ASTM D7416-09(2020)

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: D7416 − 09 (Reapproved 2020)
Standard Practice for
Analysis of In-Service Lubricants Using a Particular Five-
Part (Dielectric Permittivity, Time-Resolved Dielectric
Permittivity with Switching Magnetic Fields, Laser Particle
Counter, Microscopic Debris Analysis, and Orbital
Viscometer) Integrated Tester
This standard is issued under the fixed designation D7416; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
1.1 This practice covers procedures for analysis of in-
1.6 This international standard was developed in accor-
servicelubricantsamplesusingaparticularfive-part(dielectric
dance with internationally recognized principles on standard-
permittivity, time-resolved dielectric permittivity with switch-
ization established in the Decision on Principles for the
ing magnetic fields, laser particle counter, microscopic debris
Development of International Standards, Guides and Recom-
analysis, and orbital viscometer) integrated tester to assess
mendations issued by the World Trade Organization Technical
machine wear, lubrication system contamination, and lubricant
Barriers to Trade (TBT) Committee.
dielectric permittivity and viscosity. Analyzed results trigger
recommendedfollow-onactionswhichmightincludeconduct-
2. Referenced Documents
ing more precise standard measurements at a laboratory. Wear
2.1 ASTM Standards:
status, contamination status, and lubricant dielectric permittiv-
ityandviscositystatusarederivedquantitativelyfrommultiple D341Practice for Viscosity-Temperature Equations and
Charts for Liquid Petroleum or Hydrocarbon Products
parameters measured.
D445Test Method for Kinematic Viscosity of Transparent
1.2 This practice is suitable for testing incoming and in-
2 and Opaque Liquids (and Calculation of DynamicViscos-
servicelubricatingoilsinviscositygrades32mm /sat40°Cto
ity)
680mm /s at 40°C having petroleum or synthetic base stock.
D924Test Method for Dissipation Factor (or Power Factor)
This practice is intended to be used for testing in-service
and Relative Permittivity (Dielectric Constant) of Electri-
lubricant samples collected from pumps, electric motors,
cal Insulating Liquids
compressors, turbines, engines, transmissions, gearboxes,
D1298Test Method for Density, Relative Density, or API
crushers, pulverizers, presses, hydraulics and similar machin-
Gravity of Crude Petroleum and Liquid Petroleum Prod-
ery applications. This practice addresses operation and stan-
ucts by Hydrometer Method
dardization to ensure repeatable results.
D4057Practice for Manual Sampling of Petroleum and
1.3 This practice is not intended for use with crude oils.
Petroleum Products
D4177Practice for Automatic Sampling of Petroleum and
1.4 The values stated in SI units are to be regarded as
Petroleum Products
standard. No other units of measurement are included in this
E617Specification for Laboratory Weights and Precision
standard.
Mass Standards
1.5 This standard does not purport to address all of the
E1951Guide for Calibrating Reticles and Light Microscope
safety concerns, if any, associated with its use. It is the
Magnifications
responsibility of the user of this standard to establish appro-
D6300Practice for Determination of Precision and Bias
Data for Use in Test Methods for Petroleum Products,
Liquid Fuels, and Lubricants
This practice is under the jurisdiction ofASTM Committee D02 on Petroleum
Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcom-
mittee D02.96.07 on Integrated Testers, Instrumentation Techniques for In-Service
Lubricants. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved May 1, 2020. Published June 2020. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 2008. Last previous edition approved in 2015 as D7416–09 (2015). Standards volume information, refer to the standard’s Document Summary page on
DOI: 10.1520/D7416-09R20. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D7416 − 09 (2020)
2.2 ISO Standards: 3.2.15 large contaminant droplet (LCont D), n—indication
ISO11171Hydraulicfluidpower—CalibrationofAutomatic reporting sensor 2 detects presence of free-water drops in oil.
Particle Counters for Liquids
3.2.16 large contaminant ferrous (LCont Fe), n—indication
reporting sensor 2 detects presence of very large ferrous-metal
3. Terminology
particles in oil, which are often the kind produced by abrasive
3.1 Definitions:
wear mechanisms.
