An American National Standard

Designation: D 3235 – 06

Standard Test Method for

Solvent Extractables in Petroleum Waxes1
This standard is issued under the fixed designation D 3235; 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 (e) indicates an editorial change since the last revision or reapproval.

1. Scope* these effects are desirable or undesirable depends on the

1.1 This test method covers the determination of solvent intended use of the wax.
extractables in petroleum waxes. 5. Apparatus
1.2 The values stated in SI units are to be regarded as the
standard. The values given in parentheses are for information 5.1 Filter Stick and Assembly, consisting of a 10-mm
only. diameter sintered glass filter stick of 10 to 15 µm maximum
1.3 This standard does not purport to address all of the pore diameter as determined by the method in Appendix X1,
safety concerns, if any, associated with its use. It is the provided with an air pressure inlet tube and delivery nozzle. It
responsibility of the user of this standard to establish appro- is provided with a ground-glass joint to fit a 25 by 170-mm test
priate safety and health practices and determine the applica- tube. The dimensions for a suitable filtration assembly are
bility of regulatory limitations prior to use. shown in Fig. 1.
NOTE 1—A metallic filter stick may be employed if desired. A filter
2. Referenced Documents stick3 made of stainless steel and having a 12.7-mm (0.50-in.) disk of 10
2.1 ASTM Standards: 2 to 15 nm maximum pore diameter, as determined by Test Method E 128,
E 1 Specification for ASTM Liquid-in-Glass Thermometers has been found to be satisfactory. The metallic apparatus is inserted into
E 128 Test Method for Maximum Pore Diameter and Per- a 25 by 150-mm test tube and held in place by means of a cork.
meability of Rigid Porous Filters for Laboratory Use 5.2 Cooling Bath, consisting of an insulated box with 30 6
5-mm (1.2 6 0.2-in.) holes in the center to accommodate any
3. Summary of Test Method desired number of test tubes. The bath may be filled with a
3.1 The sample is dissolved in a mixture consisting of 50 suitable medium such as kerosine, and may be cooled by
volume % methyl ethyl ketone and 50 volume % toluene. The circulating a refrigerant through coils, or by using solid carbon
solution is cooled to −32°C (−25°F) to precipitate the wax, dioxide. A suitable cooling bath to accommodate three test
then filtered. The solvent extractables content is determined by tubes is shown in Fig. 2.
evaporating the solvent from the filtrate and weighing the 5.3 Dropper Pipet, dispensing device capable of delivering
residue. 0.5 6 0.05 g of molten wax.
5.4 Transfer Pipet, or equivalent volume dispensing device,
4. Significance and Use capable of delivering 15 6 0.06 mL.
4.1 The solvent extractables in a wax may have significant 5.5 Air Pressure Regulator, designed to supply air to the
effects on several of its properties such as strength, hardness, filtration assembly (8.5) at sufficient pressure to give an even
flexibility, scuff resistance, coefficient of friction, coefficient of flow of filtrate. Either a conventional pressure-reducing valve
expansion, melting point, and staining characteristics. Whether or a mercury bubbler-type regulator has been found satisfac-
tory. The latter type, illustrated in Fig. 3, consists of a 250-mL
glass cylinder and a T-tube held in the cylinder by means of a
1
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
3
D02.10.0A on Physical/Chemical Properties. The sole source of supply of a suitable metal filter stick with designated
Current edition approved Nov. 1, 2006. Published November 2006. Originally porosity G known to the committee at this time is the Pall Trinity Micro Corp.,
approved in 1973. Last previous edition approved in 2005 as D 3235–05. Route 281, Cortland, NY 13045. A list of United Kingdom suppliers can be obtained
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or from Energy Institute, 61 New Cavendish St., London, W1G 7AR, United King-
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM dom. If you are aware of alternative suppliers, please provide this information to
Standards volume information, refer to the standard’s Document Summary page on ASTM International Headquarters. Your comments will receive careful consider-
the ASTM website. ation at a meeting of the responsible technical committee,1 which you may attend.

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

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

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 D 3235 – 06

All dimensions are in millimetres.

