Designation: D7918 − 15

Standard Test Method for

Measurement of Flow Properties and Evaluation of Wear,
Contaminants and Oxidative Properties of Lubricating
Grease by Die Extrusion Method and Preparation1
This standard is issued under the fixed designation D7918; 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 tent in Lubricating Greases by Linear Sweep Voltammetry

1.1 This test method covers the determination and evalua- D7718 Practice for Obtaining In-Service Samples of Lubri-
tion of flow properties, wear levels, contaminants, and oxida- cating Grease
tive condition of new and in-service lubricating grease. D7843 Test Method for Measurement of Lubricant Gener-
ated Insoluble Color Bodies in In-Service Turbine Oils
1.2 This test method provides guidance on evaluating in- using Membrane Patch Colorimetry
service grease samples, NLGI grades 00 to 3, for wear, E177 Practice for Use of the Terms Precision and Bias in
consistency, contamination, and oxidation. ASTM Test Methods
1.3 The values stated in SI units are to be regarded as the E691 Practice for Conducting an Interlaboratory Study to
standard. The values given in parentheses are for information Determine the Precision of a Test Method
only.
1.3.1 Exception—The exception to this will be where units 3. Terminology
of references were developed by the developers of the test 3.1 Definitions:
equipment and necessary to report the results of the test. 3.1.1 active grease sampling device, n—device designed to
1.4 This standard does not purport to address all of the take an active sample of a lubricating grease from a bearing,
safety concerns, if any, associated with its use. It is the gear, or drive shaft located in a grease lubricated component.
responsibility of the user of this standard to establish appro- D7718
priate safety and health practices and determine the applica- 3.1.1.1 Discussion—The Grease Thief (trademarked) Type
bility of regulatory limitations prior to use. 23 is a tool which meets this description and can be used to
obtain an active grease sample from a lubricated component. A
2. Referenced Documents full description and dimensions of this device can be found in
2.1 ASTM Standards:2 Annex A2.
D217 Test Methods for Cone Penetration of Lubricating 3.1.2 active sampling, v—to use a sampling device to
Grease actively gather an in-service lubricating grease sample from a
D4175 Terminology Relating to Petroleum, Petroleum grease-lubricated component. D7718
Products, and Lubricants 3.1.3 calibration, n—the determination of the values of the
D6595 Test Method for Determination of Wear Metals and significant parameters by comparison with values indicated by
Contaminants in Used Lubricating Oils or Used Hydraulic a set of reference standards. D6595
Fluids by Rotating Disc Electrode Atomic Emission Spec-
trometry 3.1.4 consistency, n—of lubricating grease, the degree of
D7527 Test Method for Measurement of Antioxidant Con- resistance to movement under stress. D217

1 3
This test method is under the jurisdiction of ASTM Committee D02 on The Grease Thief Type I and Type II is described in US Patent No. 7984661.
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Interested parties are invited to submit information regarding the identification of an
Subcommittee D02.96.07 on Integrated Testers, Instrumentation Techniques for alternative(s) to this patented item to the ASTM International Headquarters. Your
In-Service Lubricants. comments will receive careful consideration at a meeting of the responsible
Current edition approved June 1, 2015. Published June 2015. DOI: 10.1520/ technical committee, which you may attend. The sole source of the Grease Thief
D7918-15. Type I and Type II are known to the committee is York Laboratories, LLC located
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or at 410 Kings Mill Rd., York, PA 17401. If you are aware of alternative suppliers,
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM please provide this information to ASTM International Headquarters. Your com-
Standards volume information, refer to the standard’s Document Summary page on ments will receive careful consideration at a meeting of the responsible technical
the ASTM website. committee,1 which you may attend.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

