An American National Standard

Designation: D 721 – 06

Designation: 158/69(85)

Standard Test Method for

Oil Content of Petroleum Waxes1
This standard is issued under the fixed designation D 721; 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 Department of Defense.

1. Scope* E 128 Test Method for Maximum Pore Diameter and Per-
1.1 This test method covers the determination of oil in meability of Rigid Porous Filters for Laboratory Use
petroleum waxes having a congealing point of 30°C (86°F) or 2.2 Energy Institute Standards:
higher as determined in accordance with Test Method D 938, Specification for IP Standard Thermometers4
and containing not more than 15 % of oil.2 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 4.1 The oil content of a wax may have significant effects on
and are not considered standard. several of its properties, such as strength, hardness, flexibility,
1.3 This standard does not purport to address all of the scuff resistance, coefficient of friction, coefficient of expansion,
safety concerns, if any, associated with its use. It is the melting point, and oil straining. The importance of these effects
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:3 pore diameter as determined by the method in Appendix X1,
D 938 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
E 1 Specification for ASTM Liquid-in-Glass Thermometers tube. The dimensions for a suitable filtration assembly are
shown in Fig. 1.
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 and Lubricants and is the direct responsibility of Subcommittee stick made of stainless steel and having a 12.7–mm (1⁄2-in.) disk of 10 to
D02.10.0A on Physical/Chemical Properties. 15-µm maximum pore diameter, as determined by Test Method E 128, has
Current edition approved Nov. 1, 2006. Published November 2006. Originally been found to be satisfactory.5 The metallic apparatus is inserted into a 25
approved in 1943. Last previous edition approved in 2005 as D 721-05.
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.
4
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.
5
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
2
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,
3
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 [email protected]. 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,1 which
the ASTM website. you may attend.

*A Summary of Changes section appears at the end of this standard.

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 D 721 – 06
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
through a tube of approximately 10-mm bore packed loosely to
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
All dimensions are in millimetres equipment is operating satisfactorily.
FIG. 1 Filter Stick 5.9 Analytical Balance, capable of reproducing weights to
0.1 mg.
5.10 Wire Stirrer—A piece of stiff wire, made of iron,
by 150–mm test tube and held in place by means of a cork.
stainless steel, or Nichrome wire of about No. 20 B & S (0.9
mm in diameter) or 16 swg gage, 250 mm long. A 10-mm
5.2 Cooling Bath, consisting of an insulated box with 30 6 diameter loop is formed at each end, and the loop at the bottom
5-mm (1.2 6 0.2-in.) holes in the center to accommodate any end is bent so that the plane of the loop is perpendicular to the
desired number of test tubes. The bath may be filled with a wire.
suitable medium such as kerosine, and may be cooled by
circulating a refrigerant through coils, or by using solid carbon 6. Reagents
dioxide. A suitable cooling bath to accommodate three test 6.1 Methyl Ethyl Ketone, conforming to the specifications of
tubes is shown in Fig. 2. the Committee on Analytical Reagents of the American Chemi-
5.3 Pipet, or equivalent dispensing device capable of deliv- cal Society.6
ering 1 6 0.05 g of molten wax. 6.2 Store the solvent over anhydrous calcium sulfate (5
5.4 Transfer Pipet, or equivalent volume dispensing device, weight % of the solvent). Filter prior to use.
capable of delivering 15 6 0.06 mL. 6.3 Air Supply, clean and filtered.
5.5 Air Pressure Regulator, designed to supply air to the
NOTE 3—As an alternative, it is permissible to replace all references to
filtration assembly (8.5) at the volume and pressure required to “air” used in the solvent evaporation process with “nitrogen,” provided the
give an even flow of filtrate. Either the conventional pressure- nitrogen is clean and filtered. It should be noted, however, that the
reducing valve or a mercury bubbler-type regulator has been precision statements for the test method were determined using air only
found satisfactory. The latter type, illustrated in Fig. 3, consists and that the precision associated with using nitrogen has not been
of a 250-mL glass cylinder and a T-tube held in the cylinder by determined.
means of a rubber stopper grooved at the sides to permit the
7. Sample
escape of excess air. The volume and pressure of the air
supplied to the filtration assembly is regulated by the depth to 7.1 If the sample of wax is 1 kg (2 lb) or less, obtain a
which the T-tube is immersed in mercury at the bottom of the representative portion by melting the entire sample and stirring
cylinder. Absorbent cotton placed in the space above the thoroughly. For samples over 1 kg (2 lb), exercise special care
mercury prevents the loss of mercury by spattering. The air
pressure regulatory is connected to the filter stick and assembly
by means of rubber tubing. 6
Reagent Chemicals, American Chemical Society Specifications, American
5.6 Temperature Measuring Device: Chemical Society, Washington, DC. For Suggestions on the testing of reagents not
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,
E 1, or in the Specification for IP Standard Thermometers. MD.

