Designation: D 4898 – 90 (Reapproved 2000)e1 An American National Standard

Standard Test Method for

Insoluble Contamination of Hydraulic Fluids by Gravimetric
Analysis1
This standard is issued under the fixed designation D 4898; 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.

This standard has been approved for use by agencies of the Department of Defense.

e1 NOTE—Editorial corrections were made throughout in April 2000.

1. Scope F 303 Practices for Sampling Aerospace Fluids from Com-

1.1 This test method covers the determination of insoluble ponents6
contamination in hydraulic fluids by gravimetric analyses. The F 312 Methods for Microscopical Sizing and Counting
contamination determined includes both particulate and gel- Particles from Aerospace Fluids on Membrane Filters7
like matter, organic and inorganic, which is retained on a F 314 Test Methods for Identification of Metallic and Fi-
membrane filter disk of pore diameter as required by applicable brous Contaminants in Aerospace Fluids7
specifications (usually 0.45 µm or 0.80 µm). 2.2 Military Standard:
1.2 To indicate the nature and distribution of the particulate MIL-C-81302 C Cleaning Compound Solvent Trichlorotri-
contamination, the gravimetric method should be supple- fluoroethane8
mented by occasional particle counts of typical samples in 3. Summary of Test Method
accordance with Test Method F 312.
1.3 The values stated in SI units are to be regarded as the 3.1 The insoluble contamination is determined by passing a
standard. given quantity of a fluid sample through a membrane filter disk
1.4 This standard does not purport to address all of the and measuring the resultant increase in the weight of the filter.
safety concerns, if any, associated with its use. It is the The fluid sample is drawn through the filter by a vacuum and
responsibility of the user of this standard to establish appro- the insoluble contamination is collected on the surface of the
priate safety and health practices and determine the applica- filter. In addition, the filter disk is microscopically scanned for
bility of regulatory limitations prior to use. For a specific excessively large particles, fibers, or other unusual conditions.
warning statement, see 6.1. 4. Significance and Use
2. Referenced Documents 4.1 This test method indicates and measures the amount of
2.1 ASTM Standards: insoluble contamination of hydraulic fluids. Minimizing the
A 555/A 555M Specification for General Requirements for levels of insoluble contamination of hydraulic fluids is essen-
Stainless Steel Wire and Wire Rods2 tial for the satisfactory performance and long life of the
D 1836 Specification for Commercial Hexanes3 equipment. Insoluble contamination can not only plug filters
D 2021 Specification for Neutral Detergent, 40 Percent but can damage functional system components resulting in
Alkylbenzene Sulfonate Type4 wear and eventual system failure.
E 319 Practice for the Evaluation of Single-Pan Mechanical 5. Apparatus
Balances5
F 302 Practice for Field Sampling of Aerospace Fluids in 5.1 Microbalance, accurate to 0.005 mg, and the zero shall
Containers6 not drift more than 0.005 mg during the test period. The rated
accuracy shall be obtainable by personnel actually making the
weighings, under actual conditions of use and shall be verified
1
This test method is under the jurisdiction of ASTM Committee D02 on in accordance with Practice E 319.
Petroleum and Petroleum Productsand is the direct responsibility of Subcommittee
D02.N0.02on Industrial Applications.
5.2 Membrane Filter Support, fritted glass, sintered metal,
Current edition approved May 25, 1990. Published July 1990. Originally or stainless steel screen, to support 25-mm or 47 to 51-mm
published as D 2387 – 65 T. ASTM Test Method F 313 – 70 was redesignated membrane filters. The support shall be designed to enable
D 4898 – 73 (1983)e1 in 1988. Last previous edition D 4898 – 78 (1983)e1. attachment of a vacuum flask.
2
Annual Book of ASTM Standards, Vol 01.03.
3
Annual Book of ASTM Standards, Vol 06.04.
4 7
Annual Book of ASTM Standards, Vol 15.04. Annual Book of ASTM Standards, Vol 14.02.
5 8
Annual Book of ASTM Standards, Vol 14.04. Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700
6
Annual Book of ASTM Standards, Vol 15.03. Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS.

