1、Designation: D 1168 99 (Reapproved 2003)An American National StandardStandard Test Methods forHydrocarbon Waxes Used for Electrical Insulation1This standard is issued under the fixed designation D 1168; the number immediately following the designation indicates the year oforiginal adoption or, in th
2、e case of revision, the 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 a compendium of tests thatapply to mineral waxes of petroleu
3、m origin in general, butmore specifically to the so-called microcrystalline types usedas either electrical insulation or moisture-proofing mediums, orboth, for treating, impregnating, coating, and filling electricalapparatus. These test methods are also applicable to otherwaxes of natural or synthet
4、ic origin, provided that theircharacteristics are similar to those of the so-called microcrys-talline waxes.NOTE 1There is no equivalent ISO or IEC standard.1.2 The values stated in SI units are the standard.1.3 This standard does not purport to address all of thesafety concerns, if any, associated
5、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. For specificprecautions, see Section 5.2. Referenced Documents2.1 ASTM Standards:2D6 Test Method for Loss
6、on Heating of Oil and AsphalticCompoundsD70 Test Method for Specific Gravity and Density ofSemi-Solid Bituminous Materials (Pycnometer Method)D87 Test Method for Melting Point of Petroleum Wax(Cooling Curve)D88 Test Method for Saybolt ViscosityD92 Test Method for Flash and Fire Points by ClevelandOp
7、en Cup TesterD94 Test Method for Saponification Number of PetroleumProductsD 127 Test Method for Drop Melting Point of PetroleumWax, Including PetrolatumD 176 Test Methods for Solid Filling and Treating Com-pounds Used for Electrical InsulationD 445 Test Method for Kinematic Viscosity of Transparent
8、and Opaque Liquids (the Calculation of Dynamic Viscos-ity)D 664 Test Method forAcid Number of Petroleum Productsby Potentiometric TitrationD 937 Test Method for Cone Penetration of PetrolatumD 938 Test Method for Congealing Point of PetroleumWaxes, Including PetrolatumD 974 Test Method for Acid and
9、Base Number by Color-Indicator TitrationD 1321 Test Method for Needle Penetration of PetroleumWaxesD 1500 Test Method for ASTM Color of Petroleum Prod-ucts (ASTM Color Scale)D 1711 Terminology Relating to Electrical InsulationD 2161 Practice for Conversion of Kinematic Viscosity toSaybolt Universal
10、Viscosity or to Saybolt Furol ViscosityE28 Test Method for Softening Point of Resins Derivedfrom Naval Stores by Ring-and-Ball Apparatus3. Terminology3.1 DefinitionsFor definitions of terms used in these testmethods, refer to Terminology D 1711.4. Significance and Use4.1 The significance and use of
11、the individual test methodsare to be found in the individual methods referenced. Forsignificance specifically applicable to electrical insulation ma-terials, refer to Test Methods D 176.5. Safety Precautions5.1 Ovens in which waxes are heated should have low-temperature heating elements, forced exha
12、ust, and safety doorlatches to minimize the hazard of explosion of vapors.6. Test Methods6.1 Use the following methods for testing hydrocarbonwaxes as specified for the individual material:6.1.1 ColorTest Method D 1500.1These methods are under the jurisdiction of ASTM Committee D09 onElectrical and
13、Electronic Insulating Materials and are the direct responsibility ofSubcommittee D09.01 on Electrical Insulating Varnishes, Powders, and Encapsu-lating Compounds.Current edition approved March 10, 1999. Published June 1999. Originallyapproved in 1951. Last previous edition approved in 1999 as D 1168
14、 99.2For 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 Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO
15、Box C700, West Conshohocken, PA 19428-2959, United States.6.1.2 Melting and Softening Properties:6.1.2.1 Determine melting point by Test Method D 127.6.1.2.2 Determine softening point by the ring-and-ball TestMethod E28. Make three measurements. If any measurementdiffers from the average by more tha
16、n 1C, the significance ofthe test is doubtful.6.1.2.3 Use Test Method D87for melting point of waxeshaving a plateau in their cooling curve.6.1.2.4 Determine the congealing point by Test MethodD 938. (The test value will usually be lower than the meltingpoint determined by Test Method D 127.)6.1.3 Pe
17、netration:6.1.3.1 Use Test Method D 1321 for all but very soft waxes.6.1.3.2 Use Test Method D 937 for soft waxes below therange for Test Method D 1321.6.1.3.3 Report the test method used.6.1.4 Viscosity:6.1.4.1 Unless otherwise specified, measure Saybolt Univer-sal Viscosity at 99C (210F) using Tes