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 D 721 – 06

All dimensions are in millimetres (inches)

FIG. 2 Cooling Bath

to ensure obtaining a truly representative portion, bearing in be obtained and used repeatedly.
mind that the oil may not be distributed uniformly throughout 8.2 Pipet 15 mL of methyl ethyl ketone into the test tube and
the sample, and that mechanical operations may express some place the latter just up to the level of its contents in a hot water
of the oil. or steam bath. Heat the solvent wax mixture, stirring up and
8. Procedure down with the wire stirrer, until a homogeneous solution is
obtained. Exercise care to avoid loss of solvent by prolonged
8.1 Melt a representative portion of the sample, using a boiling.
water bath or oven maintained at 70 to 100°C (158 to 212°F).
As soon as the wax is completely melted, thoroughly mix. NOTE 5—Very high-melting wax samples may not form clear solutions.
Preheat the pipet or equivalent measuring device in order to Stir until the undissolved material is well dispersed as a fine cloud.
prevent the solidification of wax in the tip, and withdraw a 8.2.1 Plunge the test tube into an 800-mL beaker of ice
portion of the sample as soon as possible after the wax has water and continue to stir until the contents are cold. Remove
melted. The mass of wax transferred to the test tube must be the stirrer. Remove the test tube from the ice bath, wipe dry on
1.00 6 0.05 g. Allow the test tube to cool, and weigh to at least the outside with a cloth, and weigh to at least the nearest 0.1 g.
the nearest 1 mg.
NOTE 6—During this operation the loss of solvent through vaporiza-
NOTE 4—The weight of a test tube which is cleaned by means of tions should be less than 1%. The weight of the solvent is therefore
solvents will not vary to a significant extent. Therefore, a tare weight may practically a constant, and after a few samples are weighed, this weight,

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 D 721 – 06
in the evaporation assembly maintained at 35 6 1°C (95 6
2°F), with the air jet centered inside the neck, and the tip 15 6
5 mm above the surface of the liquid. After the solvent has
evaporated, which usually takes less than 30 min, remove the
bottle and stopper, and place them near the balance. Allow to
stand for 10 min and weigh to the nearest 0.1 mg. Repeat the
evaporation procedure, using a 5-min evaporation period
instead of 30 min, until the loss between successive weighings
is not over 0.2 mg.

9. Calculation
9.1 Calculate the amount of oil in the wax as follows:
Oil in wax, weight % 5 ~100 AC/~BD!! – 0.15 (1)

where:
A = weight of oil residue, g,
B = weight of wax sample, g,
C = weight of solvent, g, obtained by subtracting weight
All dimensions are in millimetres of test tube plus wax sample (8.1) from weight of
FIG. 3 Air Pressure Regulator test tube and contents (8.2),
D = weight of solvent evaporated, g, obtained by sub-
tracting weight of weighing bottle plus oil residue
approximately 11.9 g, can be used as a constant factor.
from weight of weighing bottle plus filtrate (8.5),
8.3 Insert the temperature measuring device into the test and
tube and place the test tube containing the wax-solvent slurry 0.15 = average factor correcting for the solubility of wax in
in the cooling bath, which is maintained at –34.5 6 1.0°C the solvent at –32°C (–25°F).
(–30.0 6 2.0°F). During this chilling operation it is important
that stirring by means of the temperature measuring device be 10. Report
almost continuous, in order to maintain a slurry of uniform
consistency as the wax precipitates. Do not allow the wax to set 10.1 Report the result as oil content, Test Method D 721. If
up of the walls of cooling vessel nor permit any lumps of wax the result is negative, report as zero.
crystals to form. Continue stirring until the temperature reaches
–31.7 6 0.3°C (–25.0 6 0.5°F). 11. Precision and Bias
8.4 Remove the temperature measuring device from the 11.1 Precision—The precision of this test method as deter-
tube and allow it to drain momentarily into the tube; then mined by statistical examination of interlaboratory results is as
immediately immerse in the mixture the clean dry filter stick follows:
which has previously been cooled by placing it in a test tube 11.1.1 Repeatability—The difference between two test re-
and holding at –34.5 6 1.0°C (–30.0 6 2.0°F) in the cooling
sults, obtained by the same operator with the same apparatus
bath for a minimum of 10 min. Seat the ground-glass joint of
under constant operating conditions on identical test material,
the filter so as to make an airtight seal. Place an unstoppered
would in the long run, in the normal and correct operation of
weighing bottle, previously weighed together with the glass
the test method, exceed the following values only in one case
stopper to the nearest 0.1 mg, under the delivery nozzle of the
in twenty:
filtration assembly.
0.06 1 8% of the mean
NOTE 7—Take every precaution to ensure the accuracy of the weight of
the stoppered weighing bottle. Prior to determining this weight, rinse the 11.1.2 Reproducibility—The difference between two single
clean, dry weighing bottle and stopper with methyl ethyl ketone, wipe dry and independent results obtained by different operators work-
on the outside with a cloth, and place in the evaporation assembly to dry ing in different laboratories on identical test material would, in
for about 5 min. Then remove the weighing bottle and stopper, place near
the long run, in the normal and correct operation of the test
the balance, and allow to stand for 10 min prior to weighing. Stopper the
bottle during this cooling period. Once the weighing bottle and stopper method, exceed the following values only in one case in
have been dried in the evaporation assembly, lift only with forceps. Take twenty:
care to remove and replace the glass stopper with a light touch. 0.2 1 11% of the mean
8.5 Apply air pressure to the filtration assembly, and imme-
11.2 Bias—The procedure in this test method has no bias
diately collect about 4 mL of filtrate in the weighing bottle.
because the value of oil content can be defined only in terms of
Release the air pressure to permit the liquid to drain back
a test method.
slowly from the delivery nozzle. Remove the weighing bottle
immediately, and stopper and weigh to at least the nearest
12. Keywords
10 mg without waiting for it to come to room temperature.
Unstopper the weighing bottle and place it under one of the jets 12.1 oil content; petroleum wax; wax