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

1
 D 4898
5.3 Filtration Funnel, glass or stainless steel, minimum 8. Preparation of Apparatus
capacity 15 mL, designed to enable attachment to the mem- 8.1 The filtration funnel, petri dishes, graduated cylinders,
brane filter support by means of a suitable clamping device. and sample bottles shall be cleaned before each use by the
The filter funnel is calibrated to indicate volume. following method:
5.4 Vacuum Flask, 250-mL, with rubber stopper. 8.1.1 Thoroughly wash in a solution of detergent and hot
5.5 Filtered Liquid Dispensers (2)—Washing bottles or water.
other dispensers capable of delivering liquid through a 0.45-µm 8.1.2 Rinse with hot tap water and finally with distilled or
in-line membrane filter. deionized water.
5.6 Air Ionizer, alpha emitter, 18.5 MBq, of polonium-210, 8.1.3 Rinse twice with filtered isopropyl alcohol (delivered
with a useful life of 1.5 years to a final value of 1.1 MBq.9 through a filtered liquid dispenser).
5.7 Membrane Filters (2), 25 mm or 47 to 51 mm in 8.1.4 Rinse twice with filtered commercial hexane (deliv-
diameter, with pore diameter as required. ered through filtered liquid dispenser).
5.8 Microscope, capable of 353 magnification. 8.1.5 Leave approximately 1 mL of commercial hexane in
5.9 Vacuum Source, capable of pulling 550 mm Hg. An the bottom of each sample bottle. Replace sample bottle cap
electrically driven vacuum pump must be explosion-proof. (Warning-Flammable. Harmful if inhaled. Skin irritant on
5.10 Drying Oven, capable of maintaining a temperature of repeated contact. Eye irritant. Aspiration hazard.).
80°C.
5.11 Sample Bottles, with contamination-proof caps. 9. Procedure
Aluminum-foil wrapped stoppers or polyethylene liners be- 9.1 Select two membrane filters of the pore diameter re-
tween cap and bottle have proved satisfactory. quired. Allow the filters to stabilize to equilibrium with
5.12 Graduated Cylinder, 100-mL (May be replaced by ambient room conditions. Record room temperature and rela-
volume-calibrated filter funnel.) tive humidity.
5.13 Petri Dishes, covered glass, 150 mm in diameter. 9.2 Take precautions to minimize apparatus contamination
5.14 Forceps, with unserrated tips. from airborne dust. Use a protective hood or cover.
5.15 Calibration Weights, for microbalance, 10 mg and 20
NOTE 2—One of the filters mentioned in 9.1 is for a blank determina-
mg, accurate to 0.005 mg and made from nonmagnetic material
tion, which is necessary to provide a correction factor for adsorption of
conforming to Type 310 in Specification A 555/A 555M. The hydraulic fluid by the filter, desorption of filter constituents by the solvent,
accuracy is traceable to the National Bureau of Standards as and variations of moisture content of the filter. This blank should be
discussed in their Technical Note 288 . determined for each sample of a given composition and history. In a series
of samples of similar fluids with similar history, the blank need be
6. Reagents determined only once. However, with any change of sample volume, a
6.1 Commercial Hexane, conforming to Specifications new blank should be determined as the relationship of blank correction to
sample volume cannot be extrapolated.
D 1836 (Warning-Flammable. Harmful if inhaled. Skin irri-
tant on repeated contact. Eye irritant. Aspiration hazard.). 9.3 Using forceps, weigh each filter on a microbalance to
6.2 Detergent, free-rinsing. Material conforming to Specifi- the nearest 0.005 mg.
cation D 2021. 9.4 Place the filters, one above the other, in the filtration
6.3 Isopropyl Alcohol, acetone-free (Warning-Flammable. apparatus. Ground the clamp to reduce static buildup during
Harmful if inhaled. Skin irritant on repeated contact. Eye filtration.
irritant. Aspiration hazard.). 9.5 Shake the sample container for approximately 1 min.
6.4 Refrigerant-113 (trichlorotrifluoroethane) conforming to 9.6 Measure the desired sample volume with a graduated
U.S. Military Specification MIL-C-81302C (Warning- cylinder and pour into the filter funnel, or pour the required
Flammable. Harmful if inhaled. Skin irritant on repeated volume directly into a calibrated filter funnel. Apply a vacuum
contact. Eye irritant. Aspiration hazard.). and filter the entire sample.
9.7 Use a stream of filtered commercial hexane or Refrig-
7. Sample erant 113 from a filtered liquid dispenser to rinse the residual
7.1 A 100 6 1-mL fluid sample shall be used for this sample from the graduated cylinder into the filter funnel and to
method. Larger or smaller samples may be used, however, to wash down the inside of the filter funnel. The outside of the
meet problems of unusually high or low contamination levels. filter unit should also be washed at the joint between the filter
holder and filter base to remove fluid between the holder and
NOTE 1—Methods for obtaining the fluid samples are not specified in
the filter disk. Repeat the washing twice so that a total of
this method. These methods should be established by the individual
agencies or laboratories in accordance with their requirements. However, approximately 100 mL of commercial hexane or Refrigerant
extreme care should be taken to ensure that the samples are representative 113 is used for the washing process.
and free of external contamination. 9.8 With the vacuum still applied, remove the funnel, taking
7.2 The following ASTM sampling test methods should be care not to disturb the filter. With a fine steady stream, wash
used when applicable: Practices F 302 and F 303. any residual hydraulic fluid from the periphery of the filter with
filtered commercial hexane. The washing action should be
towards the center with care taken not to disturb the deposited
9
May be obtained from any source approved by U.S. Nuclear Regulatory contaminates on the filter surface. Continue washing until the
Commission. total volume of filtered hexane equals 250 to 300 mL.