1
 D7918 − 15
3.1.4.1 Discussion—The term consistency is used somewhat 3.2.11 speed 1, n—the slowest speed in which the grease is
synonymously with penetration. Generally, consistency refers extruded from the indexing die.
to the worked penetration of a grease. 3.2.12 speed 2, n—the fastest speed in which the grease is
3.1.5 linear sweep voltammetry, n—a test method designed extruded from the indexing die.
to monitor the anti-oxidant additive content in lubricating 3.2.13 speed 3, n—the intermediate speed at which the
greases. D7527 grease is extruded from the indexing die.
3.1.6 lubricating grease, n—a semi-fluid to solid product of
dispersion of a thickener in a liquid lubricant. D217 4. Summary of Test Method
3.1.6.1 Discussion—The dispersion of the thickener forms a
4.1 Testing of a grease sample includes steps that charac-
two-phase system and immobilizes the liquid lubricant by
terize the ferrous wear within the sample, the consistency of
surface tension and other physical forces. Other ingredients are
the sample, and properties related to its chemistry.
commonly included to impart special properties.
3.1.7 in-service lubricating grease, n—lubricating grease 4.2 A grease sample of known volume is measured to
that has been applied as a lubricant to a gear, bearing, or drive determine the density of ferrous material in the sample.
screw for any period of time. D7718 4.3 A grease sample held with a defined geometry sample
3.1.8 passive grease sampling device, n—a device designed holder is placed into a temperature-controlled instrument and
to gather a sample from the equipment by being attached to the extruded onto a substrate as a thin ribbon or strip of grease. The
grease reservoir at the purge point. D7718 extrusion process provides a measurement of the consistency
3.1.8.1 Discussion—The Grease Thief (trademarked) Type of the grease.
13 is a tool which meets this description and can be used to 4.4 The test method requires the grease to be tested at three
obtain a representative grease sample from a purge path. A full different rates to reflect the non-Newtonian nature of greases.
description and dimensions of this device can be found in Testing at several different rates creates a series of step changes
Annex A1. that are then compared to an unused baseline grease that has
3.1.9 passive sampling, v—to use a passive grease sampling also been tested under the same conditions.
device to collect a purged sample of in-service lubricating 4.5 While the flow properties are being measured, the grease
grease from a purge path. D7718 is simultaneously deposited onto a thin-film substrate contain-
3.2 Definitions of Terms Specific to This Standard: ing substrate segments. Each substrate segment contains ap-
3.2.1 die extrusion index, n—an average of three unique test proximately 0.25 g of grease. The individual substrate seg-
conditions of the in-service lubricating grease sample ex- ments are used for further testing of wear, contamination, and
pressed as a percent when compared to the average of three oxidative properties.
unique test conditions of the unused lubricating grease base- 4.6 The substrate is removed from the instrument and
line. processed further to obtain information related to the chemistry
3.2.2 die extrusion tester, n—a device that measures the and content of the grease sample including linear sweep
consistency of in-service lubricating greases and compares the voltammetry and grease colorimetry.
measurement to the values obtained from a baseline sample of
lubricating grease. 5. Significance and Use
3.2.3 ferrous debris level, n—the total amount of ferrous 5.1 Trending the wear, contamination, consistency, and
metal as measured by a Hall-effect sensor in the grease sample oxidative properties of a lubricating grease are a crucial part of
independent of particle size. condition monitoring programs. Changes in these properties or
3.2.4 full attenuation, n—the loss of intensity in signal deviations from the new grease can be indicative of problems
strength. within the lubricated component, such as the mixing of
3.2.5 grease colorimetry, n—the science of color measure- incompatible thickener types, excessive wear or contaminant
ment by the evaluation of the CIE LAB values of grease in the levels, or significant depletion of antioxidant levels. These test
visible light region of the electromagnetic spectrum. methods also makes it possible to develop trends that can be
used to predict failures before they occur and allow for
3.2.6 grease ribbon, n—grease that is extruded onto a
corrective action to be taken.
substrate.
3.2.7 indexing die, n—a single-use orifice die to measure the 6. Interferences
consistency as compared to the baseline.
6.1 Particulate Matter—When the in-service grease sample
3.2.8 spring cell calibration cylinder, n—a cylinder that
is heavily contaminated with particulate matter, it may be
houses a spring and a push rod to compress the spring.
necessary to perform a dilution of the sample in order to
3.2.9 substrate, n—the single-use strip onto which a ribbon properly extrude the sample onto the substrate. Larger pieces of
of grease is extruded. particulate matter may also cause spikes in the load profile
3.2.10 substrate segment, n—a peel-away section of the graph. The data from these spikes should be discounted from
substrate containing a portion of the extruded grease; the the average force calculations because they are not indicative
segments are pre-cut to hold 0.25 g of extruded grease ribbon. of changes in the flow properties of the sample.

