ASTM D4055-97
(Test Method)Standard Test Method for Pentane Insolubles by Membrane Filtration
Standard Test Method for Pentane Insolubles by Membrane Filtration
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 the 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 hazards statements, see 7.1, 8.2.1, and Annex A1.
General Information
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 4055 – 97 An American National Standard
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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope through an 0.8-μm membrane filter. The flask, funnel, and filter
are washed with additional pentane to effect a complete
1.1 This test method covers the determination of pentane
transfer of particulates onto the filter. The filter and its
insolubles for particles exceeding 0.8 μm in new and used
particulates are dried and weighed to give the pentane in-
lubricating oils.
solubles.
NOTE 1—Pentane insolubles with particle sizes less than 0.8-μm may be
studied with appropriate size membrane filters. Particle sizes above or
5. Significance and Use
below 0.8 μm can be studied. The precision of this test method has been
5.1 Pentane insolubles above 0.8 μm in size may lead to
determined only at 0.8 μm.
increased wear. This increased wear can lead to premature
1.2 The values stated in SI units are to be regarded as the
equipment failure in critical applications.
standard.
1.3 This standard does not purport to address all of the 6. Apparatus
safety concerns, if any, associated with its use. It is the
6.1 In the development of this test method, it was noted that
responsibility of the user of this standard to establish appro-
variations, particularly with respect to glassware and filter
priate safety and health practices and determine the applica-
media, can affect the test result significantly.
bility of regulatory limitations prior to use.
6.2 When the user of this test method uses an alternate
membrane filter, it is incumbent upon them to establish that the
2. Referenced Documents
alternate filter will give equal results.
2.1 ASTM Standards:
6.3 Precision data were established using the apparatus
D 4057 Practice for Manual Sampling of Petroleum and
listed and a 0.8 μm filter pore size.
Petroleum Products 3
6.4 Membrane Filter.
D 4175 Terminology Relating to Petroleum, Petroleum 4
6.5 Borosilicate Filter Holder.
Products, and Lubricants 5
6.6 Borosilicate Filtering Flask.
D 4177 Practice for Automatic Sampling of Petroleum and 6
6.7 Forceps (plain flat tips–not serrated),
Petroleum Products 7
6.8 Wash Bottle equipped with 0.8-μm membranes.
6.9 Analytical Balance, capable of weighing with an accu-
3. Terminology
racy of 60.1 mg.
3.1 Definitions:
6.10 Vacuum Source, capable of maintaining a vacuum of
3.1.1 pentane insolubles, in used oil analysis, n—separated
255 6 50 mm Hg.
matter resulting when a used oil is dissolved in pentane.
6.11 Oven, capable of maintaining 90 6 5°C.
3.1.1.1 Discussion—In this method, the separation is ef-
6.12 Oven Thermometer—ASTM Thermometer 1C.
fected by filtration through a membrane.
6.13 Aluminum Foil Weighing Dish, about 60 mm in diam-
3.1.2 used oil, n—any oil that has been in a piece of
eter.
equipment (for example, an engine, gearbox, transformer, or
6.14 Desiccator, with calcium chloride.
turbine) whether operated or not.
6.15 Mechanical Paint Shaker, three-dimensional.
D 4175
4. Summary of Test Method
Millipore AAWP04700, available from Millipore Corp, Bedford MA, 01273,
4.1 A sample of new or used lubricating oil is mixed with
has been found to be satisfactory; also an equivalent may be used.
pentane in a volumetric flask. The oil solution is filtered
Millipore XX1004700, available from Millipore Corp, Bedford MA, 01273,
has been found to be satisfactory; also an equivalent may be used.
Millipore XX1004705, available from Millipore Corp, Bedford MA, 01273,
has been found to be satisfactory; also an equivalent may be used.
This test method is under the jurisdiction of ASTM Committee D-2 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee Millipore XX6200006, available from Millipore Corp, Bedford MA, 01273,
D02.06 on Analysis of Lubricants. has been found to be satisfactory; also an equivalent may be used.
Current edition approved Dec. 10, 1997. Published February 1998. Originally Millipore XX6602500, available from Millipore Corp, Bedford MA, 01273,
published as D 4055 – 92. Last previous edition D 4055 – 92. has been found to be satisfactory; also an equivalent may be used.
2 8
Annual Book of ASTM Standards, Vol 05.02. Important—Red Devil 5400 or an equivalent is preferred.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 4055
6.16 Volumetric Flask, 100-mL with ground-glass or TFE- 8.3 Filtration:
fluorocarbon stopper. 8.3.1 Remove the membrane filter from the weighing dish
6.17 Ionizing Unit —Insert under or next to balance pan. with the flat forceps and center in the filtering apparatus.
Assemble the funnel and clamp.
7. Reagent
8.3.2 Fill the volumetric flask containing the sample to the
7.1 Pentane, reagent grade (Warning—See Note 2) con-
100-mL mark with filtered pentane. Stopper and shake well.
forming to the following requirements:
Immediately, filter the mixture using a vacuum of 255 6 50
Distillation
mm Hg (8.1.3.1). Rinse the flask and stopper twice with small
Initial boiling point, min, °C 33.3
amounts of filtered pentane, pouring the washings down the
Dry point, max, °C 40.5
sides of the filter funnel. Rinse the walls of the filter funnel
Olefins none
Isopentane, max, % 20
with a gentle stream of pentane dispensed from the wash bottle.
n-Pentane, min, % 80
8.3.3 Carefully, remove the clamp and funnel. Wash any
Reid vapor pressure, max, kPa 117
adhering insolubles from the funnel onto the membrane, using
NOTE 2—Warning: Extremely flammable. Vapors can cause flash fi
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