1、Designation: D7767 11 (Reapproved 2018)Standard 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 yea
2、r 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 test method describes a means to determine theperc
3、entage of processing, 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 apr
4、e-exposure water or 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 t
5、hisstandard.1.3 This 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.Thi
6、s standard doesnot purport to address all of the safety concerns, if any,associated with its use. It is the responsibility of the user of thisstandard to establish appropriate safety, health, and environ-mental practices and determine the applicability of regulatorylimitations prior to use.1.4 This
7、international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (T
8、BT) Committee.2. Referenced Documents2.1 ASTM Standards:2D5403 Test Methods for Volatile Content of Radiation Cur-able MaterialsE145 Specification for Gravity-Convection and Forced-Ventilation OvensE177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE691 Practice for Conducting
9、an Interlaboratory Study toDetermine 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 applica
10、tionstate to its final use state measured by tests generally related toend use performance and mutually agreeable to supplier andpurchaser.3.1.2 electron beam (EB) curing, nconversion of a coatingfrom its application state to its final use state by means of amechanism initiated by electron impingeme
11、nt generated byequipment designed for 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 cu
12、ring.1This 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 Materials.Current edition approved June 1, 2018. Published June 2018. Origi
13、nallyapproved in 2011. Last previous edition approved in 2011 as D7767 11. DOI:10.1520/D7767-11R18.2For 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 Doc
14、ument Summary page onthe ASTM website.3Available from U.S. Government Printing Office Superintendent of Documents,732 N. Capitol St., NW, 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.
15、 United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Bar
16、riers to Trade (TBT) Committee.13.1.5 processing volatiles, nthe 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
17、 oven, or both.3.1.7 thin, adjless than 15 micrometres in thickness.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, ncon
18、version of a coatingfrom its application state to its final use 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
19、range between 320 and390 nm.4. Summary of Test Method4.1 A designated quantity of an acrylate-functional material(test specimen) is 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. Thecalcula
20、ted percentage weight loss is attributed to processvolatiles. The test specimen and container lid are weighedagain after heating for 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
21、 difference between the initial sample mass and the retainedmass after exposing and heating divided by the initial mass.5. Significance 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 prescribe
22、d by the supplierof the material, most radiation curable monomers and oligom-ers provided as raw materials to formulators are not 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
23、 for themeasurement of volatiles from thin radiation-curable coatingsbecause supplier prescribed cure conditions include both athickness and an exposure specification which are difficult orimpossible to achieve in a test lab. Furthermore, inks form aspecial class of thin radiation curable coatings b
24、ecause they areformulated with known interferences (for example, pigments).As a result, Test Method D5403 does not provide a method formeasuring volatiles from monomers and oligomers used as rawmaterials in the formulation of radiation curable coatings nordoes it provide a method for measuring volat
25、iles from thinradiation curable coatings such as inks.5.2 This test method provides a means to measure thevolatile content of individual acrylate monomers, oligomers,and blends commonly used to formulate radiation curablecoatings such as printing inks. Such coatings comprise liquidor solid reactants
26、 that cure by polymerizing, crosslinking, or acombination of both and are designed to be applied as thincoatings in the absence of 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
27、or thin coatings made from them.5.3 This test method also provides a means to measure thevolatiles from acrylate monomers, oligomers, and blends curedusing ultraviolet radiation from which an estimate for thevolatiles from a thin coating cured using ultraviolet radiationcomprising these acrylate mon
28、omers, oligomers, and blendscan be calculated. A common exposure step involving aspecified amount of ultraviolet radiation in a specific spectralrange using a common photoinitiator is called for.5.4 This test method further provides a means to measurethe volatiles from thin radiation-curable coating
29、s such as inksin the absence of known interferences such as pigments. Acommon exposure step involving a specified amount of ultra-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: pro
30、cessing volatiles and potential vola-tiles. Processing volatiles are a measure of volatile loss duringthe actual cure process. Potential (or residual) volatiles are ameasure of volatile loss that might occur upon aging or underextreme storage conditions. These volatile content measure-ments may be u
