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: D8184 − 18´1

Standard Test Method for

Ferrous Wear Debris Monitoring in In-Service Fluids Using a
Particle Quantifier Instrument1
This standard is issued under the fixed designation D8184; 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.

ε1 NOTE—A Research Report footnote was added editorially in June 2019.

1. Scope D4177 Practice for Automatic Sampling of Petroleum and

1.1 This test method describes the use of offline particle Petroleum Products
quantification (often referred to as PQ) magnetometers to trend D5185 Test Method for Multielement Determination of
wear rates in machinery by monitoring the amount of ferro- Used and Unused Lubricating Oils and Base Oils by
magnetic material suspended in a fluid sample that has been in Inductively Coupled Plasma Atomic Emission Spectrom-
contact with the moving parts of the machinery. It is particu- etry (ICP-AES)
larly relevant to monitoring wear debris in lubricating oils and D6300 Practice for Determination of Precision and Bias
greases. Data for Use in Test Methods for Petroleum Products and
Lubricants
1.2 The values stated in SI units are to be regarded as D7720 Guide for Statistically Evaluating Measurand Alarm
standard. Values of the burden (mass) of ferrous wear debris in Limits when Using Oil Analysis to Monitor Equipment
the sample are reported as a PQ Index. The PQ Index is a and Oil for Fitness and Contamination
numerical value that scales with the ferrous debris burden.
1.3 This standard does not purport to address all of the 3. Terminology
safety concerns, if any, associated with its use. It is the 3.1 Definitions:
responsibility of the user of this standard to establish appro-
3.1.1 condition monitoring, n—the recording and analyzing
priate safety, health, and environmental practices and deter-
of data relating to the condition of equipment or machinery for
mine the applicability of regulatory limitations prior to use.
the purpose of predictive maintenance or optimization of
1.4 This international standard was developed in accor-
performance.
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the 3.1.2 ferromagnetic, n—metals, alloys, and other materials
Development of International Standards, Guides and Recom- that exhibit medium to high magnetic permeabilities; further
mendations issued by the World Trade Organization Technical classified into “hard” and “soft” magnetic materials when
Barriers to Trade (TBT) Committee. capable of becoming permanently magnetized or not, respec-
tively.
2. Referenced Documents 3.1.3 inductively coupled plasma optical emission spectros-
2.1 ASTM Standards:2 copy (ICP-OES), n—a form of emission spectroscopy that uses
D4057 Practice for Manual Sampling of Petroleum and a plasma to excite atoms and ions that subsequently emit
Petroleum Products electromagnetic radiation in the visible region; the emission
D4175 Terminology Relating to Petroleum Products, Liquid wavelengths are characteristic of a particular wavelength, and
Fuels, and Lubricants the intensity of emission is related to the concentration of the
emitting element.
3.1.4 machinery health, n—qualitative indication of the
1
This test method is under the jurisdiction of ASTM Committee D02 on overall condition of equipment or machinery; may depend on
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.96.06 on Practices and Techniques for Prediction and Determi-
data and trend analysis from several sources.
nation of Microscopic Wear and Wear-related Properties. 3.1.5 PQI, n—a dimensionless index related to the ferro-
Current edition approved May 15, 2018. Published June 2018. DOI: 10.1520/
magnetic content of an oil or grease sample.
D8184-18E01.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
3.1.5.1 Discussion—The scale is defined by a 750 PQI
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on primary standard developed by The University of Swansea in
the ASTM website. the 1980s. The original primary standard is currently in the

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

Copyright ASTM International

Provided by IHS Markit under license with ASTM
1Licensee=Enex Chile S.A./5985366001, User=Ruiz, Francisco
No reproduction or networking permitted without license from IHS Not for Resale, 05/04/2020 11:24:56 MDT
 D8184 − 18´1
possession of Parker Hannifin Manufacturing Ltd. debris burden within periodically extracted samples as re-
(Littlehampton, UK) who manufacture and supply secondary flected in the PQ Index.
standards for instrument validation purposes. 5.3 PQ measurements can be used as a means of rapidly
3.1.6 rotating disc electrode optical emission spectroscopy screening samples for the presence or absence of ferrous wear
(RDE-OES), n—similar to ICP-OES, but the exciting medium debris, allowing quick decisions to be made on whether or not
is now an electrical discharge between an electrode and a to proceed to a more detailed spectroscopic analysis for
rotating disc with the oil sample located within the discharge. probable wear metals in the sample.
3.1.7 trend analysis, n—the interpretation of regular or 5.4 The use of standardized sample containers and a con-
continuous (in time) condition monitoring data in order to sistent protocol enables reliable trending information to be
determine any changes indicative of deterioration or incipient recorded. Although it is not possible to assign general limits or
failure in equipment or machinery. thresholds for abnormal conditions, it is recommended that
3.1.8 wear, n—the loss of material from a surface, generally interpretation of PQ values should be carried out in consulta-
occurring between two surfaces in relative motion, and result- tion with historical data, equipment logs, and/or service history
ing from mechanical or chemical action, or a combination of in order to formulate guidelines on individual items of machin-
both. ery. Guide D7720 is particularly useful in this context.
4. Summary of Test Method 6. Interferences
4.1 Lubricating Oils—A sample of oil is extracted from the 6.1 Sample Related Interferences:
machinery and collected in a bottle to a depth sufficient to 6.1.1 PQ instruments have a high sensitivity to the presence
exceed the flux field of the sensing coil in the instrument. of low concentrations of ferromagnetic materials in the test

