1、Designation: D 1304 99 (Reapproved 2005)Standard Test Methods forAdhesives Relative to Their Use as Electrical Insulation1This standard is issued under the fixed designation D 1304; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, t
2、he year of 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 testing adhe-sives in liquid, highly viscous, solid, or set states
3、, that 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
4、of 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 1
5、4Arc 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 u
6、se. 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 InsulationD 150 Test Methods for AC Loss Characteristics and Per-mittivity (Dielectric Constant) of Solid Electrical Insula-tionD 202
7、 Test Methods for Sampling and Testing UntreatedPaper Used for Electrical InsulationD 257 Test Methods for DC Resistance or Conductance ofInsulating MaterialsD 495 Test Method for High-Voltage, Low-Current, DryArc Resistance of Solid Electrical InsulationD 897 Test Method for Tensile Properties of A
8、dhesiveBondsD 907 Terminology of Adhesives3. Terminology3.1 DefinitionsMany terms in these test methods aredefined in Terminology D 907.4. Significance and Use4.1 Insulating materials are used to isolate components of anelectrical system from each other and from ground, as well asto provide mechanic
9、al support for the components. For thispurpose, it is generally desirable to have the insulation resis-tance as high as possible, consistent with acceptable mechani-cal, chemical, and heat-resisting properties. Since insulationresistance or conductance combines both volume and surfaceresistance or c
10、onductance, its measured value is most usefulwhen the test specimen and electrodes have the same form asis required in actual use. Surface resistance or conductancechanges rapidly with humidity, while volume resistance orconductance changes slowly although the final change mayeventually be greater.4
11、.2 Resistivity 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 var
12、ioustypes. The 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 i
13、ntensity isreduced, 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).1The
14、se test methods are under the jurisdiction of ASTM CommitteeD14 and arethe direct responsibility of Subcommittee D14.80 on Metal Bonding AdhesivesCurrent edition approved April 1, 2005. Published April 2005. Originallyapproved in 1954. Last previous edition approved in 1999 as D 1304 99.2For referen
15、ced 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 Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West C
16、onshohocken, PA 19428-2959, United States.These must be known to make the measured value of resistanceor conductance meaningful.4.4 Volume resistivity or conductivity is used as an aid indesigning an insulator for a specific application. The change ofresistivity or conductivity with temperature and
17、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 quality of the mat
18、erial and thatmay not be readily detectable by other methods.4.5 Volume resistivities above 1021Vcm (1019Vm), ob-tained on specimens under usual laboratory conditions, are ofdoubtful validity, considering the limitations of commonlyused measuring equipment.4.6 Surface resistance or conductance canno
19、t 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 of accumu-lation, is affected by many factors including elec
20、trostaticcharging and interfacial tension. These, in turn, may affect thesurface resistivity. Surface resistivity or conductivity can beconsidered to be related to material properties when contami-nation is involved but is not a material property in the usualsense.5. General Considerations5.1 Defini
21、tions, 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 representatives
22、ample 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 Methods D115, with e
23、xceptions 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 D 150.8. Direct-Current Conductivity8.1 ProcedureDetermine volume resistivity and report inaccordance with Test
24、 Methods D 257, 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 as selected
25、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 3 1013Vcm. Withoutremoving the solvent from the container, add sufficient adhe-sive to result in a 2.0 6 0.1 weight percent total solids contentsolution.
26、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 coverapply
27、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 Calculations Calculate the percentage of total solidsas
28、 follows:Total solids, percent 5 wt of residue/wt of sample 3 100 (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 the solutio
29、n 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 D 202,except use a 5-g sample of adhe
30、sive 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 specified in th
31、e 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 solvent
32、 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 dissolved ordil
33、uted.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/R33 106micromhos/cm (3)where:K = cell constant (C 3 R),R2= resistance in ohms
34、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 D 202,except that the extraction procedure shall be as prescribed inSection 6 of
35、 these methods.D 1304 99 (2005)211. pH Value11.1 ProcedureDetermine the pH value of an adhesiveand report in accordance with Test Methods D 202, except thatthe extraction procedure shall be as prescribed in Section 9 ofthese test methods.12. Power Factor and Dielectric Constant of a Dried orCured Ad
36、hesive Film12.1 Test Specimens Prepare 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 adhesi
37、ve.12.2 ProcedureDetermine the power factor and dielectricconstant and report in accordance with the procedure specifiedfor films in Test Methods D 150.13. Dielectric Strength of a Dried or Cured AdhesiveFilm13.1 Test Specimens Prepare test specimens in accordancewith 12.1.13.2 ProcedureDetermine di
38、electric strength and reportin accordance with the procedure specified for determining thedielectric strength of dried varnish film in Test Methods D115.14. Volume and Surface Resistivity14.1 Test Specimens Test specimens for use in determin-ing the volume and surface resistivity of solid adhesives
39、shallconsist 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 bond
40、ed bythe 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 D 897. Thickness of the glue line shall b
41、e not 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 D 257. The voltage applied shall not exceed 30 V/mil.Read at the end of 1 min electrification.15. Arc Res
42、istance15.1 Test Specimens Prepare 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 (
43、0.13 mm).15.2 ProcedureDetermine the arc resistance of solid ad-hesives and report in accordance with Test Method D 495.16. Report16.1 Report the following information:16.1.1 Complete identification of the adherend and adhesivematerials tested, including adhesive type, source, and manu-facturers cod
44、e number.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-centimete
45、rs, of each 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 D 150.16.1.11 Dire
46、ct-current conductivity as in Test MethodsD 257.16.1.12 Extract conductivity as in Test Methods D 202.16.1.13 Acidity and alkalinity as in Test Methods D 202.16.1.14 pH value as in Test Methods D 202.16.1.15 Volume and surface resistivity as in Test MethodsD 257.16.1.16 Arc resistance as in Test Met
47、hod D 495.17. Precision 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 afuncti
48、on of the adhesive system, surface preparation, sub-strates, test temperature, cyclic stress level, and other factorsrelated to the test apparatus, laboratory, and operator variabili-ties. Precision shall be reported in terms of the standarddeviation of the data and the standard error of the mean.18
49、. Keywords18.1 adhesives; 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 SurfaceResistivity.D 1304 99 (2005)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 i
