1、Designation: D6266 00a (Reapproved 2017)Standard Test Method forDetermining the Amount of Volatile Organic Compound(VOC) Released From Waterborne Automotive Coatings andAvailable for Removal in a VOC Control Device(Abatement)1This standard is issued under the fixed designation D6266; the number imme
2、diately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This
3、 test method describes the determination of theamount of volatile organic compound (VOC) released fromapplied waterborne automotive coatings that is available fordelivery to a VOC control device. The determination isaccomplished by measuring the weight loss of a freshly coatedtest panel subject to e
4、vaporation or drying and by analysis ofthe VOC or water content in the coating.1.2 This test method is applicable to the VOC released fromapplication and baking operations after the paint has beenapplied in a simulation of a production process, or in an actualproduction facility.1.3 Symbols and calc
5、ulations from several other methodsthat determine VOC: Practice D3960, EPA 450/3-88-018 andEPA 450/3-84-019 have been incorporated into this testmethod. The majority of symbols and calculations used in thistest method are unique because this test method deals uniquelywith differences in weight of ap
6、plied paint samples that havebeen subject to drying, curing or solvent addition.NOTE 1Training and knowledge of the product being evaluated areessential for obtaining meaningful data from this test method. It isrecommended that several practice runs be performed, and the laboratoriesrepeatability ev
7、aluated before performing this test on the test samples.1.4 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.5 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresp
8、onsibility of whoever uses this standard to consult andestablish appropriate safety and health practices and deter-mine the applicability of regulatory limitations prior to its use.1.6 This international standard was developed in accor-dance with internationally recognized principles on standard-iza
9、tion established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D343 Specification for 2-Ethoxyethyl Acetate (95% Gra
10、de)(Withdrawn 1980)3D1186 Test Methods for Nondestructive Measurement ofDry Film Thickness of Nonmagnetic Coatings Applied toa Ferrous Base (Withdrawn 2006)3D1193 Specification for Reagent WaterD1475 Test Method For Density of Liquid Coatings, Inks,and Related ProductsD2369 Test Method for Volatile
11、Content of CoatingsD2697 Test Method for Volume Nonvolatile Matter in Clearor Pigmented CoatingsD3960 Practice for Determining Volatile Organic Compound(VOC) Content of Paints and Related CoatingsD4017 Test Method for Water in Paints and Paint Materialsby Karl Fischer MethodE145 Specification for Gr
12、avity-Convection and Forced-Ventilation OvensE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method2.2 U.S. EPA Standards:4EPA 450/3-88-018 (Dated December, 1988) EnvironmentalProtection Agency Protocol for Determining the DailyVolatile Organic Compound Emis
13、sion Rate ofAutomobileand Light Duty Truck Topcoat Operations. This protocol1This test method is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings, Materials, and Applications and is the direct responsibility ofSubcommittee D01.21 on Chemical Analysis of Paints and Paint Mate
14、rials.Current edition approved July 1, 2017. Published July 2017. Originally approvedin 1998. Last previous edition approved in 2011 as D6266 00a (2011). DOI:10.1520/D6266-00AR17.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org.
15、 For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.4Available from U.S. Government Printing Office Superintendent of Documents,732 N. Capitol St., NW
16、, 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 StatesThis international standard was developed in accordance with internationally recognized principles on standardization esta
17、blished in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.1describes procedures for determining VOC emission re-duction credit in abatement processes.EPA Federal R
18、eference 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 ofOrganic Compound Emitted by Paint, Ink, and OtherCoatings3. Summary of Test
19、 Method3.1 This procedure measures the loss of VOC from a freshlycoated surface by; (a) determining the difference in weight ofa coated test panel before and after various steps in a process,(b) analyzing a sample of the applied coating for VOC or watercontent, or both, by gas chromatography (GC), o
20、r Karl Fisher,or both, before and after various steps in a process, and (c)calculating the VOC directly or after subtracting the watercontent. With these analyses, it is possible to relate the VOCloss to the volume of solids deposited on the test panel at eachstep of a process. The information obtai
21、ned is used to deter-mine the amount of VOC available for removal by the VOCcontrol device at each step of a process (see Fig. 1).4. Significance and Use4.1 This test method provides basic engineering data thatmay be used to determine the amount of VOC delivered to theinlet of a VOC control device.