--``,,`,,``,,,,`,,,```,,``````,-`-`,,`,,`,`,,`---
Distortion of the flux field due to the presence of any material (iron, steel, and so forth) due to their magnetic
ferromagnetic material is determined and a numerical value susceptibility. However, large concentrations of high conduc-
(PQ Index) assigned to the extent of the distortion. This index tivity metals, for example, copper, can cause a small distortion
is related to the concentration and spatial distribution of the to the excitation field through the generation of eddy currents
ferromagnetic material within the sensing volume of the coil. If in the debris particles. These eddy currents generate an
the oil sample has been undisturbed for some time, this is the opposing ac magnetic field to the excitation field (Lenz’s law),
same as the concentration within the bulk. However, if the which causes an imbalance and hence a detectable signal. Note
ferrous burden undergoes settling, for example, from an initial that this phenomenon is several orders of magnitude lower in
well-shaken state, then the signal may exhibit a time depen- effect than that due to the magnetic permeability of ferrous
dency due to debris mobility. It is possible to derive informa- materials. The presence of any suspected high conductivity
tion on the size (mass) of the debris from the rate of any time metal contamination can be verified or eliminated by, for
dependent behavior noted. example, Test Method D5185.
4.2 Greases—A sample of grease is similarly extracted from 6.2 External (Environmental) Interferences:
a bearing housing or similar and transferred to a small volume 6.2.1 As noted in 9.2, the toner material in some printed
(5 mL) pot.3 Reliable trending information requires the use of labels can contain iron powder and care should be taken to
the same size and shape of pot for reasons of consistency. eliminate this interference by careful label positioning and/or
Mobility of debris within grease is restricted, the contents of the use of non-iron containing inks.
the pot are completely within the flux field of the sensing coil, 6.2.2 PQ instruments should not be sited on or close to large
and no time dependent behavior is observed. metallic structures due to the possibility of field distortion
caused by their proximity, see 10.1.
5. Significance and Use
5.1 This test method is intended for the application of PQ 7. Apparatus
magnetometry in assessing the progression of wear in 7.1 PQ instruments are of a propriety design and currently
machinery, for example, engines and gearboxes, by trending manufactured by Parker Hannifin Ltd., Littlehampton, U.K.4,5
the mass of ferrous debris in samples of lubricating oils or The development of PQ test methodology began at Swansea
greases. University in the 1980s. Instruments have been manufactured
5.2 In-service oil analysis is carried out routinely by com- under license, since the initial development, by Swansea Oil
mercial laboratories on a wide range of samples from many Analysis Program (SOAP) Ltd., Analex Ltd., and Kittiwake
sources and is accepted as a reliable means of monitoring Developments Ltd, and a large number are still in operation in
machinery health by trend analysis. In particular, the extent of
wear can be readily assessed from any changes in the ferrous 4
The sole source of supply of the apparatus known to the committee at this time
is Parker Hannifin Ltd., Littlehampton, U.K.. If you are aware of alternative
suppliers, please provide this information to ASTM International Headquarters.
3
The sole source of supply of the apparatus (recommended grease sample pots) Your comments will receive careful consideration at a meeting of the responsible
known to the committee at this time is Parker Hannifin Ltd., Littlehampton, UK. If technical committee,1 which you may attend.
5
you are aware of alternative suppliers, please provide this information to ASTM PQ – GB trademark number 2210262 for “Apparatus and instruments for the
International Headquarters. Your comments will receive careful consideration at a detection and/or quantification of wear debris in lubricating fluids and hydraulic
meeting of the responsible technical committee,1 which you may attend. fluids,” applies to the instrument and not the measurement index.