3.1.1 integrated tester, n—automated, or semi-automated
3.2.17 large contaminant non-ferrous (LCont NF),
stand alone instrument utilizing multiple technologies to pro-
n—indication reporting sensor 2 detects presence of very large
vide diagnostic recommendations (on-site or in-line) for con-
non-ferrous-metal particles in oil, which are often the kind
dition monitoring of in-service lubricants.
produced by abrasive wear mechanisms.
3.2 Definitions of Terms Specific to This Standard:
3.2.18 orbital viscometer, n—four-pole, magnetically
3.2.1 chemistry index (Chem Index), n—parameter com-
driven, orbital viscometer.
puted from dielectric permittivity increase compared to new
oil. The value is equal to dielectric difference multiplied by
3.2.19 new oil, n—sample of as-purchased new oil as
100.
supplied by a manufacturer for use to measure baseline
3.2.2 chemistry status (Chem Status), n—diagnosticseverity
reference values for the following reference oil properties:
ranking having 0 to 100 score based on the highest alarm
dielectric permittivity, specific gravity (Test Method D1298),
indication of dielectric permittivity and viscosity measure-
kinematic viscosity at 40°C (Test Method D445), kinematic
ments.
viscosity at 100°C (Test Method D445), and sensor 2 water
3.2.3 counts ≥ 4, n—sensor 3 measured particle counts per factor.
mL for particles ≥ 4µm.
3.2.20 particular five-part integrated tester, n—integrated
4,5
3.2.4 counts ≥ 6, n—sensor 3 measured particle counts per
tester including these five parts: sensor 1 (dielectric permit-
mL for particles ≥ 6µm.
tivity sensor), sensor 2 (time-resolved dielectric permittivity
5,6
3.2.5 counts≥ 10, n—sensor 3 measured particle counts per sensor with switching magnetic fields), sensor 3 (laser
5,7
mL for particles ≥ 10µm.
particle counter), dual-screen patch maker (initial step in
5,8 5,9
microscopic debris analysis), and orbital viscometer.
3.2.6 counts≥ 14, n—sensor3measuredparticlecountsper
mL for particles ≥ 14µm.
3.2.21 particle count ppm by volume < 6 µm (PC Vol <
3.2.7 counts≥ 18, n—sensor3measuredparticlecountsper 6 µm), n—volume of particulate debris detected using a laser
mL for particles ≥ 18µm.
particle counter in size range ≥ 4µm and < 6µm compared to
-6
volume of oil × 10 .
3.2.8 counts ≥ 22— sensor 3 measured particle counts per
mL for particles ≥ 22µm.
3.2.22 particle count ppm by volume ≥6µmand<14µm
3.2.9 counts ≥ 26—sensor 3 measured particle counts per (PC Vol 6-14 µm), n—volume of particulate debris detected
mL for particles ≥ 26µm.
using a laser particle counter in size range ≥ 4µm and < 6µm
-6
compared to volume of oil × 10 .
3.2.10 counts ≥ 32— sensor 3 measured particle counts per
mL for particles ≥ 32µm.
3.2.23 particle count ppm by volume ≥ 14 µm (PC Vol
3.2.11 counts ≥ 38—sensor 3 measured particle counts per ≥14 µm), n—volumeofparticulatedebrisdetectedusingalaser
mL for particles ≥ 38µm.
particle counter in size range ≥ 14µm compared to volume of
-6
oil×10 .
3.2.12 contaminant status (Cont Status), n—diagnostic se-
verityrankinghaving0to100scorebasedonthehighestalarm
indication of all contamination related parameters.
The analyzer is described in and covered by the following U.S. Patents:
3.2.13 dual-screen patch maker, n—apparatus with screens
5,262,732; 5,394,739; 5,604,441; 5,614,830; 5,656,767; 5,674,401; 5,817,928;
to support individual (most often) or stacked (occasionally for
6,064,480; 6,418,799; 6,582,661; 7,027,959; and 7,065,454. The sole source of
size segregation) filter patches used to extract solid particles
supply of the apparatus known to the committee at this time is Machinery Health
from in-service lubricating fluid as the fluid is evacuated from
Management, Emerson Process Management, 835 Innovation Drive, Knoxville,TN
37932.
sensor 2 test chamber. This item is often referred to simply as
If you are aware of alternative suppliers, please provide this information to
“patch maker.”