18、t Method D88.6.1.4.2 When specified, Test Method D 445 or measure-ments at other temperatures may be made.6.1.4.3 Use Practice D 2161 for conversion of viscosityvalues.6.1.5 Flash and Fire PointsTest Method D92.6.1.6 Loss on Heating:6.1.6.1 Determine by Test Method D6.6.1.6.2 For some waxes subject
19、to oxidation on heating anddue to lack of close control of air circulation, the reproducibil-ity of results may be variable.6.1.7 Saponification Number:6.1.7.1 Determine using Test Method D94, modified asspecified in 6.1.7.2-6.1.7.4.6.1.7.2 Use solvent mixtures appropriate to the meltingpoint of the
20、 wax being tested as follows:74.8C ethanol-methyl ethyl ketone77.3C isopropanol-methyl ethyl ketone80.6C isopropanol-toluol92.6C N-propanol-toluol6.1.7.3 Do not use the ASTM precipitation naphtha.6.1.7.4 Reheat the solution when necessary during titration.6.1.8 Acid and Base Number:6.1.8.1 Determine
21、 using Test Method D 664.6.1.8.2 When the color of the material permits, and whenspecified for the material, Test Method D 974 may be used.6.1.8.3 The test results on a given sample may vary depend-ing upon the method used.6.1.9 Electrical PropertiesDetermine using methodsspecified in Test Methods D
22、 176.6.1.10 Density and Volume Changes:6.1.10.1 Measure specific gravity at 25C (77F) by TestMethod D70using the procedure for cements and pitches.6.1.10.2 Measure volume contraction on cooling from liq-uid to solid using the procedures in Sections 7-10 of these testmethods.6.1.10.3 Measure density
23、at specified temperatures (eitherbelow or above the melting point) using procedures in Sections11-18 of these test methods. From the density measurement,specific gravity and specific volume may be calculated. Whenspecified for a given material, density measurements can bemade at several temperatures
24、 from which volume coefficient ofexpansion can be calculated.VOLUME CONTRACTION ON COOLING7. Scope7.1 This test method measures the volume contraction ofmicrocrystalline wax to be used for electrical insulation whencooled from 5.5C (10F) above its melting point to 27.8C(50F) below its melting point.
25、7.2 The total contraction from a temperature of 5.5C(10F) above the melting point to a temperature of 27.8C(50F) below the melting point has been used in defining acrystallinity index, which may be employed to classify micro-and macrocrystalline waxes.37.3 This test method can also be used to determ
26、ine thecontraction occurring between temperatures other than thosespecified in this section, but in this case the temperature limitsshould be stated.8. Apparatus8.1 Mixing Cylinder, 100-mL capacity.8.2 Water Bath, capable of maintaining the test temperaturewithin 60.5C (61F), and permitting submersi
27、on of at leastthe graduated portion of a 100-mL mixing cylinder.9. Procedure9.1 Heat the sample to 5.5C (10F) above its melting point(Test Method D 127) and pour exactly 100 mL of the heatedsample into a 100-mL mixing cylinder that has been brought tothe same temperature. Allow the wax to cool for 2
28、 h, protectedfrom drafts.9.2 If a thin wax layer covers the cavity formed on cooling,pierce the wax layer at the center with a pointed glass rod tomake an opening 2 to 3 mm in diameter.9.3 Immerse the mixing cylinder in a water bath maintainedat 27.8C (50F) below the melting point of the wax for 2 h
29、.Remove the cylinder from the bath and add a 50 % aqueoussolution of glycerin from a buret to reach the 100-mL mark.Apply a slight vacuum to the cylinder to remove any trappedair, and add more glycerin solution if necessary. Note the totalmillilitres of glycerin solution added, and report as “percen
30、tagecontraction.” The percentage expansion is 100 times thereciprocal of (100 percentage contraction) multiplied by thepercentage contraction.10. Precision and Bias10.1 Operators familiar with this method estimate thatduplicate determinations by the same operator should differ byno more than 2 % of
31、the value, and by different operators usingdifferent apparatus, by no more than 5 %. This precisionapplies to the usual waxes and over the range from 5.5C(10F) above to 27.8C (50F) below the melting point.10.2 A statement of bias is not applicable since a standardreference material for this property
32、 is unavailable.3See Kinsel, A., and Phillips, J., “Method for Classification of PetroleumWaxes,” Industrial and Engineering Chemistry, IECHA, Vol 17, March 15, 1945, p.152.D 1168 99 (2003)2DENSITY11. Scope11.1 This test method determines density of wax and likematerial, in both the solid and liquid
33、 phases. The results areobtained by determining the mass and volume of a liquid ofknown density, and the wax in a dilatometer, over a tempera-ture range from 15.5 to 99C (60 to 210F). From these datathe density, specific volume, specific gravity, and cubicalexpansion of the wax can be calculated.12.