FIG. 1 Filter Stick

rubber stopper grooved at the sides to permit the escape of 2 to 3 L/min per jet. One way to purify the air is to pass it
excess air. The volume and pressure of the air supplied to the through a tube of approximately 1-cm bore packed loosely to
filtration assembly is regulated by the depth to which the T-tube a height of approximately 20 cm with absorbent cotton.
is immersed in mercury at the bottom of the cylinder. Absor- Periodically check the cleanliness of the air by evaporating 4
bent cotton placed in the space above the mercury prevents the mL of the solvent mixture described in 6.3 by the procedure
loss of mercury by spattering. The air pressure regulator is specified in 8.5. When the residue does not exceed 0.1 mg, the
connected to the filter stick and assembly by means of rubber evaporation equipment is operating satisfactorily.
tubing. NOTE 2—Investigations by the European World Federation have indi-
5.6 Temperature Measuring Devices: cated that improved precision may be achieved by individually calibrating
5.6.1 Thermometers, two, having a range as shown below each nozzle to deliver a flow rate of 2 to 3 L/min.
and conforming to the requirements as prescribed in Specifi-
5.9 Analytical Balance, capable of reproducing weights to
cation E 1 or in the specifications for IP Standard Thermom-
0.1 mg.
eters. One thermometer is required for the cold bath and a
5.10 Wire Stirrer—A piece of stiff made of iron, stainless
second thermometer is required for the sample solution.
steel, or Nichrome wire of about No. 20 Bands (0.9 mm in
Thermometer Number
Temperature Range ASTM IP
diameter) or 16 swg. gage, 250 mm long. A 10-mm diameter
−37 to +21°C 71C 72C loop is formed at each end, and the loop at the bottom end is
−35 to +70°F 71F 72F bent so that the plane of the loop is perpendicular to the wire.
5.6.2 Temperature measuring devices other than those de- 6. Solvent
scribed in 5.6.1 are satisfactory for this test method, provided
they exhibit the same temperature response as the equivalent 6.1 Methyl Ethyl Ketone, conforming to the specifications of
mercury-in-glass thermometers. the Committee on Analytical Reagents of the American Chemi-
5.7 Weighing Bottles, glass-stoppered, having a typical ca- cal Society.4
pacity of 15-25 mL. 6.2 Toluene, conforming to the specifications of the Com-
5.8 Evaporation Assembly, consisting of an evaporating mittee on Analytical Reagents of the American Chemical
cabinet and connections, essentially as illustrated in Fig. 4, and Society.4
capable of maintaining a temperature of 35 6 1°C (95 6 2°F)
around the evaporation flasks. Construct the jets with an inside 4
Reagent Chemicals, American Chemical Society Specifications, American
diameter of 4 6 0.2 mm for delivering a stream of clean, dry Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
air vertically downward into the weighing bottle. Support each
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
jet so that the tip is 15 6 5 mm above the surface of the liquid and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
at the start of the evaporation. Supply purified air at the rate of MD.

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 D 3235 – 06

All dimensions are in millimetres (inches).

FIG. 2 Cooling Bath

6.3 Solvent Mixture—Prepare a mixture of 50 volume % portion of the sample as soon as possible after the wax has
methyl ethyl ketone and 50 volume % toluene. melted. The mass of wax transferred to the test tube must be
6.4 Store the solvent mixture over anhydrous calcium sul- 1.00 6 0.05 g. Allow the test tube to cool, and weigh to at least
fate (5 weight % of the solvent). Filter prior to use. the nearest 1 mg.
7. Sample NOTE 3—The weight of a test tube which is cleaned by means of
solvent will not vary to a significant extent. Therefore, a tare weight may
7.1 Obtain a representative portion by melting the entire
be obtained and used repeatedly.
sample and stirring thoroughly. This is necessary because the
extractables may not be distributed uniformly throughout the 8.2 Pipet 15 mL of the solvent mixture into the test tube and
solidified sample. 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
8. Procedure down with the wire stirrer, until a homogeneous solution is
8.1 Melt a representative portion of the sample, using a obtained. Exercise care to avoid loss of solvent by prolonged
water bath or oven maintained at 70 to 100°C (158 to 212°F). boiling.
As soon as the wax is completely melted, thoroughly mix.
Preheat the pipet or equivalent measuring device in order to NOTE 4—Very high-melting wax samples may not form clear solutions.
prevent the solidification of wax in the tip, and withdraw a Stir until the undissolved material is well dispersed as a fine cloud.

