1、Designation: D5403 93 (Reapproved 2013)Standard Test Methods forVolatile Content of Radiation Curable Materials1This standard is issued under the fixed designation D5403; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of
2、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 These test methods cover procedures for the determina-tion of weight percent volatile content of coatings, inks, andad
3、hesives designed to be cured by exposure to ultraviolet lightor to a beam of accelerated electrons.1.2 Test Method A is applicable to radiation curable mate-rials that are essentially 100 % reactive but may contain traces(no more than 3 %) of volatile materials as impurities orintroduced by the incl
4、usion of various additives.1.3 Test Method B is applicable to all radiation curablematerials but must be used for materials that contain volatilesolvents intentionally introduced to control application viscos-ity and which are intended to be removed from the materialprior to cure.1.4 These test meth
5、ods may not be applicable to radiationcurable materials wherein the volatile material is water, andother procedures may be substituted by mutual consent of theproducer and user.1.5 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard
6、.1.6 This standard does not purport to address all of thesafety problems, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. A specific ha
7、zardstatement is given in 15.7.2. Referenced Documents2.1 ASTM Standards:2D2369 Test Method for Volatile Content of CoatingsE145 Specification for Gravity-Convection and Forced-Ventilation OvensE177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE691 Practice for Conducting an I
8、nterlaboratory Study toDetermine the Precision of a Test Method3. Terminology3.1 Definitions:3.1.1 cure, nthe condition of a coating after conversion tothe final state of cure as measured by tests generally related toend use performance and mutually agreeable to supplier andpurchaser.3.1.2 ultraviol
9、et (UV) curing, nconversion of a coatingfrom its application state to its final use state by means of amechanism initiated by ultraviolet radiation generated byequipment designed for that purpose.3.1.3 electron beam (EB) curing, nconversion of a coatingfrom its application state to its final use sta
10、te by means of amechanism initiated by electron beam radiation generated byequipment designed for that purpose.3.1.4 processing volatiles, nloss in specimen weight undertest conditions that are designed to simulate actual industrialcure processing conditions.3.1.5 potential volatiles, nloss in speci
11、men weight uponheating at 110C for 60 min after radiation curing.3.1.5.1 DiscussionThis value is an estimation of volatileloss that may occur during aging or under extreme storageconditions. Potential volatiles may also be referred to asresidual volatiles.3.1.6 total volatiles, nsum of the processin
12、g volatiles andthe potential volatiles.4. Summary of Test Methods4.1 A designated quantity of material is weighed before andafter a cure step that simulates normal industrial processing.The test specimen is weighed again after heating at 110 6 5Cfor 60 min. The percent volatile is calculated from th
13、e losses inweight.5. Significance and Use5.1 These test methods are the procedures of choice fordetermining volatile content of materials designed to be cured1These test methods are under the jurisdiction of ASTM Committee D01 onPaint and Related Coatings, Materials, and Applications and are the dir
14、ectresponsibility of Subcommittee D01.55 on Factory Applied Coatings on PreformedProducts.Current edition approved June 1, 2013. Published July 2013. Originally approvedin 1993. Last previous edition approved in 2007 as D5403 93 (2007). DOI:10.1520/D5403-93R13.2For referenced ASTM standards, visit t
15、he 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.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959.