2
 D7918 − 15
6.1.1 Heavily contaminated grease samples are considered handle of the passive grease sampling device to measure the
any grease that contains solid particulate of size or quantity that force during the extrusion. The die extrusion tester is shown in
results in clogging of the die, which inhibits the completion of Fig. 1.
the test. 7.4 Constant Temperature Chamber—The test specimens in
NOTE 1—The specific steps to perform a dilution of grease samples is the passive grease sampling device should be heated in the
not addressed in this test method. temperature-controlled chamber of the die extrusion tester
6.2 Sample Size—The passive sampling device shall be at prior to performing any test. The passive grease sampling
least 70 % filled to perform the testing indicated within this test device shall have the indexing die firmly engaged on the
method. If the sampling device is insufficiently filled, the threaded open end of the device.
instrument may not record a force reading over the entirety of 7.5 Ferrous Debris Analyzer—An analyzer that allows the
the program. passive grease sampling device to be inserted completely in the
6.3 Color—The grease colorimetry test may become insig- coil geometry, designed to measure the total amount of ferrous
nificant if the color of the grease causes full attenuation and debris in the grease sample. By use of a Hall-effect sensor, the
minimal transmittance of the signal making it incomparable to total amount of ferrous debris is designed to measure quanti-
the new grease. tatively in parts per million (ppm). Upon receipt of the sample,
it is the first test performed on the grease.
7. Apparatus 7.6 Linear Sweep Voltammetry—Linear sweep voltammetry
7.1 Passive Grease Sampling Device—The device that holds measures the amount of hindered phenols, amines and zinc
the grease sample. The device is typically capable of holding dithio dialkyl phosphate (ZDDP) in a lubricating grease. Using
approximately 1.5 g to 2 g of grease when full. A full 0.25 g of grease from the substrate, one substrate segment is
description and dimensions of this device can be found in inserted into a vial and the antioxidant concentration remaining
Annex A1. in the grease is measured and compared to an unused sample of
7.2 Active Grease Sampling Device—The device that holds the same grease.
an active grease sample from a grease lubricated component. A 7.7 Grease Colorimetry—The grease colorimetry test pro-
full description and dimensions of this device can be found in vides a spectrum in the 400 nm to 700 nm region of the visible
Annex A2. light spectrum. An optical spectroscopy cell is used and the
7.3 Die Extrusion Tester4—Designed for the passive grease substrate segment is placed into the same holder. The delta-E
sampling device, the die extrusion tester is a temperature- values within the CIE LAB scale are recorded and a spectrum
controlled chamber consisting of a table that is controlled by a can be generated in a method similar to Test Method D7843.
linear actuator that holds the substrate, a bracket that holds the 8. Reagents and Materials
passive grease sampling device, and a second linear actuator to
push the handle of the passive grease sampling device. Both 8.1 Spring Cell Calibration Cylinder—This device is used
the passive grease sampling device and the second linear to perform a calibration check on the die extrusion tester prior
actuator are mounted perpendicular to the substrate table. A to use. See Annex A3 for the full calibration procedure.
load cell is mounted between the second actuator and the 8.2 Indexing Die—Threads onto the end of the passive
grease sampling device prior to performing the die extrusion
test.
8.3 Substrate—The three-layered plastic substrate shall be
4
Wurzbach, R. and Williams, L., “Die Extrusion Method For Comparing long enough to hold the grease ribbon once it is extruded from
Changes in Grease Consistency and Flow Characteristics,” Viscosity and Rheology the indexing die. The substrate’s three layers consist of a rigid
of In-Service Fluids as They Pertain to Condition Monitoring, ASTM STP 1564,
2013, ASTM International.

