ASTM D1168-99(2003)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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An American National Standard
Designation:D1168–99 (Reapproved 2003)
Standard Test Methods for
Hydrocarbon Waxes Used for Electrical Insulation
This standard is issued under the fixed designation D1168; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope D127 Test Method for Drop Melting Point of Petroleum
Wax, Including Petrolatum
1.1 These test methods cover a compendium of tests that
D176 Test Methods for Solid Filling and Treating Com-
apply to mineral waxes of petroleum origin in general, but
pounds Used for Electrical Insulation
more specifically to the so-called microcrystalline types used
D445 Test Method for Kinematic Viscosity of Transparent
aseitherelectricalinsulationormoisture-proofingmediums,or
and Opaque Liquids (the Calculation of Dynamic Viscos-
both, for treating, impregnating, coating, and filling electrical
ity)
apparatus. These test methods are also applicable to other
D664 TestMethodforAcidNumberofPetroleumProducts
waxes of natural or synthetic origin, provided that their
by Potentiometric Titration
characteristics are similar to those of the so-called microcrys-
D937 Test Method for Cone Penetration of Petrolatum
talline waxes.
D938 Test Method for Congealing Point of Petroleum
NOTE 1—There is no equivalent ISO or IEC standard.
Waxes, Including Petrolatum
1.2 The values stated in SI units are the standard. D974 Test Method for Acid and Base Number by Color-
1.3 This standard does not purport to address all of the Indicator Titration
safety concerns, if any, associated with its use. It is the D1321 Test Method for Needle Penetration of Petroleum
responsibility of the user of this standard to establish appro- Waxes
priate safety and health practices and determine the applica- D1500 Test Method for ASTM Color of Petroleum Prod-
bility of regulatory limitations prior to use. For specific ucts (ASTM Color Scale)
precautions, see Section 5. D1711 Terminology Relating to Electrical Insulation
D2161 Practice for Conversion of Kinematic Viscosity to
2. Referenced Documents
Saybolt Universal Viscosity or to Saybolt Furol Viscosity
2.1 ASTM Standards:
E28 Test Method for Softening Point of Resins Derived
D6 Test Method for Loss on Heating of Oil and Asphaltic from Naval Stores by Ring-and-Ball Apparatus
Compounds
3. Terminology
D70 Test Method for Specific Gravity and Density of
Semi-Solid Bituminous Materials (Pycnometer Method) 3.1 Definitions—For definitions of terms used in these test
D87 Test Method for Melting Point of Petroleum Wax methods, refer to Terminology D1711.
(Cooling Curve)
4. Significance and Use
D88 Test Method for Saybolt Viscosity
D92 Test Method for Flash and Fire Points by Cleveland 4.1 The significance and use of the individual test methods
are to be found in the individual methods referenced. For
Open Cup Tester
D94 Test Method for Saponification Number of Petroleum significance specifically applicable to electrical insulation ma-
terials, refer to Test Methods D176.
Products
5. Safety Precautions
These methods are under the jurisdiction of ASTM Committee D09 on
5.1 Ovens in which waxes are heated should have low-
Electrical and Electronic Insulating Materials and are the direct responsibility of
temperature heating elements, forced exhaust, and safety door
Subcommittee D09.01 on Electrical Insulating Varnishes, Powders, and Encapsu-
latches to minimize the hazard of explosion of vapors.
lating Compounds.
Current edition approved March 10, 1999. Published June 1999. Originally
6. Test Methods
approved in 1951. Last previous edition approved in 1999 as D1168–99.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
6.1 Use the following methods for testing hydrocarbon
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
waxes as specified for the individual material:
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. 6.1.1 Color—Test Method D1500.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D1168–99 (2003)
6.1.2 Melting and Softening Properties: madeatseveraltemperaturesfromwhichvolumecoefficientof
6.1.2.1 Determine melting point by Test Method D127. expansion can be calculated.
6.1.2.2 Determine softening point by the ring-and-ball Test
VOLUME CONTRACTION ON COOLING
MethodE28. Make three measurements. If any measurement
differs from the average by more than 1°C, the significance of
7. Scope
the test is doubtful.
7.1 This test method measures the volume contraction of
6.1.2.3 Use Test Method D87 for melting point of waxes
microcrystalline wax to be used for electrical insulation when
having a plateau in their cooling curve.
cooled from 5.5°C (10°F) above its melting point to 27.8°C
6.1.2.4 Determine the congealing point by Test Method
(50°F) below its melting point.
D938. (The test value will usually be lower than the melting
7.2 The total contraction from a temperature of 5.5°C
point determined by Test Method D127.)
(10°F) above the melting point to a temperature of 27.8°C
6.1.3 Penetration:
(50°F) below the melting point has been used in defining a
6.1.3.1 UseTestMethodD1321forallbutverysoftwaxes.
crystallinity index, which may be employed to classify micro-
6.1.3.2 Use Test Method D937 for soft waxes below the
and macrocrystalline waxes.
range for Test Method D1321.
