ASTM D3235-06(2011)
(Test Method)Standard Test Method for Solvent Extractables in Petroleum Waxes
Standard Test Method for Solvent Extractables in Petroleum Waxes
SIGNIFICANCE AND USE
The solvent extractables in 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 staining characteristics. Whether these effects are desirable or undesirable depends on the intended use of the wax.
SCOPE
1.1 This test method covers the determination of solvent extractables in petroleum waxes.
1.2 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.
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.
General Information
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D3235 − 06(Reapproved 2011)
Standard Test Method for
Solvent Extractables in Petroleum Waxes
This standard is issued under the fixed designation D3235; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope 5. Apparatus
1.1 This test method covers the determination of solvent 5.1 Filter Stick and Assembly, consisting of a 10-mm
extractables in petroleum waxes. diameter sintered glass filter stick of 10 to 15 µm maximum
pore diameter as determined by the method in Appendix X1,
1.2 The values stated in SI units are to be regarded as
provided with an air pressure inlet tube and delivery nozzle. It
standard. The values given in parentheses are for information
isprovidedwithaground-glassjointtofita25by170-mmtest
only.
tube. The dimensions for a suitable filtration assembly are
1.3 This standard does not purport to address all of the
shown in Fig. 1.
safety concerns, if any, associated with its use. It is the
NOTE 1—A metallic filter stick may be employed if desired. A filter
responsibility of the user of this standard to establish appro-
stick made of stainless steel and having a 12.7-mm (0.50-in.) disk of 10
priate safety and health practices and determine the applica-
to 15 nm maximum pore diameter, as determined by Test Method E128,
bility of regulatory limitations prior to use.
has been found to be satisfactory. The metallic apparatus is inserted into
a 25 by 150-mm test tube and held in place by means of a cork.
2. Referenced Documents
5.2 Cooling Bath, consisting of an insulated box with 30 6
2.1 ASTM Standards:
5-mm (1.2 6 0.2-in.) holes in the center to accommodate any
E1Specification for ASTM Liquid-in-Glass Thermometers
desired number of test tubes. The bath may be filled with a
E128Test Method for Maximum Pore Diameter and Perme-
suitable medium such as kerosine, and may be cooled by
ability of Rigid Porous Filters for Laboratory Use
circulatingarefrigerantthroughcoils,orbyusingsolidcarbon
dioxide. A suitable cooling bath to accommodate three test
3. Summary of Test Method
tubes is shown in Fig. 2.
3.1 The sample is dissolved in a mixture consisting of 50
5.3 Dropper Pipet, dispensing device capable of delivering
volume% methyl ethyl ketone and 50 volume% toluene. The
0.5 6 0.05 g of molten wax.
solution is cooled to −32°C (−25°F) to precipitate the wax,
5.4 Transfer Pipet, or equivalent volume dispensing device,
thenfiltered.Thesolventextractablescontentisdeterminedby
capable of delivering 15 6 0.06 mL.
evaporating the solvent from the filtrate and weighing the
residue. 5.5 Air Pressure Regulator, designed to supply air to the
filtration assembly (8.5) at sufficient pressure to give an even
4. Significance and Use
flow of filtrate. Either a conventional pressure-reducing valve
or a mercury bubbler-type regulator has been found satisfac-
4.1 The solvent extractables in a wax may have significant
tory.The latter type, illustrated in Fig. 3, consists of a 250-mL
effects on several of its properties such as strength, hardness,
glass cylinder and a T-tube held in the cylinder by means of a
flexibility,scuffresistance,coefficientoffriction,coefficientof
rubber stopper grooved at the sides to permit the escape of
expansion,meltingpoint,andstainingcharacteristics.Whether
excess air. The volume and pressure of the air supplied to the
these effects are desirable or undesirable depends on the
filtrationassemblyisregulatedbythedepthtowhichtheT-tube
intended use of the wax.
is immersed in mercury at the bottom of the cylinder. Absor-
bentcottonplacedinthespaceabovethemercurypreventsthe
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.10.0A on Physical/Chemical Properties.
Current edition approved Oct. 1, 2011. Published October 2011. Originally The sole source of supply of a suitable metal filter stick with designated
approved in 1973. Last previous edition approved in 2006 as D3235-06. DOI: porosity G known to the committee at this time is the Pall Trinity Micro Corp.,
10.1520/D3235-06R11. Route281,Cortland,NY13045.AlistofUnitedKingdomsupplierscanbeobtained
For referenced ASTM standards, visit the ASTM website, www.astm.org, or from Energy Institute, 61 New Cavendish St., London, W1G7AR, United King-
contact ASTM Customer Service at service@astm.org. 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, which you may attend.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3235 − 06 (2011)
All dimensions are in millimetres.