FIG. 1 Die Extrusion Tester4

3
 D7918 − 15
bottom layer of high-density polyethylene, a double-sided 12.1.2 Routine Standardization—A minimum two-point
releasable adhesive, and a top layer of low-density polyethyl- routine standardization shall be performed if the instrument
ene. The top layer of the substrate is divided into peel-away fails the validation check.
segments that, when fully covered with the grease ribbon, each 12.1.3 Set the instrument to grease mode and drop the
contains approximately 0.25 g of grease. sample into the coil.
12.1.4 Record the results in the nearest whole number in
9. Sampling ppm ferrous content.
9.1 Good grease sampling procedures are critical to good 12.2 Analysis of Grease Samples by Die Extrusion4:
analyses and samples should be taken in accordance with 12.2.1 Factory Calibration—The parameters for the analyti-
Practice D7718. cal instrumentation are pre-set by the manufacturer of the
equipment. A calibration curve must be determined prior to use
10. Preparation of Test Specimen to calculate a K constant and an offset for the reference spring
10.1 Ferrous Debris Analyzer—Prior to analysis, the pas- cell. Daily validation checks must be performed and results
sive grease sampling tool shall be removed from the storage must be within the linear range of response.
container. The passive grease sampling tool shall be placed into 12.2.2 Routine Standardization—A minimum two-point
the ferrous debris analyzer to determine the total amount of routine standardization shall be performed if the instrument
ferrous wear present (in ppm). fails the validation check. The procedure for the routine
10.2 Passive Grease Sampling Tool—Upon completion of standardization is described in Annex A4.
the ferrous debris analyzer test, the protective cap shall be 12.3 Steps for Standard and In-service Sample Preparation
removed and an indexing die shall be threaded onto the open Procedure:
end of the passive grease sampling device. 12.3.1 Load a substrate, with the segments facing up.
NOTE 2—If the in-service grease sample is received in an active grease
sampling device the stinger probe must be removed and replaced with the
12.3.2 Upon preparation of the sample, move the heated
handle of a passive grease sampling device prior to use. passive grease sampling device from the heating tray and
NOTE 3—If the in-service grease sample is received in any sampling immediately place into the sample holding bracket with the
container other than the passive or active grease sampling device, it must opening of the indexing die facing the same direction that the
be transferred into a passive grease sampling device by hand, with a clean, table moves. A new, clean indexing die and substrate shall be
single-use glove and/or a clean, single-use 10 mL slip tip syringe.
used for each analysis.
11. Preparation of Apparatus 12.3.3 The die extrusion tester shall be programmed to only
perform the test if the sample is in the appropriate temperature
11.1 Preparation of the Die Extrusion Tester: range. Therefore, if the sample loses too much heat in the
11.1.1 Heating the Chamber—Prior to the performance of loading process, it will need to be reheated. The appropriate
any tests, a thermocouple is used to regulate the temperature of temperature is verified using a non-contact thermometer that
the heating tray to achieve a temperature sufficient to pre-heat has been modeled and calibrated by the manufacturers of the
samples to meet the test temperature requirements for the trial instrument to ensure internal grease temperature of 30 °C 6
specified in 12.3.3. The samples shall be on the heating tray for 2 °C.
at least 20 min to come to thermal equilibrium, which is 12.3.4 The die extrusion tester shall be programmed to run
verified with an embedded thermocouple. the following steps:
11.1.2 Validation Check—A check shall be performed with a 12.3.4.1 The prime must be set so that it allows sufficient
spring cell calibration cylinder to confirm calibration prior to time for the die to be filled. Grease shall be exiting the die
the analysis of routine samples. The procedure and accuracy before continuing to Rate 1.
guidelines for the validation check are described in Annex A3.
12.3.4.2 Rate 1—0.15 mm/s 6 0.01 mm/s for 19 s 6 1 s.
This procedure shall be performed at the beginning of each
shift or if the instrument has not been used for an extended 12.3.4.3 Rate 2—0.73 mm/s 6 0.04 mm/s for 13 s 6 1 s
period of time. 12.3.4.4 Rate 3—0.44 mm/s 6 0.02 mm/s for 22 s 6 1 s
12.3.5 Start the program, which will extrude the lubricating
11.2 Preparation of the Optical Spectroscopy Cell—Check
grease onto the substrate and collect the flow response data.
the mirror, optical path, and the tray for cleanliness.
This methodology is good for grades 1, 2, and 3 greases.
11.3 This test method requires no additional preparation Consult the vendor manual for how to run grades 00 and 0.
steps for the other instruments.
NOTE 4—Die Extrusion testing only uses the speeds that show a force
response in the final calculation of the die extrusion index. The passive
12. Testing Procedure grease sampling device must be at least 70 % full to run the die extrusion
12.1 Procedure for Evaluation of Ferrous Debris Level: test.
12.1.1 Factory Calibration—The parameters for the analyti- 12.3.6 Verify during the prime and prior to Rate 1 step that
cal instrumentation are pre-set by the manufacturer of the the load data shows an increase from the start load. Inspect the
equipment. Daily validation checks must be performed and piston for movement. Its movement should correspond to an
analyses of test specimens must be within the linear range of increase in the load cell reading. If no change of the load cell
response. reading is observed during the prime while the piston is