16、United States1by exposure to ultraviolet light or electron beam irradiation.These types of materials contain liquid reactants that react tobecome part of the film during cure, but, which under the testconditions of Test Method D2369, will be erroneously mea-sured as volatiles. The conditions of thes
17、e test methods aresimilar to Test Method D2369 with the inclusion of a step tocure the material prior to weight loss determination. Volatilecontent is determined as two separate componentsprocessingvolatiles and potential volatiles. Processing volatiles is ameasure of volatile loss during the actual
18、 cure process.Potential volatiles is a measure of volatile loss that might occurduring aging or under extreme storage conditions. Thesevolatile content measurements are useful to the producer anduser of a material and to environmental interests for determin-ing emissions.6. Interferences6.1 The degr
19、ee to which the results of these proceduresaccurately measure the volatiles emitted during actual use isabsolutely dependent upon proper cure during the test proce-dure. Although overcure will have little or no effect uponmeasured volatiles, undercure may lead to erroneously highvalues. Since variou
20、s pieces of cure equipment may varywidely in efficiency, it is essential that dialogue betweenmaterial manufacturer and testing laboratory establish a cureschedule appropriate both to the material to be tested and to thecure equipment to be used in the procedure.TEST METHOD A7. Scope7.1 This test me
21、thod is applicable to radiation curablematerials with solvent content less than or equal to 3 %.8. Apparatus8.1 Aluminum Substrate, standard test panels (102 mm by305 mm) or heavy gage (0.05 mm minimum) foil. Test panelsare most convenient and may be cut into smaller pieces for easeof weighing. Prec
22、ondition the substrate for 30 min at 110 65C and store in a desiccator prior to use.8.2 Forced Draft Oven, Type IIA or Type IIB as specified inSpecification E145.8.3 Ultraviolet Light or Electron Beam Curing EquipmentThere are several commercial suppliers of laboratory scaleequipment that simulates
23、industrial curing processes.39. Procedure9.1 Mix the sample, if necessary, to ensure uniformity. Handstirring is recommended to avoid the entrapment of air bubbles.9.2 Weigh the preconditioned aluminum substrate, (8.1)to0.1 mg (A). The size of the aluminum substrate must allow aminimum of 0.2 g of m
24、aterial to be applied at the suppliersrecommended film thickness. Use rubber gloves or tongs, orboth, to handle samples.9.3 Apply a minimum of 0.2 g of test specimen to thealuminum substrate and reweigh to 0.1 mg (B). Prepare a totalof three test specimens.NOTE 1The elapsed time between application
25、and weighing should beno greater than 30 s. If the sample to be tested contains any reactivediluent with a vapor pressure at room temperature greater than 1.0 mm Hg(for example, styrene), the elapsed time between specimen application andweighing must be no greater than 15 s.9.4 Cure the test specime
26、n by exposure to UV or EB asprescribed by the supplier of the material.NOTE 2If there is any doubt as to the adequacy of the exposure foraffecting proper cure (6.1), an additional sample can be tested utilizing50 % additional exposure and the volatile content results compared. If theoriginal exposur
27、e was adequate, there should be no difference in theresults within the precision of the test method. If the results are different,the supplier of the material must be contacted and a revised cure scheduleestablished.9.5 Allow the test specimen to cool 15 min at roomtemperature and reweigh to 0.1 mg
28、(C).9.6 Heat the test specimen in a forced draft oven (8.2) for 60min at 110 6 5C.NOTE 3Materials that can react with atmospheric moisture duringpost cure, that is, UV cationic-curable epoxy materials, may exhibit aweight gain during procedure in 9.6. If this occurs, the sample should beretested and
29、 allowed to post cure at room temperature for 48 h afterprocedure in 9.5, and then reweighed prior to procedure in 9.6. The weightafter post cure should then be used as Weight C in the calculation ofpercent potential volatiles in 10.1.9.7 Allow the test specimen to cool to room temperature ina desic
30、cator and reweigh to 0.1 mg, (D).10. Calculations10.1 Calculate the weight percent volatiles as follows:Processing Volatiles 5 100B 2 C!/B 2 A!# (1)Potential Volatiles 5 100C 2 D!/B 2 A!# (2)Total volatiles 5 % Processing Volatiles1% Potential Volatileswhere:A = weight of aluminum substrate, g,B = w
31、eight of aluminum substrate plus test specimen, g,C = weight of aluminum substrate plus test specimen aftercure, g, andD = weight of aluminum substrate plus cured test specimenafter heating.11. Precision and Bias11.1 Interlaboratory Test ProgramAn interlaboratorystudy4of volatile content of radiatio
32、n cured materials (TestMethod A) was conducted in accordance with Practice E691 innine laboratories with three materials, with each laboratoryobtaining three test results for each material.11.2 Test ResultThe precision information given belowfor volatile content in weight percent is for the comparis