ASTM International Headquarters. Your comments will receive careful consider-
ation at a meeting of the responsible technical committee, which you may attend.
3.2.14 ferrous index (Fe Index), n—ferrous density type
The time-resolved dielectric sensor with switching electromagnets is described
parameter measuring relative concentration and size of mag-
in and covered by U.S. Patent 5,604,441.
netically responsive iron particles ≥ 5µm collected on a
Sensor3usesmethodsdescribedinandcoveredbyU.S.Patents6,064,480and
dielectric permittivity sensor.
7,065,454.
The patch maker with dual screens is described in and covered by U.S. Patent
6,418,799.
The orbital viscometer is described in and covered by U.S. Patent 5,394,739.
Available from International Organization for Standardization (ISO), ISO The sole source of supply of the apparatus known to the committee at this time is
Central Secretariat, Chemin de Blandonnet 8, CP 401, 1214 Vernier, Geneva, Machinery Health Management, Emerson Process Management, 835 Innovation
Switzerland, http://www.iso.org. Drive, Knoxville, TN 37932.
D7416 − 09 (2020)
3.2.24 particle count ppm by volume total (PC Vol Total), 4.1.4 Particle counting is measured using a laser particle
n—volume of all particulate debris detected using a laser counter gated to detect and count individual particles at eight
particlecounterinsizerange≥4µmcomparedtovolumeofoil size ranges.
-6
×10 . 4.1.5 Microscopic wear debris analysis is performed after
collecting solids on a filter patch and placing the filter patch
3.2.25 Sensor 1, n—dielectric permittivity sensor having
under an optical microscope.
oil-filled cavity between central oscillating electrode and
grounded concentric-shell. 4.2 Computer Application Software—A computer applica-
tion software program guides the test sequence and provides
3.2.26 Sensor 2, n—concentric-electrical-trace-type time-
analysis, diagnostic determination, data storage, and reporting.
resolved dielectric permittivity sensor using a ceramic fiber
filled printed circuit board and including pair of coaxial,
5. Significance and Use
switching electromagnets proximate to the underside of the
5.1 In-plant Oil Analysis—The particular five-part inte-
surface supporting the concentric electrical traces.
grated tester practice is primarily used by plant maintenance
3.2.27 Sensor 2 water factor, n—proportional measure of
personnel desiring to perform on-site analysis of as-received
time-resolved-dielectric permittivity per 1% emulsified water-
and in-service lubricating oils.
in-oil.
5.2 Detect Common Lubrication Problems—The software
3.2.28 Sensor 3, n—light-blocking-type (also called light-
application interprets data from integration of multiple sensing
extinction-type) laser particle counter sensor.
technologies to detect common lubrication problems from
3.2.29 system debris, n—calculated volume of debris in
inadvertent mixing of dissimilar lubricant viscosity grades and
entire oil compartment (PC Vol Total multiplied by volume of
from particulate or moisture contamination. The redundant
oil compartment).
views of ferrous particulates (sensor 2), all particulates larger
3.2.30 orbital viscosity at 25 °C (Visc 25C)—orbital vis- than4µm(sensor3),andallsolidparticulateslargerthanfilter
patchporesize(patchmaker)providesscreeningforoilwetted
cometer viscosity measurement reported as absolute viscosity
(mPa×sat25°C). mechanical system failure mechanisms from incipient to cata-
strophic stages.
3.2.31 orbital viscosity at 40 °C (Visc 40C)—orbital vis-
cometerviscositymeasurementreportedaskinematicviscosity
5.3 Supported by Off-Site Lab Analysis—The particular
(mm /s) at 40°C. five-part integrated tester is normally used in conjunction with
anoff-sitelaboratorywhenexploringtheparticularnatureofan
3.2.32 percent change in viscosity at 40 °C (Visc%Chng)—
alarmingoilsample.Anoff-sitelaboratoryshouldbeconsulted
parameter comparing Visc 40C between new in-service oil.
for appropriate additional tests.
