ASTM D721-06(2011)
(Test Method)Standard Test Method for Oil Content of Petroleum Waxes
Standard Test Method for Oil Content of Petroleum Waxes
SIGNIFICANCE AND USE
The oil content of a wax may have significant effects on several of its properties, such as strength, hardness, flexibility, scuff resistance, coefficient of friction, coefficient of expansion, melting point, and oil straining. The importance of these effects may be dependent upon the ultimate use of the wax.
SCOPE
1.1 This test method covers the determination of oil in petroleum waxes having a congealing point of 30°C (86°F) or higher as determined in accordance with Test Method D938, and containing not more than 15 % of oil.
Note 1—With some types of waxes, of oil contents greater than 5 %, there may be an incompatibility with MEK resulting in the formation of two liquid phases. If this occurs, the test method is not applicable to the material under test.
1.2 The values stated in inch-pound units are to be regarded as standard. The values given in parentheses are mathematical conversions to SI units that are provided for information only and are not considered standard.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
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Standards Content (Sample)
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Designation: D721 − 06(Reapproved 2011)
Designation: 158/69(85)
Standard Test Method for
Oil Content of Petroleum Waxes
This standard is issued under the fixed designation D721; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope E128 Test Method for Maximum Pore Diameter and Perme-
ability of Rigid Porous Filters for Laboratory Use
1.1 This test method covers the determination of oil in
2.2 Energy Institute Standards:
petroleum waxes having a congealing point of 30°C (86°F) or
Specification for IP Standard Thermometers
higher as determined in accordance with Test Method D938,
and containing not more than 15 % of oil.
3. Summary of Test Method
NOTE 1—With some types of waxes, of oil contents greater than 5 %,
3.1 The sample is dissolved in methyl ethyl ketone, the
there may be an incompatibility with MEK resulting in the formation of
solution cooled to –32°C (–25°F) to precipitate the wax, and
two liquid phases. If this occurs, the test method is not applicable to the
material under test.
filtered. The oil content of the filtrate is determined by
evaporating the methyl ethyl ketone and weighing the residue.
1.2 The values stated in inch-pound units are to be regarded
as standard. The values given in parentheses are mathematical
4. Significance and Use
conversions to SI units that are provided for information only
and are not considered standard. 4.1 The oil content of a wax may have significant effects on
several of its properties, such as strength, hardness, flexibility,
1.3 This standard does not purport to address all of the
scuffresistance,coefficientoffriction,coefficientofexpansion,
safety concerns, if any, associated with its use. It is the
meltingpoint,andoilstraining.Theimportanceoftheseeffects
responsibility of the user of this standard to establish appro-
may be dependent upon the ultimate use of the wax.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
5. Apparatus
2. Referenced Documents 5.1 Filter Stick and Assembly, consisting of a 10-mm
diameter sintered glass filter stick of 10 to 15 µm maximum
2.1 ASTM Standards:
pore diameter as determined by the method in Appendix X1,
D938 Test Method for Congealing Point of Petroleum
provided with an air pressure inlet tube and delivery nozzle. It
Waxes, Including Petrolatum
is provided with a ground-glass joint to fit a 25 by 170-mm test
E1 Specification for ASTM Liquid-in-Glass Thermometers
tube. The dimensions for a suitable filtration assembly are
shown in Fig. 1.
This test method is under the jurisdiction of ASTM Committee D02 on
NOTE 2—A metallic filter stick may be employed if desired. A filter
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of 1
stick made of stainless steel and having a 12.7–mm ( ⁄2-in.) disk of 10 to
Subcommittee D02.10.0A on Physical/Chemical Properties.
15-µm maximum pore diameter, as determined by Test Method E128, has
Current edition approved Oct. 1, 2011. Published October 2011. Originally 5
been found to be satisfactory. The metallic apparatus is inserted into a 25
approved in 1943. Last previous edition approved in 2006 as D721-06. DOI:
by 150–mm test tube and held in place by means of a cork.
10.1520/D0721-06R11.
In the IP, this test method is under the jurisdiction of the Standardization
Committee. This test method was issued as a joint ASTM-IP tentative in 1964.
This test method was prepared jointly by the Technical Association of Pulp and Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR,
Paper Industry and ASTM International. U.K.
This test method has been adopted for use by government agencies to replace The sole source of supply of a suitable metal filter stick with designated
Method 5431 of Federal Test Method Standard No. 79lb. porosity G known to the committee at this time is the Pall Corporation, 2200
This test method is being used by some laboratories for products of higher oil Northern Boulevard East Hills, NY 11548. A list of United Kingdom suppliers can
content. be obtained from Energy Institute, 61 New Cavendish St., London, W1G 7AR,
For referenced ASTM standards, visit the ASTM website, www.astm.org, or United Kingdom. If you are aware of alternative suppliers, please provide this
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM information to ASTM International Headquarters. Your comments will receive
Standards volume information, refer to the standard’s Document Summary page on careful consideration at a meeting of the responsible technical committee, which
the ASTM website. you may attend.