7.3 This test method can also be used to determine the
6.1.3.3 Report the test method used.
contraction occurring between temperatures other than those
6.1.4 Viscosity:
specified in this section, but in this case the temperature limits
6.1.4.1 Unlessotherwisespecified,measureSayboltUniver-
should be stated.
sal Viscosity at 99°C (210°F) using Test MethodD88.
6.1.4.2 When specified, Test Method D445 or measure-
8. Apparatus
ments at other temperatures may be made.
8.1 Mixing Cylinder, 100-mL capacity.
6.1.4.3 Use Practice D2161 for conversion of viscosity
8.2 Water Bath, capable of maintaining the test temperature
values.
within 60.5°C (61°F), and permitting submersion of at least
6.1.5 Flash and Fire Points—Test MethodD92.
the graduated portion of a 100-mL mixing cylinder.
6.1.6 Loss on Heating:
6.1.6.1 Determine by Test MethodD6.
9. Procedure
6.1.6.2 For some waxes subject to oxidation on heating and
9.1 Heat the sample to 5.5°C (10°F) above its melting point
due to lack of close control of air circulation, the reproducibil-
(Test Method D127) and pour exactly 100 mL of the heated
ity of results may be variable.
sampleintoa100-mLmixingcylinderthathasbeenbroughtto
6.1.7 Saponification Number:
the same temperature.Allow the wax to cool for 2 h, protected
6.1.7.1 Determine using Test Method D94, modified as
from drafts.
specified in 6.1.7.2-6.1.7.4.
9.2 If a thin wax layer covers the cavity formed on cooling,
6.1.7.2 Use solvent mixtures appropriate to the melting
pierce the wax layer at the center with a pointed glass rod to
point of the wax being tested as follows:
make an opening 2 to 3 mm in diameter.
74.8°C ethanol-methyl ethyl ketone
9.3 Immersethemixingcylinderinawaterbathmaintained
77.3°C isopropanol-methyl ethyl ketone
80.6°C isopropanol-toluol at 27.8°C (50°F) below the melting point of the wax for 2 h.
92.6°C N-propanol-toluol
Remove the cylinder from the bath and add a 50% aqueous
solution of glycerin from a buret to reach the 100-mL mark.
6.1.7.3 Do not use the ASTM precipitation naphtha.
Apply a slight vacuum to the cylinder to remove any trapped
6.1.7.4 Reheat the solution when necessary during titration.
air, and add more glycerin solution if necessary. Note the total
6.1.8 Acid and Base Number:
millilitresofglycerinsolutionadded,andreportas“percentage
6.1.8.1 Determine using Test Method D664.
contraction.” The percentage expansion is 100 times the
6.1.8.2 When the color of the material permits, and when
reciprocal of (100−percentage contraction) multiplied by the
specified for the material, Test Method D974 may be used.
percentage contraction.
6.1.8.3 Thetestresultsonagivensamplemayvarydepend-
ing upon the method used.
10. Precision and Bias
6.1.9 Electrical Properties—Determine using methods
10.1 Operators familiar with this method estimate that
specified in Test Methods D176.
duplicate determinations by the same operator should differ by
6.1.10 Density and Volume Changes:
nomorethan2%ofthevalue,andbydifferentoperatorsusing
6.1.10.1 Measure specific gravity at 25°C (77°F) by Test
different apparatus, by no more than 5%. This precision
MethodD70 using the procedure for cements and pitches.
applies to the usual waxes and over the range from 5.5°C
6.1.10.2 Measure volume contraction on cooling from liq-
(10°F) above to 27.8°C (50°F) below the melting point.
uid to solid using the procedures in Sections 7-10 of these test
10.2 A statement of bias is not applicable since a standard
methods.
reference material for this property is unavailable.
6.1.10.3 Measure density at specified temperatures (either
beloworabovethemeltingpoint)usingproceduresinSections
11-18 of these test methods. From the density measurement,
See Kinsel, A., and Phillips, J., “Method for Classification of Petroleum
specific gravity and specific volume may be calculated. When
Waxes,” Industrial and Engineering Chemistry,IECHA,Vol17,March15,1945,p.
specified for a given material, density measurements can be 152.
D1168–99 (2003)
DENSITY 13. Standardization of Dilatometer
13.1 Standardize the dilatometer as follows so that its exact
11. Scope
volumetric capacity at each of the calibration points will be
known:
11.1 This test method determines density of wax and like
13.1.1 Clean the dilatometer with chromic acid, and rinse a
material, in both the solid and liquid phases. The results are
number of times with distilled water. Dry, either by heating in
obtained by determining the mass and volume of a liquid of
an oven at 121
...