3.2.33 wear debris analysis classification (WDA
classification)—microscopic debris analysis classification
6. Interferences
method that closely identifies particulate debris from an oil
6.1 Wrong Solvent Selection—The particular five-part inte-
sample.
grated tester testing almost always requires the use of dilution
3.2.34 weardebrisanalysisseverity(WDAseverity)—score-
withasolventthatissolublewiththein-servicelubricantbeing
type parameter or alarming system assigned by an analyst that
tested. All petroleum-based and most synthetic lubricants
reflects a qualitative assessment of risk to machine health as
dissolveverywellinkerosineorlampoil,sothisismostoften
evidenced by microscopic viewing of collected contamination
used. However, certain synthetics remain immiscible in these
and wear debris.
solvents. See 8.3 and Table 1. It is therefore very important to
verifysolubilityofsynthetic-basedlubricantsbeingtestedwith
3.2.35 wear status—diagnostic severity ranking having 0 to
the diluents and cleaning solvents being used. To do this, add
100 score based on the highest alarm indication of all wear
a 50:50 mixture of solvent and sample in a bottle, shake
related parameters.
vigorously, and allow settling for 1 min. Layered fluids or
emulsion are signs of insolubility. This is likely to cause
4. Summary of Practice
erroneous measurements using sensors 2 and 3.
4.1 Measurements Made—The particular five-part inte-
6.2 Improper Sampling Techniques—Interferences can be
grated tester sequentially measures viscosity, dielectric
produced by improper sampling techniques. Practice D4177
permittivity, water-in-oil, ferrous debris, particle count and
shouldbefollowed.Samplescollectedfromcold,notoperating
distribution, and microscopic wear debris analysis for in-
machinery are not likely to properly represent contaminants
service oil samples.
and wear debris since these settle when the system is not hot
4.1.1 Absolute viscosity is measured based on speed of an
and flowing. Interferences may be produced by contaminated
orbiting steel ball forced by controlled magnetic fields. Tem-
bottles, uncapped new bottles, and incorrectly labeled sample
perature of fluid under test is also measured.
bottles.
4.1.2 Dielectricpermittivityismeasuredusingaconcentric-
shell-type capacitive sensor.
6.3 Particle Count Interferences—Sensor 3 is a light obscu-
4.1.3 Water-in-oil and ferrous debris are each measured ration type laser particle counter and is therefore subject to
using time-resolved dielectric sensor and are differentiated by interferences from air bubbles, dark fluids, and emulsified
using a switching dual-coil electromagnet. water. Follow manufacturer recommended procedures to avoid
D7416 − 09 (2020)
A
TABLE 1 Oil and Solvent Solubility
NOTE 1—Y=Yes, N=No
Oil Class Dielectric Original Lamp Ultra Pure Original Lamp Toluene Hexane Fluid A Fluid B Fluid C
Oil or Kerosine Lamp Oil Oil + Fluid B
Mineral Oil 2.1–2.4 Y Y Y Y Y Y Y N Most industrial
lubricants
PAO 2.1– 2.4 Y Y Y Y Y Y Y N Synthetic
Hydrocarbon
Diester 3.4– 4.3 Y Y Y Y Y Y Y Y Diester
POE + PAG 4.6– 4.8 Y Y Y Y Y Y Y Y Polyol Ester +
Polyalkylene Glycol
PAG 6.6–7.3 N N N Y Y N N N Polyalkylene
Glycol
PhE 6.0–7.1 sometimes N Y Y Y N Y Y Phosphate
Ester
A
(Warning—Both Toluene and Isopropyl Alcohol have flash points below room temperature. They require an explosion proof vacuum pump.)
these interferences. Interference caused by false counts from
air bubbles may be caused by inadequate degassing with the
30mLsyringeinaninvertedposition.Forverydarkin-service
lubricants, when sensor 3 gives an alert that oil sample may be
too dark, retest with additional dilution. Avoid false counts
fromemulsifiedwater-in-oilbyusingthewatermaskingstepin
8.4.
