1、Designation: D1304 99 (Reapproved 2012)Standard Test Methods forAdhesives Relative to Their Use as Electrical Insulation1This standard is issued under the fixed designation D1304; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the
2、 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 These test methods cover procedures for testing adhe-sives in liquid, highly viscous, solid, or set states, t
3、hat areintended to be cured by electronic heating, or that are intendedto provide electrical insulation, or that are intended for use inelectrical apparatus.1.2 The procedures appear in the following order:(1) Procedure for Testing Adhesives Before Use:SectionPower Factor and Dielectric Constant of
4、Liquid Adhesives 7Direct-Current Conductivity 8Extract Conductivity 9Acidity and Alkalinity 10pH Value 11(2) Procedures for Testing Properties of Adhesives As Used:SectionPower Factor and Dielectric Constant of a Dried or Cured AdhesiveFilm 12Dielectric Strength 13Volume and Surface Resistivity 14Ar
5、c Resistance 151.3 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.
6、 For a specifichazard statement, see 8.2.2. Referenced Documents2.1 ASTM Standards:2D115 Test Methods for Testing Solvent Containing Var-nishes Used for Electrical InsulationD150 Test Methods for AC Loss Characteristics and Permit-tivity (Dielectric Constant) of Solid Electrical InsulationD202 Test
7、Methods for Sampling and Testing UntreatedPaper Used for Electrical InsulationD257 Test Methods for DC Resistance or Conductance ofInsulating MaterialsD495 Test Method for High-Voltage, Low-Current, Dry ArcResistance of Solid Electrical InsulationD897 Test Method for Tensile Properties of Adhesive B
8、ondsD907 Terminology of Adhesives3. Terminology3.1 DefinitionsMany terms in these test methods aredefined in Terminology D907.4. Significance and Use4.1 Insulating materials are used to isolate components of anelectrical system from each other and from ground, as well asto provide mechanical support
9、 for the components. For thispurpose, it is generally desirable to have the insulation resis-tance as high as possible, consistent with acceptablemechanical, chemical, and heat-resisting properties. Sinceinsulation resistance or conductance combines both volumeand surface resistance or conductance,
10、its measured value ismost useful when the test specimen and electrodes have thesame form as is required in actual use. Surface resistance orconductance changes rapidly with humidity, while volumeresistance or conductance changes slowly although the finalchange may eventually be greater.4.2 Resistivi
11、ty or conductivity is used to predict, indirectly,the low-frequency dielectric breakdown and dissipation factorproperties of some materials. Resistivity or conductivity isoften used as an indirect measure of moisture content, degreeof cure, mechanical continuity, and deterioration of varioustypes. T
12、he usefulness of these indirect measurements is depen-dent on the degree of correlation established by supportingtheoretical or experimental investigations. A decrease of sur-face resistance will result either in an increase of the dielectricbreakdown voltage because the electric field intensity isr
13、educed, or a decrease of the dielectric breakdown voltagebecause the area under stress is increased.4.3 All the dielectric resistances or conductances depend onthe length of time of electrification and on the value of appliedvoltage (in addition to the usual environmental variables).These must be kn
14、own to make the measured value of resistanceor conductance meaningful.1These test methods are under the jurisdiction ofASTM Committee D14 and arethe direct responsibility of Subcommittee D14.80 on Metal Bonding AdhesivesCurrent edition approved Oct. 1, 2012. Published October 2012. Originallyapprove
15、d in 1954. Last previous edition approved in 2005 as D1304 99 (2005).DOI: 10.1520/D1304-99R12.2For 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
16、 Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States14.4 Volume resistivity or conductivity is used as an aid indesigning an insulator for a specific application. The change ofresistivity or conductivity wi
17、th temperature and humidity maybe great, and must be known when designing for operatingconditions. Volume resistivity or conductivity determinationsare often used in checking the uniformity of an insulatingmaterial, either with regard to processing or to detect conduc-tive impurities that affect the
18、 quality of the material and thatmay not be readily detectable by other methods.4.5 Volume resistivities above 1021Vcm (1019Vm),obtained on specimens under usual laboratory conditions, areof doubtful validity, considering the limitations of commonlyused measuring equipment.4.6 Surface resistance or
