This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles

for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D1404/D1404M − 99 (Reapproved 2019)

Standard Test Method for

Estimation of Deleterious Particles in Lubricating Grease1
This standard is issued under the fixed designation D1404/D1404M; 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 D4175 Terminology Relating to Petroleum Products, Liquid

1.1 This test method covers a procedure for the detection Fuels, and Lubricants
and estimation of deleterious particles in lubricating grease.
3. Terminology
1.2 This test method is applicable to all lubricating greases.
It can also be used to test other semi-solid or viscous materials. 3.1 Definitions—See Terminology D4175.
Grease fillers, such as graphite and molybdenum disulfide, can 3.2 Definitions:
be tested for abrasive contaminants by first mixing them into 3.2.1 lubricant, n—any material interposed between two
petrolatum or grease known to be free of deleterious particles. surfaces that reduces the friction or wear between them.
1.3 The values stated in either SI units or inch-pound units 3.2.2 lubricating grease, n—a semi-fluid to solid product of
are to be regarded separately as standard. The values stated in a dispersion of a thickener in a liquid lubricant.
each system may not be exact equivalents; therefore, each 3.2.2.1 Discussion—The dispersion of the thickener forms a
system shall be used independently of the other. Combining two-phase system and immobilizes the liquid lubricant by
values from the two systems may result in non-conformance surface tension and other physical forces. Other ingredients are
with the standard. Within the text, the SI units are shown in commonly included to impart special properties.
brackets.
3.2.3 thickener, n—in lubricating grease, a substance com-
1.4 This standard does not purport to address all of the
posed of finely-divided particles dispersed in a liquid lubricant
safety concerns, if any, associated with its use. It is the
to form the product’s structure.
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter- 3.2.3.1 Discussion—The solid thickener can be fibers (such

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mine the applicability of regulatory limitations prior to use. as various metallic soaps) or plates or spheres (such as certain
1.5 This international standard was developed in accor- non-soap thickeners), which are insoluble or, at the most, only
dance with internationally recognized principles on standard- very slightly soluble in the liquid lubricant. The general
ization established in the Decision on Principles for the requirements are that the solid particles be extremely small,
Development of International Standards, Guides and Recom- uniformly dispersed, and capable of forming a relatively stable,
mendations issued by the World Trade Organization Technical gel-like structure with the liquid lubricant.
Barriers to Trade (TBT) Committee. 3.3 Definitions of Terms Specific to This Standard:
3.3.1 deleterious particles, n—in lubricating grease, minute
2. Referenced Documents bits of solid material present as a contaminant and abrasive to
2.1 ASTM Standards:2 acrylic plastic.
D235 Specification for Mineral Spirits (Petroleum Spirits)
(Hydrocarbon Dry Cleaning Solvent) 4. Summary of Test Method
D785 Test Method for Rockwell Hardness of Plastics and 4.1 A small portion of the lubricating grease sample is
Electrical Insulating Materials placed between two clean, highly polished acrylic-plastic
plates held rigidly and parallel in metal holders. A pressure of
1
This test method is under the jurisdiction of ASTM Committee D02 on
200 psi [1.38 MPa] is applied, and one plate is rotated 30°
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of relative to the other. Particles harder than the plastic and
Subcommittee D02.G0.01 on Chemical and General Laboratory Tests. exceeding in size the distance between the plates will imbed in
Current edition approved June 1, 2019. Published July 2019. Originally approved the plates and cause characteristic, arc-shaped scratches in the
in 1956. Last previous edition approved in 2014 as D1404/D1404M – 99 (2014).
DOI: 10.1520/D1404_D1404M-99R19.
plates.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
4.2 The relative number of such solid particles can be
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on estimated by counting the total number of arc-shaped scratches
the ASTM website. on the two plates.

