ASTM D4055-04(2009)
(Test Method)Standard Test Method for Pentane Insolubles by Membrane Filtration
Standard Test Method for Pentane Insolubles by Membrane Filtration
SIGNIFICANCE AND USE
Pentane insolubles above 0.8 μm in size may lead to increased wear. This increased wear can lead to premature equipment failure in critical applications.
SCOPE
1.1 This test method covers the determination of pentane insolubles for particles exceeding 0.8 μm in new and used lubricating oils.
Note 1—Pentane insolubles with particle sizes less than 0.8 μm may be studied with appropriate size membrane filters. Particle sizes above or below 0.8 μm can be studied. The precision of this test method has been determined only at 0.8 μm.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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. For specific warning statements, see 7.1, 8.2.1, and Annex A1.
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Designation: D4055 − 04(Reapproved 2009)
Standard Test Method for
Pentane Insolubles by Membrane Filtration
This standard is issued under the fixed designation D4055; 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.
1. Scope 3.1.2 used oil, n—any oil that has been in a piece of
equipment (for example, an engine, gearbox, transformer, or
1.1 This test method covers the determination of pentane
turbine) whether operated or not. D4175
insolubles for particles exceeding 0.8 µm in new and used
lubricating oils.
4. Summary of Test Method
NOTE 1—Pentane insolubles with particle sizes less than 0.8 µm may be
4.1 A sample of new or used lubricating oil is mixed with
studied with appropriate size membrane filters. Particle sizes above or
pentane in a volumetric flask. The oil solution is filtered
below 0.8 µm can be studied. The precision of this test method has been
through an 0.8-µm membrane filter.The flask, funnel, and filter
determined only at 0.8 µm.
are washed with additional pentane to effect a complete
1.2 The values stated in SI units are to be regarded as
transfer of particulates onto the filter. The filter and its
standard. No other units of measurement are included in this
particulates are dried and weighed to give the pentane in-
standard.
solubles.
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
5. Significance and Use
responsibility of the user of this standard to establish appro-
5.1 Pentane insolubles above 0.8 µm in size may lead to
priate safety and health practices and determine the applica-
increased wear. This increased wear can lead to premature
bilityofregulatorylimitationspriortouse.FOR SPECIFIC WARNING
equipment failure in critical applications.
STATEMENTS, SEE 7.1, 8.2.1, AND ANNEX A1.
6. Apparatus
2. Referenced Documents
6.1 In the development of this test method, it was noted that
2.1 ASTM Standards:
variations, particularly with respect to glassware and filter
D4057 Practice for Manual Sampling of Petroleum and
media, can affect the test result significantly.
Petroleum Products
6.2 When the user of this test method uses an alternate
D4175 Terminology Relating to Petroleum, Petroleum
membrane filter, it is incumbent upon them to establish that the
Products, and Lubricants
alternate filter will give equal results.
D4177 Practice for Automatic Sampling of Petroleum and
Petroleum Products
6.3 Precision data were established using the apparatus
listed and a 0.8 µm filter pore size.
3. Terminology
6.4 Membrane Filter.
3.1 Definitions:
6.5 Borosilicate Filter Holder.
3.1.1 pentane insolubles, in used oil analysis, n—separated
matter resulting when a used oil is dissolved in pentane.
6.6 Borosilicate Filtering Flask.
3.1.1.1 Discussion—In this test method, the separation is
6.7 Forceps (plain flat tips, not serrated),
effected by filtration through a membrane.
6.8 Wash Bottle equipped with 0.8-µm membranes.
1 3
This test method is under the jurisdiction of ASTM Committee D02 on Millipore AAWP04700, available from Millipore Corp, Bedford MA, 01273,
Petroleum Products and Lubricantsand is the direct responsibility of Subcommittee has been found to be satisfactory; also an equivalent may be used.
D02.06 on Analysis of Lubricants. Millipore XX1004700, available from Millipore Corp, Bedford MA, 01273,
Current edition approved April 15, 2009. Published July 2009. Originally has been found to be satisfactory; also an equivalent may be used.
approved in 1992. Last previous edition approved in 2004 as D4055–04. DOI: Millipore XX1004705, available from Millipore Corp, Bedford MA, 01273,
10.1520/D4055-04R09. has been found to be satisfactory; also an equivalent may be used.
2 6
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Millipore XX6200006, available from Millipore Corp, Bedford MA, 01273,
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM has been found to be satisfactory; also an equivalent may be used.
Standards volume information, refer to the standard’s Document Summary page on Millipore XX6602500, available from Millipore Corp, Bedford MA, 01273,
the ASTM website. has been found to be satisfactory; also an equivalent may be used.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4055 − 04 (2009)
6.9 Analytical Balance, capable of weighing with an accu- desiccator containing calcium chloride or some other material
racy of 60.1 mg. that will assure an atmosphere free of moisture and hydrocar-
bon vapors.
6.10 Vacuum Source, capable of maintaining a vacuum of
8.2.3 When the membranes have reached equilibrium
255 6 50 mm Hg.
(about 30 min), weigh the membrane to the nearest 0.1 mg.
6.11 Oven, capable of maintaining 90 6 5°C.
8.2.4 Store the aluminum dish in the desiccator until ready
for use.
6.12 Oven Thermometer, ASTM Thermometer 1C.
6.13 Aluminum Foil Weighing Dish , about 60 mm in 8.3 Filtration:
8.3.1 Remove the membrane filter from the weighing dish
diameter.
with the flat forceps and center in the filtering apparatus.
6.14 Desiccator, with calcium chloride.
Assemble the funnel and clamp.
6.15 Mechanical Paint Shaker, three-dimensional.
8.3.2 Fill the volumetric flask containing the sample to the
100-mL mark with filtered pentane. Stopper and shake well.