19、conductance cannot be measuredaccurately, only approximated, because some degree of volumeresistance or conductance is always involved in the measure-ment. The measured value is also affected by the surfacecontamination. Surface contamination, and its rate ofaccumulation, is affected by many factors
20、 including electro-static charging and interfacial tension. These, in turn, mayaffect the surface resistivity. Surface resistivity or conductivitycan be considered to be related to material properties whencontamination is involved but is not a material property in theusual sense.5. General Considera
21、tions5.1 Definitions, theory, and measuring equipment pertainingto this method shall be in accordance with test methods alreadyestablished for the property under consideration.6. Test Specimens6.1 For tests that are to be performed upon the adhesiveitself, the specimens shall consist of an adequate
22、representativesample which, until required, shall be kept at room temperaturein a nearly filled, tightly sealed container to avoid contamina-tion or escape of solvents.6.2 For tests that are to be performed upon the adhesive asa film, the test specimens shall be prepared in accordance withTest Metho
23、ds D115, with exceptions as noted.7. Power Factor and Dielectric Constant of LiquidAdhesives7.1 ProcedureTest the adhesive and report in accordancewith the procedure specified for liquids in Test Methods D150.8. Direct-Current Conductivity8.1 ProcedureDetermine volume resistivity and report inaccord
24、ance with Test Methods D257, except as follows: Makevolume resistivity measurements with an electrification time of1 min, a maximum potential gradient of 15 V/mil, and with thematerial at a temperature of 73.4 6 2F. Determine the volumeresistivity of a weighed amount of suitable reagent gradesolvent
25、 as selected or agreed upon by the manufacturer anduser or as specified in the specification or purchase order. Thisresistivity, r0, shall be no less than 2.0 1013Vcm. Withoutremoving the solvent from the container, add sufficient adhe-sive to result in a 2.0 6 0.1 weight percent total solids conten
26、tsolution. Weigh adhesives in solid sheet or film form directly.For adhesives in a liquid state determine the total solids contentby the following method before adding to the above solvent.8.2 Pour approximately 10 g of the sample into a low-formweighing bottle, cover, and weigh. After removing the
27、coverapply heat at 70C until the sample reaches constant weight(see Warning). Then cool the sample in a desiccator and weigh.(WarningCare should be exercised when volatile materialsare of such a nature as to constitute toxic, fire, or explosivehazard.)8.3 CalculationsCalculate the percentage of tota
28、l solids asfollows:Total solids, percent 5 wt of residue/wt of sample 3100 (1)8.4 Stir the dried adhesive into the solvent with a clean glassrod until all the adhesive is dissolved. Return the cell to thesolution and raise and lower it in the solution several times.Determine volume resistivity of th
29、e solution r1and calculateconductivity, s , as follows:s micromho cm! 5 1/r02 1/r1(2)9. Extract Conductivity9.1 ProcedureDetermine the extract conductivity of anadhesive and report in accordance with the procedure specifiedfor Aqueous Extract Conductivity in Test Methods D202,except use a 5-g sample
30、 of adhesive in a solid state, orsufficient sample to be equivalent to5gofsolids based ondetermining percentage total solids in accordance with 4.2. Foradhesives soluble in a solvent (not water) add a suitable reagentgrade solvent as selected or agreed upon by the manufacturerand user, or as specifi
31、ed in the specification or purchase order,until the total volume is 100 ml. Stir and warm gently until thesample is completely dissolved or diluted. To the solution addslowly with constant stirring 100 ml of boiling distilled water.Gently warm with constant stirring on an electric hot plate untilthe
32、 solvent has been distilled off, which can be detected by theabsence of its characteristic odor, and the solution has beenreduced to 100 ml or less. For adhesives soluble in water, addboiling distilled water until the total volume is 100 ml. Stir andwarm gently until the sample is completely dissolv
33、ed ordiluted.9.2 After filtering, wash the residue with 100 ml of hotdistilled water. Adjust the final volume to 250 ml with hotdistilled water. The conductivity, based on a sample-to-waterratio of1gto100ml,isequal to:0.5 K/R22 K/R33106micromhos/cm (3)where:K = cell constant (C R),R2= resistance in