33、on oftwo test results, each of which is the average of three testdeterminations.3A list of such suppliers may be obtained by contacting RadTech InternationalN.A., 60 Revere Drive, Suite 500, Northbrook, IL 60062.4Supporting data have been filed at ASTM International Headquarters and maybe obtained b
34、y requesting Research Report RR:D01-1083.D5403 93 (2013)211.3 Precision:PercentProcessing Volatiles95 % repeatability limit (within laboratory) 0.995 % reproducibility limit (between laboratories) 1.6Potential Volatiles95 % repeatability limit (within laboratory) 2.295 % reproducibility limit (betwe
35、en laboratories) 4.2Total Volatiles95 % repeatability limit (within laboratory) 2.395 % reproducibility limit (between laboratories) 3.9The terms repeatability limit and reproducibility limit areused as specified in Practice E177. The respective standarddeviations among test results may be obtained
36、by dividing thelimit values by 2.8. The form of this precision statement is inaccordance with Practice E177.11.4 BiasSince there is no accepted reference material ormethod, or laboratory suitable for determining the bias for theprocedure in this test method for measuring the volatile contentof radia
37、tion cured materials, no statement of bias is beingmade.TEST METHOD B12. Scope12.1 This test method is applicable to all radiation curablematerials that will cure properly at the designated specimenweight, which corresponds to a film thickness of 50 to 75 mdepending upon solvent content. Test Method
38、 B is the methodof choice for all radiation curable materials with solventcontent greater than 3 %.12.2 This test method is not applicable to materials contain-ing styrene due to its volatility at 50C.13. Apparatus13.1 Aluminum Foil Dish, 58 mm in diameter by 18 mm inheight with a smooth (planar) bo
39、ttom surface. Precondition thedishes for 30 min in an oven at 110 6 5C and store in adesiccator prior to use.13.2 Forced Draft Oven, Type IIA or Type IIB as specifiedin Specification E145.NOTE 4The shelves of the oven must be level.13.3 Syringe, 1 mL, capable of properly dispensing thematerial under
40、 test at sufficient rate that the specimen can bedissolved in the solvent. Disposable syringes are recom-mended.13.4 Ultraviolet Light or Electron Beam CuringEquipmentThere are several commercial suppliers of labo-ratory scale equipment that simulates industrial curing pro-cesses.314. Reagents14.1 P
41、urity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform the specifications of the Committeeon Analytical Reagents of the American Chemical Society,where such specifications are available.5Other grades may beused, p
42、rovided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.15. Procedure15.1 Mix the sample, if necessary, to ensure uniformity.Hand stirring is recommended to avoid the entrapment of airbubbles.15.2 Weigh a pre
43、conditioned aluminum dish (13.1) to 0.1mg (A). Use rubber gloves or tongs, or both, to handle sampledishes.15.3 Using the syringe (see 13.3) weigh to 0.1 mg (B), bydifference, 0.3 6 0.1 g of test specimen into the foil dish towhich has been added 3 6 1 mL of acetone. Add the materialdropwise, swirli
44、ng the dish to disperse it completely in theacetone. If the material forms a lump that cannot be dispersed,discard the test specimen and prepare a new one. Prepare atotal of three samples.NOTE 5Be sure to wipe the outer surface of the syringe clean afterobtaining the test specimen. Pull the syringe
45、plunger up14 of an inch topull the material away from the neck of the syringe. Cap and weigh thesyringe. After dispensing the test specimen, do not wipe the tip of thesyringe. Remove the material from the neck of the syringe by pulling upthe plunger. Cap and reweigh the syringe. Note that sample wei
46、ght (B)equals initial weight syringe minus final weight syringe.NOTE 6Use disposable rubber gloves or polyethylene to handle thesyringe.NOTE 7If the material is not compatible with acetone, tetrahydrofuran(THF) or a blend of acetone and THF may be substituted.15.4 Heat the samples in the forced draf
47、t oven (see 13.2) for30 min at 50 6 2C.NOTE 8This step is critical since a large amount of solvent present inthe sample during cure will interfere with the cure process and aninadequate degree of cure may result, which could produce erroneousvolatile results (see 6.1). If the material contains only
48、very fast solvents,a lower temperature/shorter time may be substituted if it can be demon-strated that the conditions are adequate to remove at least 90 % of theoriginal solvent in the composition. Any remaining solvent will beremoved during the subsequent cure and heating steps. In the case ofsampl
49、es that contain volatile solvents for control of application viscosity,this step also simulates the industrial processing stage necessary to removethe solvent prior to cure.15.5 Cure the test specimen by exposure to UV or EB asprescribed by the supplier of the material (see Note 2).15.6 Allow the test specimen to cool for 5 min at roomtemperature and reweigh (C).15.7 Heat the test specimen in the forced draft oven (see13.2) for 60 min at 110 6 5C. (WarningIn addition to otherprecautions, provide adequate ventilation, consistent with ac-cepted