2
 D 4898
9.9 Dry the filters with aspirator action and release the 10. Calculations
vacuum.
10.1 Calculate the weight of the contaminant as follows:
9.10 Using forceps, remove the filters and place in a covered
petri dish. Place the petri dish in an 80°C oven for 15 min. 10.1.1 Subtract the initial weight (9.3) from the final weight
Other drying methods such as 5 min of continuous aspirator (9.12) of the test filter (upper membrane) and of the blank filter
action or vacuum dessication may be substituted for the (lower membrane).
oven-drying method if such substituted method proves superior 10.1.2 Subtract the weight change of the blank from the
to the oven method in achieving a constant weight upon weight change of the test filter.
continued drying. The nature of the contaminant will dictate 10.1.3 The contamination weight is expressed as
the drying method to be used. milligrams/100 mL of fluid sample retained on the specified
9.11 Allow the filters to equilibrate to ambient room condi- pore diameter membrane filter.
tions for 5 min in the petri dish with cover ajar. Record the
room temperature and relative humidity. When these values 11. Precision and Bias
differ from ambient conditions recorded as described in 9.1,
results will be invalid unless a blank filter is run concurrently 11.1 Precision:
(see Note 2). Remove static electricity by placing each mem- 11.1.1 Repeatability—Duplicate results by the same oper-
brane on the air ionizer for several seconds. ator should be considered suspect if they differ by more than
9.12 Weigh each filter to the nearest 0.005 mg. 3.6 % of the weight of contamination per 100 mL of the
9.13 Inspect the same filter (upper membrane) under a sample.
microscope at approximately 353. The presence of large or
11.1.2 Reproducibility—Available data do not justify any
unusual particles or fibers shall be sufficient cause for request-
statement.
ing another sampling and analysis even though the allowable
contamination weight is not exceeded. 11.2 Bias—Since there is no accepted reference material
9.14 For further examination of the filter, reference may be suitable for determining the bias for the procedure for measur-
made to Test Method F 314 (Warning-Flammable. Harmful if ing insoluble contamination, no bias can be determined.
inhaled. Skin irritant on repeated contact. Eye irritant. Aspira-
tion hazard.).

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