34、ohms of extract solution at 25 6 0.5C,andR3= resistance in ohms of water blank at 25 6 0.5C.10. Acidity and Alkalinity10.1 ProcedureDetermine the acidity or alkalinity of anadhesive and report in accordance with Test Methods D202,except that the extraction procedure shall be as prescribed inSection
35、6 of these methods.D1304 99 (2012)211. pH Value11.1 ProcedureDetermine the pH value of an adhesiveand report in accordance with Test Methods D202, except thatthe extraction procedure shall be as prescribed in Section 9 ofthese test methods.12. Power Factor and Dielectric Constant of a Dried orCured
36、Adhesive Film12.1 Test SpecimensPrepare test specimens in accordancewith the procedure specified for determining the dielectricstrength of dried varnish film in Test Methods D115. If cure isrequired, the time and temperature shall be in accordance withrecommendations of the manufacturer of the adhes
37、ive.12.2 ProcedureDetermine the power factor and dielectricconstant and report in accordance with the procedure specifiedfor films in Test Methods D150.13. Dielectric Strength of a Dried or Cured AdhesiveFilm13.1 Test SpecimensPrepare test specimens in accordancewith 12.1.13.2 ProcedureDetermine die
38、lectric strength and report inaccordance with the procedure specified for determining thedielectric strength of dried varnish film in Test Methods D115.14. Volume and Surface Resistivity14.1 Test SpecimensTest specimens for use in determiningthe volume and surface resistivity of solid adhesives shal
39、lconsist of two metal disks, one18 by 2 in. (3 by 51 mm) indiameter, the other18 by 1.5 in. (3 by 38 mm) diameter, and ametal ring18 by 2 in. in outside diameter by 1.75 in. (3 by 51by 44 mm) in inside diameter, bonded together by the sampleadhesive as shown in Fig. 1. The specimen shall be bonded b
40、ythe application of heat and pressure, if necessary, by means ofparallel platens in a suitable press. Preparation of areas to becemented, and gluing, shall be in accordance with the recom-mendations of the manufacturer of the adhesive and with TestMethod D897. Thickness of the glue line shall be not
41、 greaterthan 0.060 in. (1.52 mm) nor less than 0.0020 in. (0.051 mm).14.2 ProcedureDetermine the volume and surface resis-tivity of solid adhesives and report in accordance with TestMethods D257. The voltage applied shall not exceed 30 V/mil.Read at the end of 1 min electrification.15. Arc Resistanc
42、e15.1 Test SpecimensPrepare test specimens for use indetermining the arc resistance of adhesives in accordance withSection 12, except usea4by4in.sheet of XXX grade flatphenolic laminate for the base material, and the thickness ofthe adhesive film shall be between 0.002 (0.05 mm) and 0.005in (0.13 mm
43、).15.2 ProcedureDetermine the arc resistance of solid ad-hesives and report in accordance with Test Method D495.16. Report16.1 Report the following information:16.1.1 Complete identification of the adherend and adhesivematerials tested, including adhesive type, source, and manu-facturers code number
44、.16.1.2 Curing conditions used.16.1.3 Conditioning environment and test environment.16.1.4 Number of specimens tested per sample.16.1.5 Dimensions of each test specimen including glue linethickness.16.1.6 Corrected resistances of each test specimen.16.1.7 Volume resistivity, in ohm-centimeters, of e
45、ach testspecimen.16.1.8 Average volume resistivity of the sample, when morethan one test specimen per sample is used.16.1.9 Standard deviation of the volume resistivity mea-surements when more than one test specimen per sample isused.16.1.10 Power factor as in Test Methods D150.16.1.11 Direct-curren
46、t conductivity as in Test MethodsD257.16.1.12 Extract conductivity as in Test Methods D202.16.1.13 Acidity and alkalinity as in Test Methods D202.16.1.14 pH value as in Test Methods D202.16.1.15 Volume and surface resistivity as in Test MethodsD257.16.1.16 Arc resistance as in Test Method D495.17. P
47、recision and Bias17.1 PrecisionPrecision and Bias for this test method isbeing determined and will be available by September 2004.17.2 BiasA statement of bias cannot be made because ofthe lack of a standard reference material.17.3 The precision and bias of this test method are afunction of the adhes
48、ive system, surface preparation,substrates, test temperature, cyclic stress level, and otherfactors related to the test apparatus, laboratory, and operatorvariabilities. Precision shall be reported in terms of thestandard deviation of the data and the standard error of themean.18. Keywords18.1 adhes
49、ives; arc resistivity; d-c conductivity; dielectricstrength; electrical insulation; power factor; surface resistivity;volume resistivityMetric Equivalentsin.18 112 2mm 3 38 51FIG. 1 Test Specimen for Use in Determining Volume and Sur-face Resistivity.D1304 99 (2012)3ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of
