeterminetheamount
of VOC available for removal by the VOC control device at each step of a process (see Fig. 1).
4. Significance and Use
4.1 This test method provides basic engineering data that may be used to determine the amount of VOC delivered to the inlet
of aVOC control device.The procedure is useful for establishing the quantity ofVOC that is evolved from the coating in the flash
zone or bake oven and available to be incinerated, although the same procedure can be followed when other forms of VOC
abatement are used.
4.2 The total amount of VOC removed from the process by the VOC control device is a function of the amount available as
given by this test method combined with the VOC removal efficiency of the control device.
5. Apparatus and Materials for the Analyses
NOTE 2—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 specification of the Committee onAnalytical Reagents of theAmerican 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 the
determination. The references to purity of water, unless otherwise indicated, shall be understood to mean Type II reagent grade water conforming to
Specification D1193.
Sample Preparation:
2 2
5.1 Thin Steel Panels, with an area of 310 cm (48 in. ) or smaller.
5.2 Laboratory Balance, with accuracy to 0.001 g (minimum).
5.3 Laboratory Spray Booth, for application of the test coating, with air flow representative of production conditions.
5.4 Spray Application Equipment , selected to represent that used in a production process or sufficiently similar that the
equipment will produce comparable performance.
5.5 Film Thickness Gage, for measuring dry paint thickness on metal surfaces (see Test Methods D1186).
5.6 Laboratory Force-Draft Bake Oven, Type-IIA or Type IIB, as specified in Specification E145.
5.7 Wide-Mouth Glass Jars, with TFE-fluorocarbon-lined caps or polypropylene copolymer bottles, one for each sample.
5.8 Smooth Aluminum Foil, (grade may vary).
FIG. 1 Test Panel Processing
D6266–00a (2011)
5.9 Ultrasonic Cleaner unit, with 0.95 L (1 qt) capacity minimum.
5.10 Laboratory Scale Paint Shaker (violent agitation) 3.8 L (1-gal) capacity.
5.11 Wood tongue Depressor or Tweezers, if desired to roll foil.
Apparatus and Reagents for GC Analysis:
5.12 Gas Chromatograph, equipped with a flame ionization detector, electronic reporting integrator, capillary split injection
port, and autosampler (where available).
5.13 Chromatographic Syringe, (10.0 µL).
5.14 Analytical Balance, accurate to 0.1mg is needed, for this method.
5.15 Sealable Vials, (20 mL) scintillation.
5.16 Medicine Droppers.
5.17 Analytical Column—capillary, (30 meter) (0.25 mm) inside diameter,
5.17.1 film thickness, fused silica DB-5 or equivalent.
5.18 Autosampler Vials.
5.19 Pipet, Volumetric.
5.20 Volumetric Flask, for calibration standard and internal standard solutions.
5.21 Bottles, with good sealing caps for standard solutions.
5.22 Solvents Standards, expected to be found in the coating to be tested.
5.23 Tetrahydrofuran (THF)—HPLC grade, uninhibited.
5.24 Cyclohexanol—98 % or appropriate grade reagent.
5.25 Water.
5.26 Acetone—HPLC grade.
5.27 Methanol—HPLC grade.
5.28 Dimethylformamide (DMF)—HPLC grade.
5.29 Chromatography Gases—Helium of 99.9995 % purity or higher. Hydrogen of 99.9995 % minimum purity. Air, “dry”
quality, free of hydrocarbons.
Apparatus and Reagents for KF Analysis:
5.30 40-mL Volatile Organic Analysis (VOA) Vials, with TFE-fluorocarbon lined caps.
5.31 Methanol—Low water grade (<0.008 % by K.F.)
5.32 Karl Fisher Titrator, or equivalent coulometric.
5.33 Reagents, appropriate for titrator.
5.34 Associated Glassware, for the tests (pipetes, volumetric flasks, etc).
5.35 Water, for calibration of the test instrument.
Apparatus and Reagents for Solids Density (Test Methods D2369, D1475, D2697; EPA Federal Reference Method 24):
5.36 Syringe, 5 mL.
5.37 Weighing or Bottle with eye dropper.
5.38 Test Tube, with new cork stopper.
5.39 Aluminum Foil Dish, 58 mm (2.3 in.) in diameter by 18 mm (0.71 in.) high with a smooth bottom surface.
5.40 Laboratory Force-Draft Bake Oven Type IIA or Type-IIB, as specified in Specification E145.
5.41 Analytical Balance, with accuracy to 0.1 mg.
5.42 Toluene, minimum technical grade,
5.43 Ethoxyethyl Acetate, minimum technical grade, Specification D343.
6. Coating Materials
6.1 The coating materials used are to be in the “as applied condition,” for example, representative of the specific formulation
used in the coating process to be evaluated.