6.16 Volumetric Flask, 100-mL with ground-glass or TFE-
Immediatelyfilterthemixtureusingavacuumof255 650mm
fluorocarbon stopper.
Hg (see 8.1.3.1). Rinse the flask and stopper twice with small
6.17 Ionizing Unit , insert under or next to balance pan.
amounts of filtered pentane, pouring the washings down the
sides of the filter funnel. Rinse the walls of the filter funnel
7. Reagen
...
This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
An American National Standard Designation: D 4055 – 04 (Reapproved 2009)
Designation:D4055–02
Standard Test Method for
Pentane Insolubles by Membrane Filtration
This standard is issued under the fixed designation D 4055; 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.
1. Scope *
1.1 This test method covers the determination of pentane insolubles for particles exceeding 0.8 µm in new and used lubricating
oils.
NOTE 1—Pentane insolubles with particle sizes less than 0.8-µm 0.8 µm may be studied with appropriate size membrane filters. Particle sizes above
or below 0.8 µm can be studied. The precision of this test method has been determined only at 0.8 µm.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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. For specific hazardswarning statements, see 7.1, 8.2.1, and Annex A1.
2. Referenced Documents
2.1 ASTM Standards:
D 4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D 4175 Terminology Relating to Petroleum, Petroleum Products, and Lubricants
D 4177 Practice for Automatic Sampling of Petroleum and Petroleum Products
3. Terminology
3.1 Definitions:
3.1.1 pentane insolubles, in used oil analysis, n—separated matter resulting when a used oil is dissolved in pentane.
3.1.1.1 Discussion—In this test method, the separation is effected by filtration through a membrane.
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.06 on
Analysis of Lubricants.
Current edition approved Dec. 10, 2002. Published March 2003. Originally approved in 1992. Last previous edition approved in 2001 as D4055–01.on Analysis of
Lubricants.
Current edition approved April 15, 2009. Published July 2009. Originally approved in 1992. Last previous edition approved in 2004 as D 4055–04.
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
, Vol 05.02.volume information, refer to the standard’s Document Summary page on the ASTM website.
*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.
D 4055 – 04 (2009)
3.1.2 used oil, n—any oil that has been in a piece of equipment (for example, an engine, gearbox, transformer, or turbine)
whether operated or not. D4175
4. Summary of Test Method
4.1 Asample of new or used lubricating oil is mixed with pentane in a volumetric flask. The oil solution is filtered through an
0.8-µmmembranefilter.Theflask,funnel,andfilterarewashedwithadditionalpentanetoeffectacompletetransferofparticulates
onto the filter. The filter and its particulates are dried and weighed to give the pentane insolubles.
5. Significance and Use
5.1 Pentane insolubles above 0.8 µm in size may lead to increased wear. This increased wear can lead to premature equipment
failure in critical applications.
6. Apparatus
6.1 In the development of this test method, it was noted that variations, particularly with respect to glassware and filter media,
can affect the test result significantly.
6.2 When the user of this test method uses an alternate membrane filter, it is incumbent upon them to establish that the alternate
filter will give equal results.
6.3 Precision data were established using the apparatus listed and a 0.8 µm filter pore size.
6.4 Membrane Filter.
6.5 Borosilicate Filter Holder.
6.6 Borosilicate Filtering Flask.
6.7 Forceps (plain flat tips–not serrated), (plain flat tips, not serrated),
6.8 Wash Bottle equipped with 0.8-µm membranes.
6.9 Analytical Balance, capable of weighing with an accuracy of 60.1 mg.
6.10 Vacuum Source, capable of maintaining a vacuum of 255 6 50 mm Hg.
6.11 Oven, capable of maintaining 90 6 5°C.
6.12 Oven Thermometer—ASTM Thermometer 1C. , ASTM Thermometer 1C.
6.13 Aluminum Foil Weighing Dish , about 60 mm in diameter.
6.14 Desiccator, with calcium chloride.
6.15 Mechanical Paint Shaker, three-dimensional.
6.16 Volumetric Flask, 100-mL with ground-glass or TFE-fluorocarbon stopper.
6.17 Ionizing Unit —Insert, insert under or next to balance pan.
7. Reagent
7.1 Pentane, reagent grade or better. ( Warning—Extremely flammable. Vapors can cause flash fire. See A1.1.)
8. Procedure
8.1 Using either Practice D 4057 (manual sampling) or Practice D 4177 (automatic sampling), obtain a representative sample
of the material to be tested.
8.1.1 Preparation of Sample and Materials :
8.1.2 Warm the oil in the original container, if possible, to 60 6 5°C. Shake for a minimum of 30 min on the mechanical shaker
to resuspend the insolubles uniformly.
NOTE 2—Deviation from this sample preparation will normally result in poor precision. Correct sample size is particularly important.
8.1.3Weigh8.1.3 Weigh1gofa representative sample of the oil into a 100-mL volumetric flask to the nearest 0.01 g.
8.1.3.1 Certain oils may require smaller size samples to prevent plugging the membrane. When the 100 mLof the mixture has
not passed through the membrane after 2 min, discard the test and repeat with a smaller sample size (610 %) in the order listed:
0.80 0.33 0.13 0.05
0.64 0.26 0.11 0.04
0.51 0.21 0.09 0.03
0.41 0.17 0.07 0.02
8.1.4 Filter pentane through an 0.8-µm filter.
Millipore AAWP04700, available from Millipore Corp, Bedford MA, 01273, has been found to be satisfactory; also an equivalent may be used.
Millipore XX1004700, available from Millipore Corp, Bedford MA, 01273, has been found to be satisfactory; also an equivalent may be used.
Millipore XX1004705, availab
...
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