1、Designation: D7767 11Standard Test Method toMeasure Volatiles from Radiation Curable AcrylateMonomers, Oligomers, and Blends and Thin Coatings Madefrom Them1This standard is issued under the fixed designation D7767; the number immediately following the designation indicates the year oforiginal adopt
2、ion 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 test method describes a means to determine thepercentage of processi
3、ng, potential, and total volatiles fromradiation curable acrylate monomers, oligomers, and blends.The results can be used to estimate the volatiles from thinradiation curable coatings that cannot otherwise be measuredwith the restriction that those coatings are not subjected to apre-exposure water o
4、r solvent drying step. It also provides ameans to determine the volatiles of thin radiation curablecoatings in the absence of known interferences such aspigments in inks.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 Th
5、is standard does not purport to address all of thesafety concerns, 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.2. Referenced Documen
6、ts2.1 ASTM Standards:2D5403 Test Methods for Volatile Content of RadiationCurable MaterialsE145 Specification for Gravity-Convection and Forced-Ventilation OvensE177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE691 Practice for Conducting an Interlaboratory Study toDetermine
7、the Precision of a Test Method2.2 Other Document:3EPA Method 24 Determination of Volatile Matter Content,Water Content, Density, Volume Solids, and Weight Solidsof Surface Coatings3. Terminology3.1 Definitions:3.1.1 cure, nconversion of a coating from its applicationstate to its final use state meas
8、ured by tests generally related toend use performance and mutually agreeable to supplier andpurchaser.3.1.2 electron beam (EB) curing, nconversion of a coat-ing from its application state to its final use state by means ofa mechanism initiated by electron impingement generated byequipment designed f
9、or that purpose.3.1.3 pigment, nan insoluble substance added to a formu-lation to modify the visual appearance of a coating made fromthe formulation.3.1.4 potential volatiles, nthe percentage loss in specimenweight upon heating at 110C for 60 min after radiation curing.3.1.5 processing volatiles, nt
10、he percentage loss in speci-men weight under process conditions that are designed tosimulate actual industrial cure processing conditions.3.1.6 retained weight, nthe mass of specimen remainingafter exposing to the UV source, heating in an oven, or both.3.1.7 thin, adjless than 15 micrometres in thic
11、kness.3.1.8 total volatiles, nthe percentage loss in specimenweight under process conditions that are designed to simulateactual industrial cure processing conditions and after heating at110C for 60 min.3.1.9 ultraviolet (UV) curing, nconversion of a coatingfrom its application state to its final us
12、e state by means of amechanism initiated by ultraviolet radiation in the range from200 to 400 nm generated by equipment designed for thatpurpose.3.1.10 UVA, nthe region of the electromagnetic spectrumcomprising wavelengths falling in the range between 320 and390 nm.1This test method is under the jur
13、isdiction 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 Materials.Current edition approved Nov. 1, 2011. Published November 2011. DOI:10.1520/D7767-11.2For referenced AST
14、M 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.3Available from U.S. Government Printing Office Superintendent of Documents,732
15、N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http:/www.access.gpo.gov.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.4. Summary of Test Method4.1 A designated quantity of an acrylate-functional material(test specimen) i
16、s weighed in a container lid before and after aUV exposure step sufficient to ensure a thorough cure of thetest specimen to obtain the percent solids retained. Thecalculated percentage weight loss is attributed to processvolatiles. The test specimen and container lid are weighedagain after heating f
17、or 60 min at 110 6 5C to obtain thepercent solids retained. Any additional weight loss is attributedto potential volatiles. The total volatiles for a test specimen arethe difference between the initial sample mass and the retainedmass after exposing and heating divided by the initial mass.5. Signifi
18、cance and Use5.1 This test method is an extension of Test Method D5403.While Test Method D5403 specifies that a test specimen becured by exposure to UV or EB as prescribed by the supplierof the material, most radiation curable monomers and oligom-ers provided as raw materials to formulators are not
19、designedto be used alone but rather as blends of monomers andoligomers so that there are no “supplier prescribed” exposureconditions. Test Method D5403 is not appropriate for themeasurement of volatiles from thin radiation-curable coatingsbecause supplier prescribed cure conditions include both athi
20、ckness and an exposure specification which are difficult orimpossible to achieve in a test lab. Furthermore, inks form aspecial class of thin radiation curable coatings because they areformulated with known interferences (for example, pigments).As a result, Test Method D5403 does not provide a metho
21、d formeasuring volatiles from monomers and oligomers used as rawmaterials in the formulation of radiation curable coatings nordoes it provide a method for measuring volatiles from thinradiation curable coatings such as inks.5.2 This test method provides a means to measure thevolatile content of indi
