1、Designation: D 5403 93 (Reapproved 2007)Standard Test Methods forVolatile Content of Radiation Curable Materials1This standard is issued under the fixed designation D 5403; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year o
2、f 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 These test methods cover procedures for the determina-tion of weight percent volatile content of coatings, inks, an
3、dadhesives 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 i
4、nclusion 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 m
5、ethods 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 thisstand
6、ard.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
7、 hazardstatement is given in 15.7.2. Referenced Documents2.1 ASTM Standards:2D 2369 Test Method for Volatile Content of CoatingsE 145 Specification for Gravity-Convection and Forced-Ventilation OvensE 177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE 691 Practice for Conducti
8、ng an Interlaboratory 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 ul
9、traviolet (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 coat-ing from its application state to its fina
10、l use state by means ofa mechanism initiated by electron beam radiation generated byequipment designed for that purpose.3.1.4 processing volatiles, nloss in specimen weight un-der test conditions that are designed to simulate actual indus-trial cure processing conditions.3.1.5 potential volatiles, n
11、loss in specimen 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
12、the processing 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 calcu
13、lated from the losses inweight.5. Significance and Use5.1 These test methods are the procedures of choice fordetermining volatile content of materials designed to be curedby exposure to ultraviolet light or electron beam irradiation.These types of materials contain liquid reactants that react tobeco
14、me part of the film during cure, but, which under the test1These test methods are under the jurisdiction of ASTM Committee D01 onPaint and Related Coatings, Materials, and Applications and are the directresponsibility of Subcommittee D01.55 on Factory Applied Coatings on PreformedProducts.Current ed
15、ition approved June 1, 2007. Published July 2007. Originally approvedin 1993. Last previous edition approved in 2002 as D 5403 - 93 (2002).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume
16、 information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.conditions of Test Method D 2369, will be erroneously mea-sured as volatiles. The conditions of these test
17、methods aresimilar to Test Method D 2369 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 cure
18、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 degree to
19、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 various piec
20、es 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 method i
21、s 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. Preconditi
22、on 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 E 145.8.3 Ultraviolet Light or Electron Beam CuringEquipmentThere are several commercial suppliers of labo-ratory scale equipment that simulates indu
23、strial curing pro-cesses.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 mate
24、rial 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 and
25、 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 specimen b
26、y 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 exposure w
27、as 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 (C)
28、.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 al
29、lowed 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 desiccat
30、or and reweigh to 0.1 mg, (D).10. Calculations10.1 Calculate the weight percent volatiles as follows:Processing Volatiles 5 100 B 2 C!/B 2 A!# (1)Potential Volatiles 5 100 C 2 D!/B 2 A!# (2)Total volatiles 5 % Processing Volatiles 1 % Potential Volatileswhere:A = weight of aluminum substrate, g,B =
31、weight 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 speci-men after heating.11. Precision and Bias11.1 Interlaboratory Test ProgramAn interlaboratorystudy4of volatile content of radia
32、tion cured materials (TestMethodA) was conducted in accordance with Practice E 691 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 compa
33、rison 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 60062.4Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Societ
34、y, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.D
35、5403 93 (2007)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 (between laboratories) 4.2Total Volatiles95 % re
36、peatability limit (within laboratory) 2.395 % reproducibility limit (between laboratories) 3.9The terms repeatability limit and reproducibility limit areused as specified in Practice E 177. The respective standarddeviations among test results may be obtained by dividing thelimit values by 2.8. The f
37、orm of this precision statement is inaccordance with Practice E 177.11.4 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 radiation cured materials, no statement of bi
38、as 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 B is the methodof choice for all radiat
39、ion 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) bottom surface. Precondition thedishes for
40、 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 E 145.NOTE 4The shelves of the oven must be level.13.3 Syringe, 1 mL, capable of properly dispensing thematerial under test at sufficient rate that the speci
41、men 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.414. Reagents14.1 Purity of ReagentsReagent grade chemical
42、s 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, provided it is first ascertained that th
43、e 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 preconditioned aluminum dish (13.1) to 0.1
44、mg (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, swirling the dish to disperse it completely i
45、n 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 plunger up14 of an inch topull the mate
46、rial 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 weight (B)equals initial weight syringe mi
47、nus 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 draft oven (see 13.2) for30 min at 50 6 2C.
48、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 very fast solvents,a lower temperature/
49、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 ofsamples 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
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