Copyright ASTM International

Provided by IHS Markit under license with ASTM
2Licensee=Enex Chile S.A./5985366001, User=Ruiz, Francisco
No reproduction or networking permitted without license from IHS Not for Resale, 05/04/2020 11:24:56 MDT
 D8184 − 18´1
many commercial laboratories. Current PQ instruments are 9. Sampling, Test Specimens, and Test Units
marketed and supported globally by Parker Hannifin Ltd. 9.1 In-service oil and grease samples should be collected in
7.2 A description of the apparatus and method can be found accordance with the practices described in Practice D4057 or
in the patents listed in Related Materials. In brief, PQ instru- Practice D4177. Oil samples should be transferred to clean
ments comprise an excitation coil providing an ac magnetic 100 mL bottles or 5 mL pots and sealed (Fig. 3). Grease
field with a frequency between 1 kHz and 10 kHz, two sense samples should be transferred to 5 mL pots and similarly
coils arranged above and below the excitation coil and with the sealed. Suitable containers are available from several manu-
sample sited close to one of the excitation coils. See Fig. 1 and facturers. For oil samples in 100 mL bottles, a minimum fill
Fig. 2 for details. In Fig. 2, 11 and 13 are the sample and a depth of 40 mm is recommended (Fig. 4). The 5 mL pots
support plate, 2 is the excitation coil wound on a former (1), 3 should be completely filled with either oil or grease samples; a
is an oscillator driving this coil, 4 and 5 are the two sense coils consistent approach with respect to sample volume in this step
arranged in a differential manner (initially balanced by some will provide the most reliable results.
means to provide a null signal), with 6 through 8 providing a 9.2 Note that certain printer toners and inks can contain iron
means to detect and amplify any subsequent imbalance in the oxides. If it is required to attach printed labels to sample bottles
two sense coils from the presence of wear debris in the sample. for identification purposes, it is recommended that either the
9 is a display or recording device for this out-of-balance signal. labels are sited well away from the measurement zone or that
7.3 To measure the ferrous burden in a sample in the form the labels be prepared using thermal type printers, in order to
of the PQ index, the response of the instrument must be avoid erroneous measurements.
calibrated against the primary standard. This will have been 9.3 Check standards are available from the manufacturer to
done by the manufacturer who will also supply secondary use as test specimens for day to day validation and confidence
check standards to verify the long-term performance of the checking.
instrument on an appropriate usage schedule. Consult the
manual for guidance on this matter. Note that the sample platter 10. Preparation of Apparatus
also contains an embedded ferrous reference for the purposes
of compensating for any short-term drift. 10.1 PQ instruments are susceptible to variable temperature
effects and the presence of stray magnetic fields. They should
7.4 A full operational cycle consists of three measurements;
be sited in a stable, draft-free environment and kept well away
zero PQI, embedded reference, and finally, the test sample.
from any sources of electromagnetic interference, for example:
This is achieved by rotating the platter on which the sample is
power supplies, generators, microwave ovens, loudspeakers,
placed in a stepwise fashion, pausing at each position to make
and so forth. Note also that the close proximity of large steel or
the appropriate measurement.
iron equipment may also disturb the measurement field and PQ
instruments should not be sited near to gas cylinders or placed
8. Reagents and Materials on steel workbenches.
8.1 No reagents are required in order to determine the PQ 10.2 Sufficient time should be allowed for the instrument to
Index of a sample. warm up and equilibrate after first switch on. The manufactur-
8.2 It is recommended that PQ instruments are regularly ers recommend waiting for a 2 h period before performing
calibrated and their performance monitored using the manu- tests. It is anticipated that most PQ instruments will be left in
facturer’s recommendations and check standards. a “permanently on/standby” state.

FIG. 1 Principle of PQ Magnetometry (left) and a Modern Instrument (right)

--``,,`,,``,,,,`,,,```,,``````,-`-`,,`,,`,`,,`---

Copyright ASTM International

Provided by IHS Markit under license with ASTM
3Licensee=Enex Chile S.A./5985366001, User=Ruiz, Francisco
No reproduction or networking permitted without license from IHS Not for Resale, 05/04/2020 11:24:56 MDT
 D8184 − 18´1

FIG. 2 PQ Instrument Schematic

FIG. 3 A 5 mL Pot (left) and 100 mL Bottle (right)

--``,,`,,``,,,,`,,,```,,``````,-`-`,,`,,`,`,,`---

FIG. 4 Recommended 100 mL Bottle Fill Depth

10.3 In addition, cold sample bottles may affect the instru-

ment when placed on the measurement platter, and they should
also be given sufficient time to equilibrate before performing
measurements.