4
 D7918 − 15
moving, immediately terminate the test by stopping the instru- 13.1.2 To calculate the die extrusion index take the average
ment. If the load cell displays a zero reading during extrusion, stable die extrusion load obtained for each speed, divide by the
it could be an indication of misalignment or instrument value obtained for the baseline, average over the three speeds,
malfunction. Return to 12.3.1 and repeat the test until a and then multiply by 100. The calculation can be seen below in
satisfactory validation step is achieved. Eq 1.
12.3.7 Once the test is complete, the data shall be trans- Die Extrusion Index5
ferred to a computer to be analyzed. For calculations see
Section 13.
12.3.8 Remove the empty passive grease sampling device
FS Load 1 s
Load 1 b DS
3 100 1
Load 2 s
Load 2 b
3 100 1 DS
Load 3 s
Load 3 b
3 100 DG
3
from the die extrusion tester and dispose in the trash.
(1)
12.3.9 Remove the substrate containing the grease ribbon
NOTE 6—Load xs represents the average load for speed x of the sample
for additional testing. and Load xb represents the average load for speed x of the baseline.
12.4 Procedure for Grease Colorimetry: NOTE 7—In instances where the force readings may have spiked or
12.4.1 General Test Procedure—The test procedure will dropped due to large particles or air bubbles, the data should be modified
to exclude these spikes or drops in the final calculations for the die
consist of an unused grease reference reading and the sample extrusion index.
(in-service grease) reading. NOTE 8—There is software available to perform these calculations,
12.4.2 Prepare the grease according to 12.3. which is provided with the purchase of the die extrusion tester.
12.4.3 Calibration of the Spectrophotometer: 13.2 Ferrous Debris Level:
12.4.3.1 Place the blank substrate segment into the drawer 13.2.1 Number is calculated and reported as a whole num-
of the optical spectroscopy cell to collect the background ber ppm value.
spectrum.
12.4.3.2 Attach the surface head to the cell so that it is NOTE 9—For cases where the passive grease sampling device is not
perpendicular to the substrate (or the separator is parallel to the completely filled, the passive grease sampling device will be tared and
weighed to compensate for the low volume sample. A mass compensation
side of the cell containing the drawer). calculation will be done to normalize the results for fdM+.
12.4.3.3 Turn the i-Lab on using the power button in the
center of the unit. 13.3 Linear Sweep Voltammetry:
12.4.3.4 Using the arrow keys, highlight GreaseBk and 13.3.1 Calculations shall be performed following Test
press the power button to select. Method D7527.
12.4.3.5 Remove the protective cap from the i-Lab and 13.4 Grease Colorimetry:
place it onto surface head, which should already be attached to 13.4.1 A series of transmittance values are gathered from
the cell. 400 nm to 700 nm on a handheld spectrophotometer. The data
12.4.3.6 Press the Power button again to obtain the back- shall be graphed using x-y smooth curve plot. On the x-axis
ground spectrum. shall be wavelength and on the y-axis shall be transmittance.
12.4.3.7 Remove the unit from the cell.
12.4.4 Procedure for Sample Data Collection: 14. Report
12.4.4.1 Using the arrow keys, select the GreaseCIE method
and press power. 14.1 The report shall include the die extrusion load 1s, load
12.4.4.2 Invert the unit back onto the surface head and press 2s, and load 3s. The load values shall be rounded to the nearest
power again to obtain the spectrum of the sample. whole number value. The die extrusion index shall be reported
12.4.4.3 Repeat test as needed for multiple samples. using rounded whole number values only. The die extrusion
12.4.5 Procedure for Linear Sweep Voltammetry: index for the baseline grease shall be assigned a value of 100.
12.4.5.1 Prepare the grease sample according to 12.3. NOTE 10—The results of the test depend on the choice of an appropriate
baseline sample or specimen for reference. Typical acceptable references
12.4.5.2 Add one substrate segment with 0.25 g of grease to include unused grease of the same type that the in-service sample is
the vial and follow the procedure outlined in section 8.5.1 in suspected to be. It is the responsibility of the analyst to decide which
Test Method D7527 to perform a linear sweep voltammetry baseline to choose so the comparison data provides the most meaningful
test. results.