FIG. 1 Filter Stick
loss of mercury by spattering. The air pressure regulator is Periodically check the cleanliness of the air by evaporating 4
connected to the filter stick and assembly by means of rubber mL of the solvent mixture described in 6.3 by the procedure
tubing. specified in 8.5.When the residue does not exceed 0.1 mg, the
evaporation equipment is operating satisfactorily.
5.6 Temperature Measuring Devices:
5.6.1 Thermometers, two, having a range as shown below
NOTE 2—Investigations by the European World Federation have indi-
catedthatimprovedprecisionmaybeachievedbyindividuallycalibrating
and conforming to the requirements as prescribed in Specifi-
each nozzle to deliver a flow rate of 2 to 3 L/min.
cation E1 or in the specifications for IP Standard Thermom-
eters. One thermometer is required for the cold bath and a 5.9 Analytical Balance, capable of reproducing weights to
second thermometer is required for the sample solution. 0.1 mg.
Thermometer Number
5.10 Wire Stirrer—A piece of stiff made of iron, stainless
Temperature Range ASTM IP
steel, or Nichrome wire of about No. 20 Bands (0.9 mm in
−37 to +21°C 71C 72C
diameter) or 16 swg. gage, 250 mm long. A 10-mm diameter
−35 to +70°F 71F 72F
loop is formed at each end, and the loop at the bottom end is
5.6.2 Temperature measuring devices other than those de-
bent so that the plane of the loop is perpendicular to the wire.
scribed in 5.6.1 are satisfactory for this test method, provided
they exhibit the same temperature response as the equivalent
6. Solvent
mercury-in-glass thermometers.
6.1 Methyl Ethyl Ketone,conformingtothespecificationsof
5.7 Weighing Bottles, glass-stoppered, having a typical ca-
theCommitteeonAnalyticalReagentsoftheAmericanChemi-
pacity of 15-25 mL.
cal Society.
5.8 Evaporation Assembly, consisting of an evaporating
6.2 Toluene, conforming to the specifications of the Com-
cabinetandconnections,essentiallyasillustratedinFig.4,and
mittee on Analytical Reagents of the American Chemical
capable of maintaining a temperature of 35 6 1°C (95 6 2°F)
Society.
aroundtheevaporationflasks.Constructthejetswithaninside
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
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For Suggestions on the testing of reagents not
at the start of the evaporation. Supply purified air at the rate of
listed by the American Chemical Society, see Annual Standards for Laboratory
2 to 3 L/min per jet. One way to purify the air is to pass it
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
through a tube of approximately 1-cm bore packed loosely to
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
a height of approximately 20 cm with absorbent cotton. MD.
D3235 − 06 (2011)
All dimensions are in millimetres (inches).
FIG. 2 Cooling Bath
6.3 Solvent Mixture—Prepare a mixture of 50 volume% melted. The mass of wax transferred to the test tube must be
methyl ethyl ketone and 50 volume% toluene. 1.00 60.05g.Allowthetesttubetocool,andweightoatleast
the nearest 1 mg.
6.4 Store the solvent mixture over anhydrous calcium sul-
fate (5 weight% of the solvent). Filter prior to use. NOTE3—Theweightofatesttubewhichiscleanedbymeansofsolvent
will not vary to a significant extent. Therefore, a tare weight may be
obtained and used repeatedly.
7. Sample
8.2 Pipet15mLofthesolventmixtureintothetesttubeand
7.1 Obtain a representative portion by melting the entire
placethelatterjustuptothelevelofitscontentsinahotwater
sample and stirring thoroughly. This is necessary because the
or steam bath. Heat the solvent-wax mixture, stirring up and
extractables may not be distributed uniformly throughout the
down with the wire stirrer, until a homogeneous solution is
solidified sample.
obtained. Exercise care to avoid loss of solvent by prolonged
8. Procedure boiling.
NOTE4—Veryhigh-meltingwaxsamplesmaynotformclearsolutions.
8.1 Melt a representative portion of the sample, using a
Stir until the undissolved material is well dispersed as a fine cloud.
water bath or oven maintained at 70 to 100°C (158 to 212°F).
As soon as the wax is completely melted, thoroughly mix. 8.2.1 Plunge the test tube into an 800-mL beaker of ice
Preheat the pipet or equival
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