Copyright ASTM International

Provided by IHS Markit under license with ASTM
4Licensee=Enex Chile S.A./5985366001, User=Ruiz, Francisco
No reproduction or networking permitted without license from IHS Not for Resale, 05/04/2020 11:24:56 MDT
 D8184 − 18´1
11. Calibration and Standardization around during the rotation of the platter. The correct adaptor
11.1 PQ instruments should be regularly recalibrated using should always be used to ensure this, see Fig. 5.
the supplied secondary standards and the procedure detailed in
13. Procedure
the manual to counteract any potential long-term drift.
13.1 Bottle Samples—One recommended procedure is de-
11.2 Note that the rotating platter contains an embedded
scribed below with a further optional procedure for individual
secondary standard. As part of the test cycle, this embedded
laboratories to adapt as required. As noted previously the
standard is repetitively presented to the measurement coil and
laboratory temperature should be stable, preferably to within
used to correct for any short-term drift between cycles.
62 °C.
12. Conditioning and Sample Presentation 13.1.1 Procedure A—This should be carried out within 1 h
of completion of the homogenization step in 12.1. The sample
12.1 For bottle measurements, it is essential that the sample bottle should be shaken vigorously for a minimum of 30 s so as
is well homogenized prior to testing. This is best achieved with to distribute any ferrous wear debris evenly within the bulk and
laboratory shakers, although vigorous manual shaking is ac- then immediately inserted in an inverted manner (lid down-
ceptable. A minimum time of 5 min is recommended, although wards) into the platter aperture. Two repeat measurements
for viscous samples (for example, thick gearbox oils), this should be taken and the average recorded as the PQ index of
should be extended to 10 min. The samples should be tested as the sample.
soon as possible after this homogenization process, preferably 13.1.2 Procedure B—Time dependent PQ. Procedure A may
within 1 h. be adapted if information is required on the mass distribution
12.2 For pot measurements, no sample conditioning is of the sample by recording measurements from the first until
required, however the pot should be completely filled and the PQ value stabilizes. The time (or number of cycles) to
sealed with a cap prior to measurement. achieve this is indicative of the size (mass) of the debris with
larger debris requiring shorter times to settle. Individual
12.3 For accurate and consistent results, it is important that
laboratories should determine if this procedure is useful and
the bottle bottom, or lid if inverted measurements are
experiment with shaking times and measurement cycles as
performed, should be perfectly flat and even. Any exterior pips
required to achieve consistency. Once both of these parameters
or protuberances left over from the manufacturing process
have been defined, a laboratory procedure should be written
should be removed with a sharp knife or similar to ensure a
and all subsequent measurements on received samples should
stable, non-rocking stance. It is worth noting that bottle lids are
follow the same practice. More information is available in
often flatter than the bottle bases, and measurements are more
Jones and Massoudi.6
likely to be consistent when the bottle is inverted in the platter
aperture. Foil-lined lid-sealing inserts should be avoided when 13.2 Pot Samples—With the sample in 5 mL pots, the
carrying out these type of measurements in case of interfer- sample is fully contained within the measurement field of the
ence.
12.4 In addition, the bottle or pot should maintain a con- 6
Jones, M. H., and Massoudi, A. R., “The TDPQ: a solution to the analysis of
centric stance within the measurement aperture and not wander large wear particles,” Insight, Vol 37, 1995, pp. 606–610.

--``,,`,,``,,,,`,,,```,,``````,-`-`,,`,,`,`,,`---

FIG. 5 A 5 mL Pot (left) and 100 mL Bottle (right) with Appropriate Adaptor Rings