NOTE 5—Step 8.5.1.3 in Test Method D7527 shall be replaced with a 14.2 The load data obtained from the die extrusion test shall
single grease strip from the substrate; instead of smearing the grease be graphed as a function of time as the ribbon is extruded from
evenly on the inside of the 7 mL vial, the user shall take one full strip of the die. The baseline graph and sample graph shall overlay
the grease substrate and curl it to fit inside the 7 mL vial. User may each other to demonstrate the changes in flow properties. On
proceed following the remainder of the steps in section 8.5.1 in Test the x-axis shall be time and on the y-axis shall be in grams. The
Method D7527.
integer values in grams for speed 1, speed 2, speed 3, and the
13. Calculations calculated die extrusion index shall also be reported for the
13.1 Die Extrusion Test: sample and baseline on the report.
13.1.1 The flow response data obtained from the die extru- 14.3 Ferrous debris level, linear sweep voltammetry, and
sion tester shall be transferred onto a computer for calculation grease colorimetry data are gathered and reported as graphs
of the die extrusion index for the used or in-service grease and numbers on a grease analysis report that evaluates overall
sample. condition of the grease in four areas: wear, consistency,

5
 D7918 − 15
contamination, and oxidation. The data gathered is reported as TABLE 2 Load 2 (grams)
part of a comprehensive condition based maintenance program. Repeatability
Repeatability
AverageA Standard
Material Limit
15. Precision and Bias Deviation
x̄ sr r
15.1 The precision of this test method is based on an Sample Type 1 365.05 27.19 76.13
interlaboratory study of Test Method D7918, conducted in Sample Type 2 687.30 50.40 141.12
2014. Two operators tested six different types of grease at three Sample Type 3 1069.90 58.69 164.33
Sample Type 4 651.70 19.85 55.58
loads and calculated GTI based on obtained load values. Every Sample Type 5 702.45 35.09 98.25
“test result” represents an individual determination, and all Sample Type 6 618.80 24.92 69.77
participants were instructed to report ten replicate test results A
The average of the laboratories’ calculated averages.
per material. Practice E691 was followed for the design and
analysis of the data; the details are given in ASTM Research
Report No. RR:D02-1802.5 TABLE 3 Load 3 (grams)
15.1.1 Repeatability (r)—The difference between repetitive Repeatability
Repeatability
results obtained by the same operator in a given laboratory AverageA Standard
Material Limit
Deviation
applying the same test method with the same apparatus under
x̄ sr r
constant operating conditions on identical test material within
Sample Type 1 300.6 30.6 85.6
short intervals of time would in the long run, in the normal and Sample Type 2 582.3 50.1 140.3
correct operation of the test method, exceed the following Sample Type 3 927.2 71.1 199.2
values only in one case in 20. Sample Type 4 562.9 21.5 60.3
Sample Type 5 586.4 37.1 103.9
15.1.1.1 Repeatability can be interpreted as maximum dif- Sample Type 6 526.4 34.6 96.7
ference between two results, obtained under repeatability A
The average of the laboratories’ calculated averages.
conditions, that are accepted as plausible due to random causes
under normal and correct operation of the test method.
15.1.1.2 Repeatability limits are listed in Tables 1-4. TABLE 4 GTI (dimensionless)
15.1.2 Reproducibility (R)—The difference between two Repeatability
single and independent results obtained by different operators Repeatability
AverageA Standard
Material Limit
applying the same test method in different laboratories using Deviation
different apparatus on identical test material would, in the long x̄ sr r
run, in the normal and correct operation of the test method, Sample Type 4 97.5 3.3 9.2
Sample Type 5 102.7 6.2 17.4
exceed the following values only in one case in 20. Sample Type 6 92.9 5.1 14.4
15.1.2.1 Reproducibility can be interpreted as maximum A
The average of the laboratories’ calculated averages.
difference between two results, obtained under reproducibility
conditions, that is accepted as plausible due to random causes
under normal and correct operation of the test method.
15.1.2.2 Reproducibility could not be determined from the 15.2 Bias—At the time of the study, there was no accepted
limited amount of data collected. reference material suitable for determining the bias for this test
15.1.3 The above terms (repeatability limit and reproduc- method, therefore no statement on bias is being made.
ibility limit) are used as specified in Practice E177. 15.3 The precision statement was determined through sta-
15.1.4 Any judgment in accordance with statements 15.1.1 tistical examination of all 420 reported results, from two
and 15.1.2 would have an approximate 95 % probability of operators, on six different greases. These six materials were
being correct. described as the following:
(1) Sample Type 1: NLGI 1
(2) Sample Type 2: NLGI 2
5
Supporting data have been filed at ASTM International Headquarters and may (3) Sample Type 3: NLGI 3
be obtained by requesting Research Report RR:D02-1802. Contact ASTM Customer
Service at [email protected]. (4) Sample Type 4: 50/50 mixture lithium complex thick-
ener: polyurea thickener
TABLE 1 Load 1 (grams) (5) Sample Type 5: copper particulate concentration
Repeatability
(6) Sample Type 6: worked sample
Repeatability
AverageA Standard 15.4 To judge the equivalency of two test results, it is
Material Limit
Deviation
recommended to choose the material closest in characteristics
x̄ sr r
to the test material.
Sample Type 1 300.55 23.73 66.43
Sample Type 2 537.65 44.32 124.08
Sample Type 3 822.25 57.29 160.42 16. Keywords
Sample Type 4 497.55 20.23 56.63
Sample Type 5 514.55 66.95 187.47
16.1 consistency; die extrusion index; die extrusion tester;
Sample Type 6 485.60 33.75 94.50 ferrous debris level; grease colorimetry; in-service lubricating
A
The average of the laboratories’ calculated averages. grease sampling; linear sweep voltammetry; lubricating grease;
lubricating grease sampling device