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 D1404/D1404M − 99 (2019)
5. Significance and Use [25.4 mm 6 1.3 mm square by 3.2 mm 6 0.64 mm] uniformly
5.1 The significance of the number of scratches as far as thick, having a Rockwell M hardness of 94 6 10 (Test Method
correlation with field performance is concerned has not been D785), and having highly polished surfaces protected on both
established. A particle which is abrasive to plastic will not sides with protective paper.
necessarily be abrasive to steel or other bearing materials. NOTE 3—Whether dimensioned in inches or millimetres, the plastic test
Some correlation was obtained in that the contaminant used in plates should be fabricated to match the square recesses in holders 2 and
Sample 3 (see 10.1.1) had a greater wear rate in a laboratory 7.
ball bearing abrasive wear test than the contaminant in Sample
2. 7. Reagents and Materials
NOTE 1—The number of scratches obtained cannot be used to draw fine 7.1 Stoddard solvent conforming to Specification D235.
differences between greases, but rather, to group them into two or three (Warning—Flammable. Vapor harmful.)
general classes. One such possible division could be:
NOTE 4—Other naphthas or pure paraffinic hydrocarbons, such as
1 ... . less than 10 scratches
n-heptane, can be substituted providing they are suitably volatile and do
2 ... . 10 to 40 scratches
3 ... . more than 40 scratches not soften or otherwise attack acrylic plastic.

5.2 An advantage of this test method is that each test takes

8. Procedure
only a few minutes to run.
8.1 Use a fine, smoothing file to break sharp edges of one
5.3 This test method is used for quality control and speci-
face of each test plate. (A sharp edge could scratch the face of
fication purpose.
the opposite plate.) Remove plastic filings and dust. Do not
6. Apparatus remove protective paper at this time.
6.1 The test apparatus is shown in Figs. 1 and 2. As 8.2 Completely remove the tension from the spring and
illustrated in Fig. 2, the plastic test plates (commercial acrylic disassemble the apparatus from the top, Fig. 1b. Snap a test
plastic, produced in uniform, highly polished sheets),3,41, are plate into each of the square recesses of holders 2 and 7 (Fig.
rigidly held in a parallel position in square recesses in parts 2 2); locate the plates such that the surfaces with the filed edges
and 7. The holder, 7, is part of the cap assembly, 7 to 11, which are opposite each other.
can be removed as a unit from the body, 3, by removing four NOTE 5—The square recesses should be clean, that is, free of solid
cap screws. The lower plate holder, 2, can slide along the axis material, to preclude uneven loading of the plastic plates.
of the main housing, but it is restricted from turning by keys 8.3 Remove the protective paper from the test plates. The
spaced 180° apart. Pressure is applied to the plastic plates, 13, exposed polished surfaces must be free of scratches and dust.
through the holder, 2, by means of the coil spring, 4, spring Remove any incidental dust with a soft brush (beware of static
follower plate, 5, and loading screw, 6. The large loading screw charges attracting more dust), damp chamois skin, or
also serves as a base for the apparatus. The indicator pin, 12, on compressed-gas (ionizing-type recommended) dust remover.
the spring follower plate, 5, shows the linear amount of spring
compression, which in turn, is a measure of the pressure 8.4 Place a pea-sized (about 0.25 g), representative sample
applied to the two plastic plates. The upper holder, 7, is kept of the test grease on the face of the lower test plate. Bolt on the
from rotating by the threaded pin, 9, which projects through a cap assembly, making sure the threaded pin, 9, is against one
milled slot in cap, 8, and ends with a locking wing nut, 14. To stop. Use the locking wing nut, 14, to retain this position. Turn
the loading screw to apply a pressure of 200 psi [1.38 MPa] as
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rotate the upper plate and holder, the wing nut is loosened, and
the handle, 11, is turned. A leather washer, 10 , between holder, indicated by the pointer and scale and the apparatus maker’s
7, and cap, 8, is used to facilitate turning. spring calibration.
NOTE 2—Although 6.1 describes an apparatus of specific design, any NOTE 6—The scale indicates linear displacement and does not directly
other device that provides the essential operating conditions can be used. indicate pressure. The apparatus should be supplied with a calibration to
Such device is permitted if it can hold the two plastic test plates parallel convert the scale reading to pressure. (Consult the manufacturer if this
to each other; apply and measure a minimum pressure of 200 psi [1.38 calibration information is missing.) One equipment maker reported the
MPa] on the plastic plates; and provide for 30° relative rotation of the two following calibration:
plates.
Scale reading of 29 5 200 psi @ 1.38 mPA# ,65 %. (1)
6.2 Plastic Test Plates4 ,5—acrylic plastic test plates (two Equipment made at other times or by other manufacturers can vary and
per test), 1 in. 6 0.050 in. square by 1⁄8 in. 6 0.025 in. can have different calibrations.
NOTE 7—The pressure applied to the plates determines the thickness of
the grease layer between them. A pressure of 200 psi [1.38 MPa] gave a
3
The sole source of supply of sized test plates known to the committee at this
thinner layer than 100 psi [0.69 MPa], but increasing the pressure from
time is Koehler Instrument Company, Inc., 1595 Sycamore Ave., Bohemia, NY 200 psi to 500 psi [1.38 MPa to 3.45 MPa] caused very little change.
11716. 8.5 With this pressure applied, loosen the locking wing nut,
4
If you are aware of alternative suppliers, please provide this information to
ASTM International Headquarters. Your comments will receive careful consider- 14, on the cap assembly and turn handle, 11, once as far as it
ation at a meeting of the responsible technical committee,1 which you may attend. will go (about 30°).
5
The apparatus shown in Figs. 1 and 2 is available from Falex Corp., 1020
Airpark Dr., Sugar Grove, IL 60554–9585, and from Koehler Instrument Company, 8.6 Release the spring pressure and disassemble the appa-
Inc., 1595 Sycamore Ave., Bohemia, New York 11716. ratus. Carefully remove the plastic plates from their holders.