22、The procedure is useful forestablishing the quantity of VOC that is evolved from thecoating in the flash zone or bake oven and available to beincinerated, although the same procedure can be followedwhen other forms of VOC abatement are used.4.2 The total amount of VOC removed from the process bythe
23、VOC control device is a function of the amount available asgiven by this test method combined with the VOC removalefficiency of the control device.5. Apparatus and Materials for the AnalysesNOTE 2Purity of ReagentsReagent grade chemicals shall be used inall tests. Unless otherwise indicated, it is i
24、ntended that all reagents shallconform to the specification of the Committee on Analytical Reagents ofthe American Chemical Society, where such specifications are available.Other grades may be used, provided it is ascertained that the reagent is ofsufficiently high purity to permit its use without l
25、essening the accuracy ofthe determination. The references to purity of water, unless otherwiseindicated, shall be understood to mean Type II reagent grade waterconforming to Specification D1193.Sample Preparation:5.1 Thin Steel Panels, with an area of 310 cm2(48 in.2)orsmaller.5.2 Laboratory Balance
26、, with accuracy to 0.001 g (mini-mum).5.3 Laboratory Spray Booth, for application of the testcoating, with air flow representative of production conditions.5.4 Spray Application Equipment, selected to represent thatused in a production process or sufficiently similar that theequipment will produce c
27、omparable performance.5.5 Film Thickness Gage, for measuring dry paint thicknesson metal surfaces (see Test Methods D1186).5.6 Laboratory Force-Draft Bake Oven, Type-IIA or TypeIIB, as specified in Specification E145.5.7 Wide-Mouth Glass Jars, with TFE-fluorocarbon-linedcaps or polypropylene copolym
28、er bottles, one for each sample.5.8 Smooth Aluminum Foil, (grade may vary).5.9 Ultrasonic Cleaner unit, with 0.95 L (1 qt) capacityminimum.5.10 Laboratory Scale Paint Shaker (violent agitation) 3.8L (1-gal) capacity.5.11 Wood tongue Depressor or Tweezers, if desired to rollfoil.FIG. 1 Test Panel Pro
29、cessingD6266 00a (2017)2Apparatus and Reagents for GC Analysis:5.12 Gas Chromatograph, equipped with a flame ionizationdetector, electronic reporting integrator, capillary split injectionport, and autosampler (where available).5.13 Chromatographic Syringe, (10.0 L).5.14 Analytical Balance, accurate
30、to 0.1mg is needed, forthis method.5.15 Sealable Vials, (20 mL) scintillation.5.16 Medicine Droppers.5.17 Analytical Columncapillary, (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 ca
31、libration standard and internalstandard solutions.5.21 Bottles, with good sealing caps for standard solutions.5.22 Solvents Standards, expected to be found in the coatingto be tested.5.23 Tetrahydrofuran (THF)HPLC grade, uninhibited.5.24 Cyclohexanol98 % or appropriate grade reagent.5.25 Water.5.26
32、AcetoneHPLC grade.5.27 MethanolHPLC grade.5.28 Dimethylformamide (DMF)HPLC grade.5.29 Chromatography GasesHelium of 99.9995 % purityor 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 (VO
33、A) Vials, withTFE-fluorocarbon lined caps.5.31 MethanolLow 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, volumet-ric flasks, etc).5.35 Water, for calibration of the test ins
34、trument.Apparatus and Reagents for Solids Density (Test MethodsD2369, 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 18mm (0.71 in.) high with a s
35、mooth 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, Speci-fication D343.6. Coating Materials6.1 Th
36、e coating materials used are to be in the “as appliedcondition,” for example, representative of the specific formu-lation used in the coating process to be evaluated.7. Conditions7.1 Prior to beginning the test, determine the followingconditions that represent the production process:(1) Dry film thi