6
 D7918 − 15

ANNEXES

(Mandatory Information)

A1. GREASE THIEF TYPE 1

A1.1 This is a cylinder with a 1⁄8-in. national pipe thread at grease to purge when the cylinder becomes full of sample.
either end of a precision bore cylinder. Inside the cylinder is a There are molded barbs in the handle that prevent the piston
precision-molded piston with a handle extending out the back and handle from sliding forward out of the cylinder. The
of the piston that allows for movement of the piston. There is Grease Thief Type 1 is depicted in Fig. A1.1.
a pair of relief holes on the cylinder for excess lubricating

7
 D7918 − 15

FIG. A1.1 Grease Thief Type 1

A2. GREASE THIEF TYPE 2

A2.1 This is a cylinder with a 1⁄8-in. national pipe thread at length of the piston. Also, the piston should have a handle that
either end of a precision bore cylinder. There is a pair of relief extends out the opposite end of the cylinder that allows the
holes at one end of the cylinder to allow for purging of excess piston and probe assembly to be attached to an active grease-
lubricating grease. Inside of the cylinder is a precision-molded sampling device extension rod. The Grease Thief Type 2 is
piston with a stinger probe the length of the cylinder minus the depicted in Fig. A2.1.

8
 D7918 − 15

FIG. A2.1 Grease Thief Type 2

A3. VALIDATION CHECK

A3.1 Remove any objects from the substrate table, includ- A3.4 Locate two data points sufficiently far apart and within
ing the substrates. the linear response of the spring cell calibration cylinder,
datapoints X1 and X2. Their corresponding force values should
A3.2 Place the spring cell calibration cylinder into the lie within 65 % deviation of the spring cell calibration curve
sample bracket.
provided with the spring cell following the form: f1(x) = A*x
A3.3 Run the instrument in calibration mode. + B, where A and B are constants, x is the datapoint the
function is evaluated.
A3.3.1 Calibration mode consists of a test run at 0.25 mm/s
for 70 s.

A4. ROUTINE STANDARDIZATION TO CALCULATE NEW LOAD CELL SCALE AND OFFSET

A4.1 Set the load cell scale (K) to 1 and the load cell offset A4.6 The new load cell scale is found by the equation: K =
to 0. A/C. The new offset is found by the equation: offset =
f1(X1)–f2(X1)*K. Enter the K and offset value determined into
A4.2 Secure the spring cell calibration cylinder in the the instrument.
sample holding bracket.
A4.7 Following steps A4.1 to A4.6, determine if the instru-
A4.3 Run the instrument in calibration mode.
ment is within calibration.
A4.4 Locate two data points sufficiently far apart and within
A4.8 If the calibration procedure fails twice the load cell
the linear response of the spring cell calibration cylinder at
datapoints X1 and X2. may be damaged or the instrument may require factory
calibration.
A4.5 Create a load cell calibration curve following the form
f2(x) = C*x + D, by calculating the best fit linear plot between
the selected points. If the R2 value of the best fit to the entire
dataset is less than 0.95, the spring cell may be compromised
or the trial may need to be run again.

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