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D721 − 06 (2011)
Thermometer Number
Temperature Range ASTM IP
–37 to +21°C 71C 72C
–35 to +70°F 71F 72F
5.6.2 Temperature measuring devices other than those de-
scribed in 5.6.1 are satisfactory for this test method, provided
that they exhibit the same temperature response as the equiva-
lent mercury-in-glass thermometers.
5.7 Weighing Bottles, glass-stoppered, having a typical ca-
pacity of 15 to 25 mL.
5.8 Evaporation Assembly, consisting of an evaporating
cabinet and connections, essentially as illustrated in Fig. 4, and
capable of maintaining a temperature of 35 6 1°C (95 6 2°F)
around the evaporation flask. Construct the jets with an inside
diameter of 4 6 0.2 mm for delivering a stream of clean, dry
air vertically downward into the weighing bottle. Support each
jet so that the tip is 15 6 5 mm above the surface of the liquid
at the start of the evaporation. Supply purified air at the rate of
2 to 3 L/min per jet. One way to purify the air is by passage
throughatubeofapproximately10-mmborepackedlooselyto
a height of approximately 200 mm with absorbent cotton.
Periodically check the cleanliness of the air by evaporating 4
mL of methyl ethyl ketone by the procedure specified in 8.5.
When the residue does not exceed 0.1 mg, the evaporation
equipment is operating satisfactorily.
All dimensions are in millimetres
5.9 Analytical Balance, capable of reproducing weights to
FIG. 1 Filter Stick
0.1 mg.
5.10 Wire Stirrer—A piece of stiff wire, made of iron,
5.2 Cooling Bath, consisting of an insulated box with 30 6
stainless steel, or Nichrome wire of about No. 20 B & S (0.9
5-mm (1.2 6 0.2-in.) holes in the center to accommodate any
mm in diameter) or 16 swg gage, 250 mm long. A 10-mm
desired number of test tubes. The bath may be filled with a
diameter loop is formed at eachend, and the loopatthebottom
suitable medium such as kerosine, and may be cooled by
end is bent so that the plane of the loop is perpendicular to the
circulating a refrigerant through coils, or by using solid carbon
wire.
dioxide. A suitable cooling bath to accommodate three test
tubes is shown in Fig. 2.
6. Reagents
5.3 Pipet, or equivalent dispensing device capable of deliv-
6.1 Methyl Ethyl Ketone,conformingtothespecificationsof
ering 1 6 0.05 g of molten wax.
theCommitteeonAnalyticalReagentsoftheAmericanChemi-
5.4 Transfer Pipet, or equivalent volume dispensing device, cal Society.
capable of delivering 15 6 0.06 mL.
6.2 Store the solvent over anhydrous calcium sulfate (5
5.5 Air Pressure Regulator, designed to supply air to the weight % of the solvent). Filter prior to use.
filtration assembly (8.5) at the volume and pressure required to
6.3 Air Supply, clean and filtered.
give an even flow of filtrate. Either the conventional pressure-
NOTE 3—As an alternative, it is permissible to replace all references to
reducing valve or a mercury bubbler-type regulator has been
“air”usedinthesolventevaporationprocesswith“nitrogen,”providedthe
nitrogen is clean and filtered. It should be noted, however, that the
found satisfactory.The latter type, illustrated in Fig. 3, consists
precision statements for the test method were determined using air only
of a 250-mLglass cylinder and aT-tube held in the cylinder by
and that the precision associated with using nitrogen has not been
means of a rubber stopper grooved at the sides to permit the
determined.
escape of excess air. The volume and pressure of the air
supplied to the filtration assembly is regulated by the depth to
7. Sample
which the T-tube is immersed in mercury at the bottom of the
7.1 If the sample of wax is 1 kg (2 lb) or less, obtain a
cylinder. Absorbent cotton placed in the space above the
representative portion by melting the entire sample and stirring
mercury prevents the loss of mercury by spattering. The air
pressureregulatoryisconnectedtothefilterstickandassembly
by means of rubber tubing.
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For Suggestions on the testing of reagents not
5.6 Temperature Measuring Device:
listed by the American Chemical Society, see Annual Standards for Laboratory
5.6.1 Thermometer, having a range as shown below and
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
conforming to the requirements as prescribed in Specification
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
E1, or in the Specification for IP Standard Thermometers. MD.
D721 − 06 (2011)
All dimensions are in millimetres (inches)
FIG. 2 Cooling Bath
solvents will not vary to a significant extent. Therefore, a tare weight may
thoroughly. For samples over 1 kg (2 lb), exercise special care
be obtained and used repeatedly.
to ensure obtaining a truly representative portion, bearing in
8.2 Pipet15mLofmethylethylketoneintothetesttubeand
mind that the oil may not be distributed uniformly throughout
the sample, and that mechanical operations may express some place the latter just up to the level of its contents in a hot water
or steam bath. Heat the solvent wax mixture, stirring up and
of the oil.
down with the wire stirrer, until a homogeneous solution is
8. Procedure
obtained. Exercise care to avoid loss of solvent by prolonged
b
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