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 D 721 – 06

All dimensions are in millimetres (inches)

FIG. 4 Evaporation Assembly

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 D 721 – 06

APPENDIX

(Nonmandatory Information)

X1. TEST METHOD FOR MEASUREMENT OF MAXIMUM PORE DIAMETER OF RIGID POROUS FILTERS

X1.1 Scope
X1.1.1 This test method covers the determination of the
acceptability of porous filter sticks used for filtration in Test
Method D 721. This test method establishes the maximum pore
diameter and also provides a means of detecting and measuring
changes which occur form continued use.
X1.2 Definition
X1.2.1 maximum pore diameter—the diameter in microme-
ters of the largest opening in the filter.
NOTE X1.1—It is recognized that the maximum pore diameter as
defined herein does not necessarily indicate the physical dimensions of the
largest pore in the filter. It is further recognized that the pores are highly
irregular in shape. Because of the irregularity in shape and other
phenomena characteristic of filtration, a filter may be expected to retain all
particles larger than the maximum pore diameter as defined and deter- FIG. X1.1 Assembly of Apparatus for Checking Pore Diameter or
mined herein, and will generally retain particles which are much smaller Filter Sticks
than the determined diameter.

X1.3 Summary of Test Method X1.5.4 Immerse the filter just below the surface of the
X1.3.1 The filter is cleaned and wetted with water. It is then water.
immersed in water and air pressure is applied against its upper NOTE X1.2—If a head of liquid exists above the surface of the filter, the
surface until the first bubble of air passes through the filter. The back pressure produced must be deducted from the observed pressure.
maximum pore diameter is calculated from the surface tension
X1.5.5 Increase the air pressure to about 10 mm Hg (or
of water and the applied pressure.
equivalent pressure value if using different units) below the
X1.4 Apparatus acceptable pressure limit and then at a slow uniform rate
X1.4.1 Pressure Measuring Device, mercury-filled manom- equivalent to about 3 mm Hg/min until the first bubble passes
eter or equivalent, capable of measuring pressures in incre- through the filter. This can be conveniently observed by
ments of 0.5 mm of Hg. placing the beaker or test tube over a mirror. Read the pressure
X1.4.2 Air Supply, clean and filtered. measuring device when the first bubble passes off the underside
X1.4.3 Air Pressure Regulator, needle-valve type. of the filter.
X1.4.4 Drying Oven.
X1.6 Calculation
X1.5 Procedure X1.6.1 Calculate the pore diameter as follows:
X1.5.1 Clean the filter sticks by soaking in concentrated D 5 2180/p
hydrochloric acid, and then wash them with distilled water.
Rinse with acetone, air dry, and place in drying oven at 220°F where:
(105°C) for 30 min. D = pore diameter, µm, and
X1.5.2 Thoroughly wet the clean filter to be tested by p = pressure reading, mm Hg.
soaking it in distilled water. NOTE X1.3—From this equation, pressure corresponding to the upper
X1.5.3 Assemble the apparatus as shown in Fig. X1.1. and lower limits of the specified pore diameters can be calculated. These
Apply pressure slowly from a source of clean air. pressures may be used for acceptance testing.

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 D 721 – 06
SUMMARY OF CHANGES

Subcommittee D02.10 has identified the location of selected changes to this standard since the last issue
(D 721–05) that may impact the use of this standard.

(1) Revised 8.1. (3) Revised 8.3-8.5.

(2) Revised 8.2.1.

Subcommittee D02.10 has identified the location of selected changes to this standard since the last issue
(D 721–04) that may impact the use of this standard.

(1) Corrected Eq 1. (3) Revised 5.2, 5.7, 5.9, 8.3, and 8.4.
(2) Added 5.6.2. Renumbered 5.6 and 5.6.1.

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