6.4 CoincidenceErrors—Sensor3laserparticlecounterwill
experience abnormally high coincidence errors when it at-
tempts to count more than 20000 particles per millilitre.
Coincidenceerrorsresultwhenmoreoneparticleisinthelaser
window at one time. When two small particles are coinciden-
tallyinthelaserwindow,theyareeffectivelycountedlikethey
are a single particle having double cross-section. This artifi-
cially lowers measured counts at small sizes and inflates the
FIG. 1 Example of Layout for a Particular Five-Part Integrated
counts at larger sizes. Coincidence errors >10% are not
Tester
acceptable. Avoid coincidence by performing second dilution
priortosensor3testing.Forexample,ifyoudilute4-to-1,then
you can expect to detect less than5×20000or100000
displaced as the fluid rises to fill the entire volume of the
particles per millilitre.
sensor. It takes approximately 8mLof test fluid to completely
fill the tubing and sensor. Dielectric permittivity measurement
7. Apparatus
ismadebymeasuringcapacitanceofthecalibratedsensor.The
7.1 Bench Top Setup—The particular five-part integrated
concentric-shell-type-capacitor dielectric permittivity is cali-
,10
tester with example arrangement shown in Fig. 1.
brated to within 61% of known values for standardization
fluids A, B, and C.
7.2 Core Analyzer—The core analyzer as shown on right in
7.2.2 Sensor 2 includes (1) a concentric-trace-type-
Fig. 1 incorporates sensor 1 (dielectric permittivity sensor),
capacitor dielectric permittivity measurement sensor mounted
sensor 2 (time-resolved-dielectric-permittivity measurement
above (2) a dual-coil electromagnet suitable for introducing
with switching electromagnet), sensor 3 (laser particle count-
switching magnetic fields through the sensing surface.
ing sensor), and a patch maker as outlined in the following
7.2.2.1 Sensor 2 performs a time-resolved-dielectric-
paragraphs.Thecoreanalyzerconnectsdirectlytothebalance,
permittivity measurement involving 360 separate measure-
orbital viscometer, and computer application. In addition, it
ments taken at 0.5s intervals covering a total elapsed test time
creates filter patches for wear debris analysis (WDA) classifi-
of 3min. During the first 2min, the switching electromagnet
cation and WDA severity determination.
produces alternating axial-field and then radial-field patterns
7.2.1 Sensor 1 includes a concentric-shell-type-capacitor
which orient and re-orient ferrous particles on the sensor
dielectric permittivity measurement sensor. Test fluid is in-
surface at 0.5s intervals, synchronous with the sequential
jected into a port and pushed up around the annular space
dielectric permittivity measurements. After 2min, the field
betweenacentralmetalelectrodeandtheelectricallygrounded
patternsaremodifiedtodrawferrousdebrisentirelyawayfrom
outer metal shell. By filling the cavity from the bottom, air is
the concentric-trace-type capacitor sensor. The maximum fer-
rous concentration on the sensor is detected at the end of 240
Thesolesourceofsupplyoftheapparatusknowntothecommitteeatthistime
measurements (2min) and the maximum non-ferrous particle
is A520010 Comprehensive Minilab, apparatus, and accessories, available from
and water concentration is detected at the end of 360 measure-
Machinery Health Management, Emerson Process Management, 835 Innovation
Drive, Knoxville, TN 37932. ments (3min). After the test sequence is completed, the
D7416 − 09 (2020)
orbital viscometer constantly pulls air around the electromag-
net coils to keep the orbital viscometer from self heating. The
computer application software processes and controls the
orbitalviscometer,andusestheviscosity-temperaturerelation-
ship as defined in Test Method D341 to translate values from
room temperature absolute viscosity (mPa × s) into 25°C
absoluteviscosity(mPa×s)andinto40°Ckinematicviscosity
(mm /s). To do this, the application software uses laboratory
measured values from its new oil database: specific gravity,
kinematicviscosityat40°C,andkinematicviscosityat100°C.
NOTE 1—The viscosity measurement is performed at room temperature
and converted to 40°C using calculation based on user supplied new oil
information.