37、ckness,(2) Process sequence flash times,(3) Air flow,(4) Percent solids content after dehydration, and(5) Temperature and humidity conditions for each signifi-cant step of the process.7.1.1 With the information obtained, establish test param-eters that represent the range of conditions found in the
38、plant.Specific application parameters need not duplicate exact pro-duction conditions as long as the above parameters are con-trolled for this test.7.2 Identify all locations in the process sequence in whichflash zone/oven effluent is vented directly to a VOC controldevice. The number of locations w
39、ill affect the number of panelweight measurements taken and the number of panels that needto be tested.8. Procedures8.1 Parameters to Evaluate and General Method to CollectSamples:8.1.1 Parameters to be evaluated are as follows:(1) Determination of water content by Karl Fisher Titration(KF) or(2) De
40、termination of organic solvent content by gas chro-matography (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 panelsin duplicate as a minimum or as agreed upon be
41、tween theinvolved parties.NOTE 3Thin steel panels 101.6 by 304.8 mm (4 by 12 in.) arepreferred. If spray area is limited, smaller panels such as 101.6 by 152.4mm (4 by 6 in.) can be used. Foils should be 13 mm (12 in.) larger in sizethan the area to be sprayed for easiness in handling.8.2.2 Specifie
42、d time at which the samples need to becollected. The following is suggested as a guideline throughoutthe 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 e
43、xhausted to the VOCControl Device for example calculations in Section 11.8.2.3 Preparation of Samples:D6266 00a (2017)38.2.3.1 Dry and label sufficient sheets of foil (i=1, ., n) foreach test (Ai; Bi; Ci) to constant weight to remove residualmoisture.8.2.3.2 Record each foil weight (FAi; FBi; FCi).8
44、.2.4 Wrap or secure foils on panels so some area (mini-mum of12 in. (13 mm) per side) remains unpainted for thefuture handling.8.2.5 Weigh jars and lids prior to spraying. Record the data.Record each jar and lid weight (JAi; JBi; JCi).8.2.6 Prepare as a minimum one additional steel panel perspray ou
45、t (for film thickness verification) to be sprayed with thefoiled panels. All panels can be sprayed simultaneously.Alternatively, the spraying could be broken into families ofvarious panels for each one of the requested tests for % NV,KF, and GC.NOTE 4“Trip blanks” are analyzed for all parameters of
46、interest. Tripblanks are often prepared by the laboratory and submitted to the samplingteam when bottle ware is delivered. The trip blank accompanies all of theproject samples through all custody changes in possession, coolers, andrefrigerators. Trip blanks are not opened by the sampling team. The t
47、ripblanks provide information with respect to contamination that is “picked-up” during sample packaging, shipping and storage.NOTE 5The “field blank” is a portion of the sampling matrix that iscarried through the entire analytical scheme. The field blank is treatedexactly as the actual sample is tre
48、ated. For example, the field blank vial isopened and closed when the corresponding sample vial is opened andclosed. It is important that the volume/weight of the field blanks be thesame as that of the samples.8.3 Spraying Samples:8.3.1 Apply basecoat using an automated device (preferredfor consisten
49、cy) to target film build simulating assembly plantprocessing conditions.8.4 Collection of Samples:8.4.1 At the sampling points specified in 8.2.2, the foilsamples for KF and GC analyses need to be placed in jars witha specified solvent (8.5 and 8.6). The samples for % NV justneed to be weighed at the sampling point. Then, they are bakedat final bake condition and re-weighed.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 sizedepending upon foil size. Weigh jars, lids, and coated foils.Record we
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