31、seful to the producer of a material, a formulatorusing such materials, or to environmental interests for deter-mining and reporting 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 ult
32、raviolet radiation hasnot been verified. Use of an electron beam to cure the acrylatemonomers, oligomers, and blends or thin coatings 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 procedureaccur
33、ately measure the volatiles emitted is absolutely depen-dent upon proper cure during the test procedure. Althoughovercure will have little or no effect upon measured volatiles,undercure may lead to erroneously high values. To minimizevariability in the cure conditions, an ultraviolet source provid-i
34、ng a given irradiance in a specific spectral region and anexposure energy is specified as is a photoinitiator and concen-tration.6.2 The presence of strong ultraviolet absorbing non-acrylate species such as pigments and ultraviolet blockers caninterfere with the ability of this test procedure to acc
35、uratelymeasure volatiles. These additives are designed to absorb,reflect, luminesce, or scatter visible or ultraviolet radiation.Such additives interfere with the proper cure of materials testedusing this method and are to be avoided.6.3 Photoinitiators are strong ultraviolet absorbers but theirpres
36、ence is required for proper curing.D7767 11 (2018)27. Apparatus7.1 Container Lids, metal can lids having an OD of 35 mmand a height of 14 mm with 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 inSpecific
37、ation E145.7.3 Ring Stand, a device designed to support items usingvarious clamps.7.4 Versatile Clamp, a 3-pronged clamp with adjustableclosure for 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
38、device able to measure irradiance andenergy in the UVA spectral region.67.7 Balance, an instrument capable of weighing a mass tothe nearest 0.1 mg.7.8 Gloves, personal protective wear for handling chemi-cals.7.9 Forceps or Tongs, a means to handle a specimen withoutdirect contact in order to minimiz
39、e mass transfer.7.10 Spreading Tool, a small metal or PTFE spatula or awooden applicator stick for spreading resin.8. Preparation of Apparatus8.1 The tip of the quartz fiber guide shall be positionednormal to the center of a container lid (7.1) at a height ofapproximately 80 to 85 mm from the contai
40、ner lid to providean illuminated circular area of approximately 40 to 45 mm indiameter in the plane on which the container lid (7.1) sets inorder to approximate uniform irradiance of the test specimen.8.2 Identify the approximate center of the illuminated areawith a mark which will later assist in p
41、ositioning of a containerlid with a test specimen. A 25 mm filter paper disk taped to thework area surface works well for this. A proper setup is shownin Fig. 1.NOTE 1Placement of a mark is best accomplished with the shutteropen. Wear appropriate eye protection before opening the shutter andplacing
42、the mark.8.3 Center the optical window of the radiometer on the mark(8.2). Using the ultraviolet radiation source (7.5) set at 100 %power with the fiber (8.1) and radiometer optical window (7.6)properly aligned, open the shutter and measure the UVA peakirradiance at the sample plane. If necessary, a
43、djust the fiberheight to achieve a UVApeak irradiance of 115 6 15 mW/cm2.Once positioned, the fiber should not be moved relative to themark (8.2).8.4 Position the radiometer window (7.6) on the mark (8.2)and measure the UVA energy after an 80 s exposure. Ifnecessary, adjust the exposure time to achi
44、eve a UVA targetenergy of 9.0 6 0.2 joules/cm2. This determination should berepeated daily to verify proper exposure conditions.9. Procedure9.1 Dissolve 2.0 % by weight of ethyl-2,4,6-trimethylbenzoyphenylphosphinate (TPO-L) photoinitiator inthe material to be tested. Mix thoroughly to ensure homoge
45、-neity. Store the test specimen in a dark container.9.2 Precondition the container lids for 30 min at 110 6 5Cand store in a desiccator prior to use.9.3 Weigh a preconditioned container lid (7.1) to 0.1 mg(A). Use gloves, forceps, or tongs to handle the container lid.9.4 Place the container lid upsi
46、de down on the balance panand add 0.2 6 0.02 g of the test specimen (9.1) to the recessedarea. Spread the test specimen using a spreading tool to ensureuniform coverage of the recessed area. Do not allow the testspecimen to contact any surface of the container lid outside ofthe recessed area. Weigh
47、the container lid with test specimen to0.1 mg (B).NOTE 2It is helpful to hold the container lid with one hand using4Metal can lids for this method can be obtained from SKS Bottle the details are given inASTM Research Report RR:D01-1159.11.1.1 Repeatability Limit (r)Two test results obtainedwithin on
48、e 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 same material, obtained by the same operatorusing the same equipment on the same day in the samelaboratory.11.
49、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; “R” is the interval representing the critical7Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D01-1159. ContactASTM CustomerService at serviceastm.org.TABLE 2 Determination of Volatiles from Blends and Fully Formulated Coatings using Method BComponents inComposition (I)Weight Percentageof each Componentin Ful