7. Conditions
7.1 Prior to beginning the test, determine the following conditions that represent the production process:
(1) Dry film thickness,
(2) Process sequence flash times,
(3) Air flow,
(4) Percent solids content after dehydration, and
(5) Temperature and humidity conditions for each significant step of the process.
7.1.1 With the information obtained, establish test parameters that represent the range of conditions found in the plant. Specific
application parameters need not duplicate exact production conditions as long as the above parameters are controlled for this test.
7.2 Identify all locations in the process sequence in which flash zone/oven effluent is vented directly to a VOC control device.
D6266–00a (2011)
The number of locations will affect the number of panel weight measurements taken and the number of panels that need to be
tested.
8. Procedures
8.1 Parameters to Evaluate and General Method to Collect Samples:
8.1.1 Parameters to be evaluated are as follows:
(1) Determination of water content by Karl Fisher Titration (KF) or
(2) Determination of organic solvent content by gas chromatography (GC), or both, and
(3) Determination of volatiles and nonvolatiles (% NV) during flash/baking operations.
8.2 Use of Panels and Foil:
8.2.1 For each location identified in 7.2, prepare test panels in duplicate as a minimum or as agreed upon between the involved
parties.
NOTE 3—Thin steel panels 101.6 by 304.8 mm (4 by 12 in.) are 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 than the area to be sprayed for easiness in handling.
8.2.2 Specified time at which the samples need to be collected. The following is suggested as a guideline throughout the rest
of this procedure:
(1) Immediately after paint application, (Sample A)
(2) Entrance to Dehydration Ovens, (Sample B)
(3) Exit of Dehydration Oven, (Sample C)
Where only the dehydration oven is exhausted to the VOC Control Device for example calculations in Section 11.
8.2.3 Preparation of Samples:
8.2.3.1 Dry and label sufficient sheets of foil (i=1, ., n) for each test (A;B;C) to constant weight to remove residual moisture.
i i i
8.2.3.2 Record each foil weight (F ; F ; F ).
Ai Bi Ci
8.2.4 Wrap or secure foils on panels so some area (minimum of ⁄2 in. (13 mm) per side) remains unpainted for the future
handling.
8.2.5 Weigh jars and lids prior to spraying. Record the data. Record each jar and lid weight (J ; J ; J ).
Ai Bi Ci
8.2.6 Prepareasaminimumoneadditionalsteelpanelpersprayout(forfilmthicknessverification)tobesprayedwiththefoiled
panels. All panels can be sprayed simultaneously. Alternatively, the spraying could be broken into families of various panels for
each one of the requested tests for % NV, KF, and GC.
NOTE 4—“Trip blanks” are analyzed for all parameters of interest.Trip blanks are often prepared by the laboratory and submitted to the sampling team
when bottle ware is delivered.The trip blank accompanies all of the project samples through all custody changes in possession, coolers, and refrigerators.
Trip blanks are not opened by the sampling team. The trip blanks provide information with respect to contamination that is “picked-up” during sample
packaging, shipping and storage.
NOTE 5—The “field blank” is a portion of the sampling matrix that is 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 opened and closed when the corresponding sample vial is opened and closed. It is
important that the volume/weight of the field blanks be the same as that of the samples.
8.3 Spraying Samples:
8.3.1 Apply basecoat using an automated device (preferred for consistency) to target film build simulating assembly plant
processing conditions.
8.4 Collection of Samples:
8.4.1 Atthesamplingpointsspecifiedin8.2.2,thefoilsamplesforKFandGCanalysesneedtobeplacedinjarswithaspecified
solvent (8.5 and 8.6). The samples for % NV just need to be weighed at the sampling point. Then, they are baked at final bake
condition and re-weighed.
8.4.2 Roll up foil paint side out for KF (8.5) and GC (8.6)
...