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 D 3235 – 06
lift only with forceps. Take care to remove and replace the glass stopper
with a light touch.
8.5 Apply air pressure to the filtration assembly and imme-
diately collect about 4 mL of filtrate in the weighing bottle.
Release the air pressure to permit the liquid to drain back
slowly from the delivery nozzle. Remove the weighing bottle
immediately, and stopper and weigh to at least the nearest 10
mg without waiting for it to come to room temperature.
Unstopper the weighing bottle and place it under one of the jets
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, stopper, and place near the balance. Allow to stand for
10 min and weigh to the nearest 0.1 mg. Repeat the evaporation
procedure, using 5 min evaporation periods, until the loss
between successive weighings is not over 0.2 mg.

All dimensions are in millimetres.

9. Calculation
FIG. 3 Air Pressure Regulator 9.1 Calculate the amount of extractables in the wax as
follows:
Solvent extractables, weight % 5 100 AC/BD (1)
8.2.1 Plunge the test tube into an 800-mL beaker of ice
water and continue to stir until the contents are cold. Remove where:
the stirrer. Remove the test tube from the ice bath, wipe dry on A = weight of extractables residue, g,
the outside with a cloth, and weigh to at least the nearest 0.1 g. B = weight of wax sample, g,
C = weight of solvent, g, obtained by subtracting weight of
NOTE 5—During this operation the loss of solvent through vaporization
should be less than 1 %. The weight of the solvent is, therefore, practically
test tube plus wax sample (8.1) from weight of test
a constant, and after a few samples are weighed, this weight can be used tube and contents (8.2), and
as a constant factor. D = weight of solvent evaporated, in g, obtained by sub-
tracting weight of weighing bottle plus extractables
8.3 Place the test tube containing the wax-solvent slurry in
residue from weight of weighing bottle plus filtrate
the cooling bath, which is maintained at −34.5 6 1.0°C (−30.0
(8.5).
6 2.0°F). During this chilling operation, stir the contents of the
tube by means of a temperature measurement device placed in 10. Report
the tube. It is important that stirring by means of the tempera-
ture measurement device be almost continuous, in order to 10.1 Report the result as solvent extractables, weight %,
maintain a slurry of uniform consistency as the wax precipi- Test Method D 3235. If the result is negative, report as zero.
tates. Do not allow the wax to set up on the walls of the cooling
11. Precision and Bias
vessel nor permit any lumps of wax crystals to form. Continue
stirring until the temperature reaches −31.7 6 0.3°C (−25.0 6 11.1 The precision of this test method as determined by
0.5°F). statistical examination of interlaboratory results is as follows:
8.4 Remove the temperature measurement device from the 11.1.1 Repeatability—The difference between two test re-
tube and allow it to drain momentarily into the tube, then sults, obtained by the same operator with the same apparatus
immediately immerse in the mixture the clean, dry filter stick, under constant operating conditions on identical test material
which has previously been cooled by placing it in a test tube would, in the long run, in the normal and correct operation of
and holding at −34.5 6 1.0°C (−30.0 6 2.0°F) in the cooling the test method, exceed the following values only in one case
bath for a minimum of 10 min. Seat the ground-glass joint of in twenty:
the filter so as to make an airtight seal. Place an unstoppered Range Repeatability
weighing bottle, previously weighed together with the glass 15 to 55 % 2%
stopper to the nearest 0.1 mg, under the delivery nozzle of the
filtration assembly. 11.1.2 Reproducibility—The difference between two single
and independent results obtained by different operators work-
NOTE 6—Take every precaution to ensure the accuracy of the weight of ing in different laboratories on identical test material would, in
the stoppered weighing bottle. Prior to determining this weight, rinse the
the long run, in the normal and correct operation of the test
clean, dry weighing bottle and stopper with the solvent mixture described
in 6.3, wipe dry on the outside with a cloth, and place in the evaporation method, exceed the following values only in one case in
assembly to dry for about 5 min. Then remove the weighing bottle and twenty:
stopper, place near the balance, and allow to stand for 10 min prior to Range Reproducibility
weighing. Stopper the bottle during this cooling period. Once the
weighing bottle and stopper have been dried in the evaporation assembly, 15 to 55 % 5%

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 D 3235 – 06

All dimensions are in millimetres (inches).