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 D1404/D1404M − 99 (2019)

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(a) Assembled View

(b) Unassembled View

FIG. 1 Apparatus for Determining Deleterious Particles in Lubricating Grease

8.7 Mark the plates for identification and remove the pro- 9. Report
tective paper from the back faces. Wash the test grease from the
9.1 Report the following information:
plates with filtered Stoddard solvent (Warning—Flammable.
Vapor harmful) and blow dry with filtered air. Handle the test 9.1.1 Date,
plates very carefully to avoid accidental scratches. 9.1.2 Grease identity,
8.8 Count and record the total number of arc-shaped 9.1.3 Test pressure to the nearest 10 psi [0.07 MPa], and
scratches on the two plastic test plates. See Fig. 3 for examples 9.1.4 Total number of scratches on the two test plates.
of different degrees of scratching.

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 D1404/D1404M − 99 (2019)

1 plastic test plates

2 lower plate holder
3 body FIG. 3 Plastic Test Plates Showing Different Degrees of Scratch-
4 spring ing
5 spring follower plate
6 loading screw
7 upper plate holder
8 cap
9 threaded pin
10 leather washer
10.1.1 A series of cooperative tests were run on three grease
11 handle samples, two of which were artificially contaminated. The
12 indicator pin results from six different laboratories were:
13 key
14 wing nut Sample Average No. Standard
of Scratches Deviation
1 4 6
2 41 8
3 113 27

10.2 Bias—The procedure in Test Method D1404/D1404M

has no bias because the value of the estimation of deleterious
particles in lubricating grease can be defined only in terms of
FIG. 2 Cross-section View of Apparatus a test method.
10. Precision and Bias6 11. Keywords
10.1 Precision—The precision of this test method was not 11.1 abrasive particles; cleanliness; contamination; deleteri-
determined with any currently acceptable guidelines of either
ous particles; lubricating grease; particles; scratch test
ASTM or Committee D02.

6
There is no research report on file because this test method was developed
before research report guidelines were instituted and data are no longer available.

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