1、Designation: D 6266 00a (Reapproved 2005)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 D 6266; the number im
2、mediately 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 (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 T
3、his 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 t
4、o evaporation 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 c
5、alculations from several other methodsthat determine VOC: Practice D 3960, 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 o
6、f applied 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 laboratoriesrepeatabilit
7、y evaluated 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 the
8、responsibility 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.2. Referenced Documents2.1 ASTM Standards:2D 343 Specification for 2Ethoxyethyl Acetate (95 %)Grade3D 1186 Test Met
9、hods for Nondestructive Measurement ofDry Film Thickness of Nonmagnetic Coatings Applied toa Ferrous BaseD 1193 Specification for Reagent WaterD 1475 Test Method for Density of Liquid Coatings, Inks,and Related ProductsD 2369 Test Method for Volatile Content of CoatingsD 2697 Test Method for Volume
10、Nonvolatile Matter inClear or Pigmented CoatingsD 3960 Practice for Determining Volatile Organic com-pound (VOC) Content of Paints and Related CoatingsD 4017 Test Method for Water in Paints and Paint Materialsby Karl Fisher MethodE 145 Specification for Gravity-Convention and Forced-Ventilation Oven
11、sE 691 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 Emission Rate ofAutomobileand Light Duty Truck
12、 Topcoat Operations. This protocoldescribes procedures for determining VOC emission re-duction credit in abatement processes.EPA Federal Reference Method 24 - (Ref. 40CFR, part 60,Appendix A). Determination of Volatile Matter Content,1This test method is under the jurisdiction of ASTM Committee D01
13、on Paintand Related Coatings, Materials, and Applications and is the direct responsibility ofSubcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.Current edition approved July 1, 2005. Published August 2005. Originallyapproved in 1998. Last previous edition approved in 2000 as D 62
14、66 00a.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Withdrawn.4Available from the Superintendent of Docum
15、ents, U.S. Government PrintingOffice, Washington, DC 20402.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.Water Content, Density, Volume Solids and Weight Solids,of Surface Coatings.EPA 450/3-84-019 Procedures for Certifying Quantit
16、y ofOrganic Compound Emitted by Paint, Ink, and OtherCoatings3. Summary of Test 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
17、applied coating for VOC or watercontent, 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 watercontent. With these analyses, it is possible to relate the VOCloss to the volume of sol
18、ids deposited on the test panel at eachstep of a process. The information obtained 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
19、 to determine the amount of VOC delivered to theinlet of a VOC control device. 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
20、 abatement are used.4.2 The total amount of VOC removed from the process bythe 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
21、 grade chemicals shall be used inall tests. Unless otherwise indicated, it is intended 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 ascerta
22、ined that the reagent is ofsufficiently high purity to permit its use without lessening the accuracy ofthe determination. The references to purity of water, unless otherwiseindicated, shall be understood to mean Type II reagent grade waterconforming to Specification D 1193.Sample Preparation:5.1 Thi
23、n Steel Panels, with an area of 310 cm2(48 in.2)orsmaller.5.2 Laboratory Balance, 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
24、in a production process or sufficiently similar that theequipment will produce comparable performance.5.5 Film Thickness Gage, for measuring dry paint thicknesson metal surfaces (see Test Methods D 1186).5.6 Laboratory Force-Draft Bake Oven, Type-IIA or TypeIIB, as specified in Specification E 145.5
25、.7 Wide-Mouth Glass Jars, with TFE-fluorocarbon-linedcaps or polypropylene copolymer 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.
26、11 Wood tongue Depressor or Tweezers, if desired to rollfoil.Apparatus 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
27、L).5.14 Analytical Balance, accurate to 0.1mg is needed, forthis method.5.15 Sealable Vials, (20 mL) scintillation.5.16 Medicine Droppers.FIG. 1 Test Panel ProcessingD 6266 00a (2005)25.17 Analytical Columncapillary, (30 meter) (0.25 mm)inside diameter,5.17.1 film thickness, fused silica DB-5 or equ
28、ivalent.5.18 Autosampler Vials.5.19 Pipet, Volumetric.5.20 Volumetric Flask, for calibration 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 gra
29、de, uninhibited.5.24 Cyclohexanol98 % or appropriate grade reagent.5.25 Water.5.26 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 hydrocarb
30、ons.Apparatus and Reagents for KF Analysis:5.30 40-mL Volatile Organic Analysis (VOA) 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 t
31、ests (pipetes, volumet-ric flasks, etc).5.35 Water, for calibration of the test instrument.Apparatus and Reagents for Solids Density (Test MethodsD 2369, D 1475, D 2697; EPA Federal Reference Method24):5.36 Syringe, 5 mL.5.37 Weighing or Bottle with eye dropper.5.38 Test Tube, with new cork stopper.
32、5.39 Aluminum Foil Dish, 58 mm (2.3 in.) in diameter by 18mm (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 E 145.5.41 Analytical Balance, with accuracy to 0.1 mg.5.42 Toluene, minimum technical grade,5.43 Ethoxy
33、ethyl Acetate, minimum technical grade, Speci-fication D 343.6. Coating Materials6.1 The 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, d
34、etermine the followingconditions 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 signifi-cant step of the process.7.1.1 With the information ob
35、tained, establish test param-eters that represent the range of conditions found in the 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
36、zone/oven effluent is vented directly to a VOC controldevice. The number of locations will 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
37、are as follows:(1) Determination of water content by Karl Fisher Titration(KF) or(2) Determination 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 locati
38、on identified in 7.2, prepare test panelsin duplicate as a minimum or as agreed upon between 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
39、 in.) larger in sizethan the area to be sprayed for easiness in handling.8.2.2 Specified 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,
40、 (Sample B)(3) Exit of Dehydration Oven, (Sample C)Where only the dehydration oven is exhausted to the VOCControl 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) foreach test (Ai; Bi; Ci) to constant weight to rem
41、ove residualmoisture.8.2.3.2 Record each foil weight (FAi; FBi; FCi).8.2.4 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;
42、JCi).8.2.6 Prepare as a minimum one additional steel panel perspray out (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 %
43、 NV,KF, and GC.NOTE 4“Trip blanks” are analyzed for all parameters of 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, an
44、drefrigerators. Trip blanks are not opened by the sampling team. The tripD 6266 00a (2005)3blanks 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
45、 entire analytical scheme. The field blank is treatedexactly as the actual sample is treated. 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
46、 Spraying Samples:8.3.1 Apply basecoat using an automated device (preferredfor consistency) 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
47、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 upo
48、n foil size. Weigh jars, lids, and coated foils.Record weights (KAi; KBi; KCi) including field blanks (see8.2.6).8.4.4 Fold foils paint side in for%NV(8.7).8.5 Water Content by KF:8.5.1 Water Content Solvent Preparation:8.5.1.1 Analyze a sample of the bulk methanol for watercontent by the Karl Fisch
49、er Method in accordance with TestMethod D 4017 to check purity of reagent.8.5.1.2 Fill each jar (as described in 8.4.1.1) with 30 mL ofmethanol. Foil should be completely submerged in methanol.8.5.1.3 Reweigh jars, lids, coated foils and methanol andrecord weights (LAi; LBi; LCi).8.5.1.4 Place the capped jars containing methanol and foilstrips into an ultrasonic cleaning unit until sample is uniformlydispersed into the methanol.8.5.2 Sample Analysis:8.5.2.1 Follow the procedure for KF Titration in accordancewith Test Method D 4017.8.5.2.2 Fill a 5.0-mL disposable