Copyright ASTM International

Provided by IHS Markit under license with ASTM
5Licensee=Enex Chile S.A./5985366001, User=Ruiz, Francisco
No reproduction or networking permitted without license from IHS Not for Resale, 05/04/2020 11:24:56 MDT
 D8184 − 18´1
sensing coil and only one procedure is appropriate. It is the methods described in Practice D6300, the following preci-
identical to Procedure A above. Note that multi-stacker acces- sion statements can be written for the three samples:
sories are available to preload multiple pots for automated 16.1.1 Repeatability—The difference between two test re-
measurements on large numbers of samples. sults obtained by the same operator with the same apparatus
under constant operating conditions on identical test material
14. Calculation or Interpretation of Results would, in the long run and in the normal and correct operation
14.1 As noted in the procedures in Section 13, the PQ value of the test method, exceed the following values in only 1 case
to be returned is the average of two repeat measurements and in 20.
no further interpretation is required. Sample Mean Repeatability
Low value 100 4.2
15. Report Medium value 524 20.6
High value 3342 100.1
15.1 Sample PQ values should be reported as a numerical
index in rounded integer format from the average calculated in 16.1.2 Reproducibility—To be determined by a full inter-
Section 14. laboratory study.
16.2 Bias—There is no bias for the values reported in this
16. Precision and Bias7 test method as it is the only test that determines the PQ index
16.1 Procedure A—An interim repeatability study has been of an in-service oil or grease sample.
performed using three samples of iron powder dispersed in
16.3 Precision—The above interim repeatability statement
base oil representing low, medium, and high PQ values. Using
is only available at this time.
7
Supporting data have been filed at ASTM International Headquarters and may 17. Keywords
be obtained by requesting Research Report RR:D02-1901. Contact ASTM Customer
Service at [email protected]. 17.1 ferrous wear debris; oil analysis; PQ Index

APPENDIX

(Nonmandatory Information)

X1. PQ IN PRACTICE

X1.1 Comparison with Iron Concentration from Spectro- discharge as the debris size exceeds a dimensional value of
scopic Determinations some 8 µm to 10 µm. Concentration levels may therefore be
X1.1.1 Iron concentration levels are often determined in the under-reported if the sample contains a significant proportion
laboratory by optical emission spectroscopic methods such as of such larger particles.
ICP-OES or RTD-OES. The following points should be noted X1.1.1.3 From a consideration of X1.1.1.2, if both PQ
when comparing trends in samples tested by PQ instruments values and ppm (by mass) concentrations are available for the
and these methods. same sample (for example, from ICP-OES), we may deduce
X1.1.1.1 OES determines iron in its “atomic” form and does the following approximate classification rules:
not provide any information on the chemical nature of the iron. (1) PQ high, ppm (by mass) low: indicative of large
It is therefore not possible to say if the measured iron content particles (>>10 µm).
can be attributed solely to elemental iron or an iron compound, (2) PQ and ppm (by mass) comparable: indicative of
for example, iron oxide (rust) or a combination of both. PQ medium particles (~10 µm).
instruments respond only to ferromagnetic materials: metallic (3) PQ low, ppm (by mass) high: indicative of small
iron and steel, for example. PQ is therefore more applicable to particles (<<10 µm).
the trending of wear progression patterns in hard bearing
elements, gears, and similar components. X1.2 Typical PQ Values for Different Types of Machinery
X1.1.1.2 Unless the oil sample has been treated to acid and Equipment
digestion, OES techniques have an upper limitation on the size
of the debris particles. This is due to the incomplete vaporiza- X1.2.1 Some guideline limits/values obtained through ex-
tion (atomization) of the particle in either the plasma or the perience with earth moving equipment are given in Table X1.1.

--``,,`,,``,,,,`,,,```,,``````,-`-`,,`,,`,`,,`---

Copyright ASTM International

Provided by IHS Markit under license with ASTM
6Licensee=Enex Chile S.A./5985366001, User=Ruiz, Francisco
No reproduction or networking permitted without license from IHS Not for Resale, 05/04/2020 11:24:56 MDT
 D8184 − 18´1
TABLE X1.1 Guideline PQ ValuesA
Equipment PQ OK PQ Caution PQ Abnormal
Engines <15 15–20 >20
Truck Final Drive <90 90–250 >250
Track Drives <165 165–700 >700
Differential Gears <100 100–200 >200
Transmissions <20 20–30 >30
Hydraulics <15 15–25 >25
A
Data from Machine Plant & Systems Monitor, Jan/Feb 2000, “How to maximize
PQ (particle quantifier) technology”, Ken Burnett, ANALEX International Ltd.

RELATED MATERIAL

Published Patents: GB 2269235 (1994), Wear monitoring by measuring ferromagnetic

The following patents are listed for further information. Note, all have particles in liquid
now expired. US 5404100 (1995), Method of quantifying wear particles in a lubricant
GB 2160655 (1985), Method and apparatus for assessing particle deposits sample

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
--``,,`,,``,,,,`,,,```,,``````,-`-`,,`,,`,`,,`---

if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or [email protected] (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222
Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http://www.copyright.com/

Copyright ASTM International

Provided by IHS Markit under license with ASTM
7Licensee=Enex Chile S.A./5985366001, User=Ruiz, Francisco
No reproduction or networking permitted without license from IHS Not for Resale, 05/04/2020 11:24:56 MDT