22、vidual acrylate monomers, oligomers,and blends commonly used to formulate radiation curablecoatings such as printing inks. Such coatings comprise liquidor solid reactants that cure by polymerizing, crosslinking, or acombination of both and are designed to be applied as thincoatings in the absence of
23、 water or solvent and to be cured byexposing to ultraviolet radiation. There is currently no directmethod for measuring the volatiles from the individual mate-rials used or thin coatings made from them.5.3 This test method also provides a means to measure thevolatiles from acrylate monomers, oligome
24、rs, and blends curedusing ultraviolet radiation from which an estimate for thevolatiles from a thin coating cured using ultraviolet radiationcomprising these acrylate monomers, oligomers, and blendscan be calculated. A common exposure step involving aspecified amount of ultraviolet radiation in a sp
25、ecific spectralrange using a common photoinitiator is called for.5.4 This test method further provides a means to measurethe volatiles from thin radiation-curable coatings such as inksin the absence of known interferences such as pigments. Acommon exposure step involving a specified amount of ultra-
26、violet radiation in a specific spectral range using a commonphotoinitiator is called for.5.5 If desired, volatile content can be determined as twoseparate components: processing volatiles and potential vola-tiles. Processing volatiles are a measure of volatile loss duringthe actual cure process. Pot
27、ential (or residual) volatiles are ameasure of volatile loss that might occur upon aging or underextreme storage conditions. These volatile content measure-ments may be useful to the producer of a material, a formulatorusing such materials, or to environmental interests for deter-mining and reportin
28、g emissions.5.6 The validity of this test method for non-acrylatedradiation-curable chemistries such as methacrylates, thiol-ene,vinyl ethers, and epoxies cured using ultraviolet radiation hasnot been verified. Use of an electron beam to cure the acrylatemonomers, oligomers, and blends or thin coati
29、ngs made fromthem, including inks, has not been verified using this methodand cannot be assumed.6. Interferences6.1 The degree to which the results of this procedureaccurately measure the volatiles emitted is absolutely depen-dent upon proper cure during the test procedure. Althoughovercure will hav
30、e little or no effect upon measured volatiles,undercure may lead to erroneously high values. To minimizevariability in the cure conditions, an ultraviolet source provid-ing a given irradiance in a specific spectral region and anexposure energy is specified as is a photoinitiator and concen-tration.6
31、.2 The presence of strong ultraviolet absorbing non-acrylate species such as pigments and ultraviolet blockers caninterfere with the ability of this test procedure to accuratelymeasure volatiles. These additives are designed to absorb,reflect, luminesce, or scatter visible or ultraviolet radiation.S
32、uch additives interfere with the proper cure of materials testedusing this method and are to be avoided.6.3 Photoinitiators are strong ultraviolet absorbers but theirpresence is required for proper curing.7. Apparatus7.1 Container Lids, metal can lids having an OD of 35 mmand a height of 14 mm with
33、a 25 mm diameter protrusionwhich, when inverted, creates a 0.6 mm deep, 25 mm diameterwell.47.2 Forced Draft Oven, Type IIA or IIB as specified inSpecification E145.7.3 Ring Stand, a device designed to support items usingvarious clamps.7.4 Versatile Clamp, a 3-pronged clamp with adjustableclosure fo
34、r holding items.7.5 Ultraviolet Radiation Source, the focused output from ashort-arc 200W Xe/Hg bulb delivered by a quartz fiber guide.57.6 Radiometer, a device able to measure irradiance andenergy in the UVA spectral region.64Metal can lids for this method can be obtained from SKS Bottle the detail
35、s are given inASTM Research Report No. D011159.11.1.1 Repeatability Limit (r)Two test results obtainedwithin one laboratory shall be judged not equivalent if theydiffer by more than the “r” value for that material; “r”istheinterval representing the critical difference between two testresults for the
36、 same material, obtained by the same operatorusing the same equipment on the same day in the samelaboratory.11.1.1.1 Repeatability limits are listed in Table 3.11.1.2 Reproducibility Limit (R)Two test results shall bejudged not equivalent if they differ by more than the “R” valuefor that material; “
37、R” is the interval representing the criticaldifference between two test results for the same material,obtained by different operators using different equipment indifferent laboratories.11.1.2.1 Reproducibility limits are listed in Table 3.11.1.3 The above terms (repeatability limit and reproduc-ibil
38、ity limit) are used as specified in Practice E177.11.1.4 Any judgment in accordance with statements 11.1.1and 11.1.2 would have an approximate 95 % probability ofbeing correct.11.2 BiasAt the time of the study, there was no acceptedreference material suitable for determining the bias for this testme
39、thod, therefore no statement on bias is being made.11.3 The precision statement was determined through sta-tistical examination of 189 test results, reported by ninelaboratories, on three types of materials.12. Keywords12.1 acrylic monomers; acrylics; blends; electron beamcuring; inks; oligomers; ph
40、otoinitiator; pigmented coatings;radiation curable material; radiation curing; ultraviolet curing;volatile content7Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D01-1159.D7767 115ASTM International takes no position respecting
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