FIG. 4 Evaporation Assembly

11.2 The procedure in this test method has no bias because 12. Keywords
the value of solvent extractables can be defined only in terms
12.1 petroleum waxes; solvent extractables; wax
of a test method.

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 D 3235 – 06
APPENDIX

(Nonmandatory Information)

X1. TEST METHOD OF TEST FOR MEASUREMENT OF MAXIMUM PORE DIAMETER

OF RIGID POROUS FILTERS

X1.1 Scope X1.5.3 Assemble the apparatus as shown in Fig. X1.1.

X1.1.1 This test method covers the determination of the Apply pressure slowly from a source of clean air.
acceptability of porous filter sticks used for filtration in Test X1.5.4 Immerse the filter just below the surface of the
Method D 3235. This method establishes the maximum pore water.
diameter and also provides a means of detecting and measuring NOTE X1.1—If a head of liquid exists above the surface of the filter, the
changes which occur from continued use. back pressure produced must be deducted from the observed pressure.

X1.2. Terminology X1.5.5 Increase the air pressure to about 10 mm Hg (or

equivalent pressure value if using different units) below the
X1.2.1 Definitions: acceptable pressure limit and then at a slow uniform rate
X1.2.1.1 maximum pore diameter—the diameter in na- equivalent to about 3 mm Hg/min until the first bubble passes
nometres of the largest opening in the filter. through the filter. This can be conveniently observed by
Discussion—It is recognized that the maximum pore diam- placing the beaker or test tube over a mirror. Read the pressure
eter as defined herein does not necessarily indicate the physical measuring device when the first bubble passes off the underside
dimensions of the largest pore in the filter. It is further of the filter.
recognized that the pores are highly irregular in shape. Because
of the irregularity in shape and other phenomena characteristic X1.6 Calculation
of filtration, a filter may be expected to retain all particles X1.6.1 Calculate the pore diameter as follows:
larger than the maximum pore diameter as defined and deter-
D 5 2180/p (X1.1)
mined herein, and will generally retain particles which are
much smaller than the determined diameter. where:
D = pore diameter, nm, and
X1.3 Summary of Test Method p = pressure reading, mm Hg.
X1.3.1 The filter is cleaned and wetted with water. It is then
NOTE X1.2—From this equation, pressure corresponding to the upper
immersed in water and air pressure is applied against its upper
and lower limits of the specified pore diameters can be calculated. These
surface until the first bubble of air passes through the filter. The pressures may be used for acceptance testing.
maximum pore diameter is calculated from the surface tension
of water and the applied pressure.
X1.4 Apparatus
X1.4.1 Pressure Measuring Device, mercury filled manom-
eter or equivalent, capable of measuring pressures in incre-
ments of 0.5 mm of Hg.
X1.4.2 Air Supply, clean and filtered.
X1.4.3 Air Pressure Regulator, needle-valve type.
X1.4.4 Drying Oven.
X1.5 Procedure
X1.5.1 Clean the filter sticks by soaking in concentrated
hydrochloric acid, and then wash them with distilled water.
Rinse with acetone, air dry, and place in drying oven at 220°F
(105°C) for 30 min.
X1.5.2 Thoroughly wet the clean filter to be tested by FIG. X1.1 Assembly of Apparatus for Checking Pore Diameter or
soaking it in distilled water. Filter Sticks

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 D 3235 – 06
SUMMARY OF CHANGES

Subcommittee D02.10.0A has identified the location of selected changes to this standard since the last issue
(D 3235–05) that may impact the use of this standard. (Approved Nov. 1, 2006.)

(1) Revised 8.1. (4) Revised 8.4.

(2) Revised 8.2.1. (5) Revised 8.5.
(3) Revised 8.3.

Subcommittee D02.10.0A has identified the location of selected changes to this standard since the last issue
(D 3235–04) that may impact the use of this standard. (Approved Nov. 1, 2005.)

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

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