34、 Apparatus and Materials12.1 Dilatometer, constructed of heat-resistant glass asshown in Fig. 1.12.2 Glass-Walled Constant-Temperature Water or OilBath, of such depth as to permit observation of the submergedactive length of the capillary arm of the dilatometer.12.3 Analytical Balance.12.4 Wooden Fr
35、ames and Cellulose Film or Shallow MetalContainer, for casting wax specimens.12.5 Glycerin, cp.13. Standardization of Dilatometer13.1 Standardize the dilatometer as follows so that its exactvolumetric capacity at each of the calibration points will beknown:13.1.1 Clean the dilatometer with chromic a
36、cid, and rinse anumber of times with distilled water. Dry, either by heating inan oven at 121C (250F) for 30 min or by rinsing withacetone. If acetone is used, remove all traces of vapor bysuction.13.1.2 Assemble the dilatometer, using a minimum amountof stopcock lubricant.13.1.3 Determine the mass
37、of the instrument on a balance,using a suitable hanger for suspending the dilatometer from thepan stirrup. Note the position of the dilatometer, and replace itin a like position for each successive weighing.13.1.4 Deaerate distilled water by boiling vigorously. Coolslowly, without stirring, to appro
38、ximately 15C (60F).13.1.5 Charge the dilatometer with the prepared distilledwater. Draw the water up into the capillary to approximatelythe 1.8-mL point by applying gentle suction. Replace the plug,with stopcock open, and permit the excess water to drain out.Close the stopcock and remove all traces
39、of water from thestopcock outlet tube and from the hole through the body andplug of the stopcock. Dry the outside of the dilatometer anddetermine the mass of the water.13.1.6 Place in a constant-temperature bath at 20 6 0.05C(68 6 0.1F) and, when temperature equilibrium is attained asindicated by th
40、e constancy of volume readings at three succes-sive 5-min intervals, record the volume reading.13.1.7 Remove the dilatometer from the bath and changethe mass of water by opening the stopcock and drawing off aportion, lowering the volume in the capillary to about the 0.2point. Remove all moisture, an
41、d weigh as described in 13.1.5.13.1.8 Repeat the procedure described in 13.1.6.13.1.9 Remove the dilatometer from the bath and repeat theprocedure described in 13.1.1, 13.1.2, 13.1.3, and 13.1.5, andcharging the dilatometer so that the capillary arm will be filledto the 1.3-mL point, and repeating 1
42、3.1.6 and 13.1.7.Inrepeating the procedure in 13.1.7, lower the capillary volumeto the 0.6 point.13.1.10 From the volume readings, mass of water, and thestandard tabulated value of the density of water, calculate thevolume at each of the determined points. The four volumereadings, when plotted, shal
43、l fall on a straight line. From thisgraph determine the volumetric capacity of the dilatometer ateach test temperature.14. Preparation of Specimens14.1 Heat the sample to approximately 17C (30F) aboveits melting point and pour into a shallow container to a liquiddepth of approximately 3 mm (18 in.).
44、 A suitable container foruse in the preparation of test specimens consists of a membraneof regenerated cellulose film stretched across a rectangularopening between a four-sided wooden frame, approximately 3by 5 in. (76 by 127 mm), made from 12 by 31-mm (12 by114-in.) maple wood. The film may be fast
45、ened to the woodenframe by pressure-sensitive tape or thumb tacks. After mount-ing the film, place a second wooden frame, identical in sizeMetric Equivalentsin. mm13 330214 5734 19FIG. 1 DilatometerD 1168 99 (2003)3with the first, on top of the film and line up the two frames.Give the lower inner fa
46、ces of the upper frame a thin coating ofclear amber petrolatum to facilitate removal of the cake ofsolidified wax. Cover the sample with a sheet of metal orcardboard to reduce heat losses, and permit it to cool until itsolidifies. When the wax has cooled to room temperature,remove it from the contai
47、ner by rapidly chilling it in anice-water bath. This will cause the sample to contract andpermit its easy removal in thin cake form. Strip the film fromthe wax sample. Select a section of the cake that is free fromall visible entrained air bubbles and cut in 50 by 9.5-mm (2 by38-in.) pieces. Smooth
48、cut sides to eliminate all voids either byheating the cut sides or by mechanical means.15. Determination of Density of Glycerin15.1 To ensure the effective cancellation of buoyancy,meniscus, and other minor errors, determine the density of theglycerin over the entire temperature range as follows:15.
49、1.1 Repeat the procedure described in 13.1.1, 13.1.2, and13.1.3.15.1.2 Carefully charge the dilatometer with the glycerin toavoid entrainment of air bubbles. When properly charged, themeniscus of the glycerin in the capillary arm will be slightlyabove the first calibration mark at the bottom of the capillary.Carefully remove all excess glycerin from the exterior andfrom the stopcock as described in 13.1.5.15.1.3 Determine the mass of the glycerin, taking cogni-zance of the position of the dilatometer as pointed in 13.1.3.15.1.4 Plac