7.4 Microscope—A microscope enables the operator to
perform analytical wear debris analysis of 25mm diameter
filter patches. As a minimum the microscope shall provide
FIG. 2 Cross Section View of Orbital Viscometer
viewing stage with top-lighting and magnification from 30× to
230×. The microscope imaging system is standardized on the
computer display (pixels per micron) using application soft-
electromagnet coils are pulsed through a demagnetization or
ware and a captured image from a NIST traceable length
degaussing sequence so that ferrous debris are easily flushed
standard (see 12.5).
away during cleaning.
7.2.2.2 The concentric-trace-type-capacitor dielectric per-
7.5 Computer Application Software—The computer appli-
mittivity measuring sensor is constructed using gold plated
cation software provides the functionality for the particular
copper traces on a ceramic-fiber reinforced PTFE (polytetra-
five-part integrated tester: an electronic user interface, hierar-
fluoroethylene) substrate with a grounded metal backplane.
chical equipment database to store and analyze and manage
The sensor is calibrated to within 62% of standard values for
data, step-by-step testing guide, imbedded logic for data
standardization fluids A, B, and C.
interpretation, and automatic reporting tools.
7.2.2.3 The dual-coil electromagnet is used to collect and
7.6 Solvent Filtration Device—This device is used for
manipulate ferrous debris on the sensor surface. The dual-coil
dispensingthedilutingandcleaningsolvents.Thedevicefilters
electromagnet produces –300G 6 30G field strength on the
solvents from the pressurized dispenser by passing the fluid
sensor surface above the center-post when both coils are
through a 0.8µm (typical) filter patch.
powered with fields adding, and it produces 70G 6 2G field
strength when the magnets when the polarity of the outer coil
8. Reagents and Materials
is reversed so it effectively overpowers the inner coil. These
8.1 Disposable Luer-tip 10 mL Syringes—Syringes shall be
relative field strengths allow the analyzer to gather ferrous
supplied individually wrapped to prevent contamination. Sy-
debris above the center-post, orient ferrous debris in axial and
ringes are all plastic with no rubber seals on plunger. Rubber
radial geometric pattern, and sweep ferrous debris off the
materialsmayhavematerialcompatibilityproblemswithsome
sensor surface.
solvents. Syringes are not reusable.
7.2.3 Sensor 3 includes a laser particle counting sensor
8.2 Disposable Luer-tip 30 mL Syringes—Syringes shall be
mounted immediately below a Luer-tip injection port. Sample
test fluid is diluted, homogenized, drawn into 30mL syringe, supplied individually wrapped to prevent contamination. Sy-
degassed, and then injected via the Luer-tip port through the ringes are all plastic with no rubber seals on plunger. Rubber
laser window. Flow rate through the particle counter is main- materialsmayhavematerialcompatibilityproblemswithsome
tained at constant 50mL⁄min using a stepper-motor controlled solvents. Syringes are not reusable.
syringe pump. Sensor 3 is standardized using MTD standard-
8.3 Cleaning and Diluting Solvent—Sensors 1, 2, and 3 are
ization fluid in accordance with ISO 11171.
all cleaned using a solvent that is soluble with the base oils
7.3 Orbital Viscometer—The orbital viscometer measures tested. See Table 1 for oil and solvent solubility. Fluids A, B,
absoluteviscosity,alsocalleddynamicviscosity,ataparticular and C are standardization fluids. See 12.2.1.
temperature in units of centigrade (°C). A cross section of the
8.4 WaterMaskingSolvent—Watermaskingeliminatesfalse
orbital viscometer is shown in Fig. 2. The ~12mLsample test
particle count interference from water droplets.Water masking
cup is filled with test fluid and contains a steel ball that orbits
solvents are selected to dissolve water-in-oil. See Table 2 for
around the base of the test cup under the influence of four 5,11
water masking solvent materials and procedures.
sequentially powered electromagnets. Under the circular path
8.5 Filter Patches—The WDA filter patches are 25mm
of the ball are four ball-position sensors. Each time the ball
diameter circular patches with ~5µm pore size or another pore
passes over one sensor, the next electromagnet is energized,
thereby
...