INTERNATIONAL ISO

STANDARD 1 1 1 71

Fourth edition
2020-11

Hydraulic fluid power — Calibration o f

automatic particle counters for liquids
Transmissions hydrauliques — Étalonnage des compteurs
automatiques de particules en suspension dans les liquides

Reference number
ISO 11171:2020(E)

© ISO 2020
ISO 1 1 1 71 : 2 02 0(E)

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 ISO 1 1 1 71 : 2 02 0(E)

Contents Page

Foreword ........................................................................................................................................................................................................................................ iv
Introduction ................................................................................................................................................................................................................................ vi
1 Scope ................................................................................................................................................................................................................................. 1
2 Normative references ...................................................................................................................................................................................... 1
3 Terms and definitions ..................................................................................................................................................................................... 1
4 Materials and equipment ............................................................................................................................................................................ 3
5 Sequence o f APC calibration procedures .................................................................................................................................... 5
6 Sizing calibration procedure.................................................................................................................................................................... 9
7 Data presentation ............................................................................................................................................................................................. 1 9
8 Identification statement ............................................................................................................................................................................ 2 0
Annex A (normative) Preliminary APC check .......................................................................................................................................... 2 1
Annex B (normative) Coincidence error procedure .......................................................................................................................... 2 5
Annex C (normative) Flow rate limit determination ........................................................................................................................ 2 9
Annex D (normative) Resolution determination .................................................................................................................................. 3 4
Annex E (normative) Verification o f particle-counting accuracy ........................................................................................ 3 9
Annex F (normative) Preparation and verification o f bottles o f secondary calibration
suspensions ............................................................................................................................................................................................................ 42
Annex G (normative) Dilution o f calibration suspension samples .................................................................................... 46
Annex H (informative) Verification o f particle size distribution o f calibration samples ........................... 49
Bibliography ............................................................................................................................................................................................................................. 5 1

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Foreword
ISO (the International Organization for Standardization) is a worldwide federation o f national standards
bodies (ISO member bodies). The work o f preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters o f
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular, the di fferent approval criteria needed for the
di fferent types o f ISO documents should be noted. This document was dra fted in accordance with the
editorial rules o f the ISO/IEC Directives, Part 2 (see www.iso .org/directives).
Attention is drawn to the possibility that some o f the elements o f this document may be the subject o f
patent rights. ISO shall not be held responsible for identi fying any or all such patent rights. Details o f
any patent rights identified during the development o f the document will be in the Introduction and/or
on the ISO list o f patent declarations received (see www.iso .org/patents).
Any trade name used in this document is in formation given for the convenience o f users and does not
constitute an endorsement.
For an explanation o f the voluntary nature o f standards, the meaning o f ISO specific terms and
expressions related to con formity assessment, as well as in formation about ISO's adherence to the
World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see www.iso .org/
iso/foreword .html.
This document was prepared by Technical Committee ISO/TC 131 Fluid power systems, SC 6,
Contamination control .
This fourth edition cancels and replaces the third edition (ISO 11171:2016), which has been technically
revised.
The main changes compared to the previous edition are as follows:
— Clause 1 and 4.4: SRM 2806b are not used for sizing calibration purposes with this document;
— 3.1: the definition o f an automatic particle counter (APC) is clarified;
— 3.8 (Note 1 to entry): the particle size distribution for primary calibration suspension samples is
found in Table 3 of the SRM 2806x Certificate of Analysis;
— 4.6: ISO medium test dust (MTD) or other test dust con forming to ISO 12103-1 for secondary
calibration suspension is permitted;
— 4.8: APC are required to have a minimum o f 8 channels that can be set instead o f only 6;
— 6.1: latex spheres are required for primary calibration at particle sizes greater than 30 µm(c);
— 6.1: secondary calibration suspensions can be used for secondary calibration at particle sizes
greater than 30 µm(c);
— 6.2: both re ference and certified data from the SRM 2806x particle size distribution are used for
primary sizing calibration;
— 6.2: data from at least 16 di fferent particle sizes taken from the certified particle size distribution
are used to create the APC calibration curve;
— 6.3: data obtained from at least 12 di fferent APC threshold voltage settings are used to relate
particle concentrations to threshold settings;

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— 6.6: the data acceptance criteria are based upon the mean number o f particles counted rather than
particle concentration;
— 6.6: dilution o f calibration suspensions is permitted to allow the calibration o f APCs at sizes that
would otherwise be in coincidence error for calibration suspensions;
— 6.9: the constrained cubic spline method o f interpolation is specified and a tool for its use to relate
threshold voltage setting to particle size is provided;
— 6.9: the standard uncertainty in particle concentration at each threshold setting is calculated and
reported;
— 6.11 – 6.14: the modified di fferential hal f-count method for relating particle size and threshold
setting using latex spheres is specified for primary calibration o f particle sizes greater than 30 µm(c);
— 6.15: the constrained cubic spline method o f interpolation is specified for relating threshold voltage
setting to particle size and a tool for its use to relate threshold voltage setting to particle size and to
construct an APC calibration curve is provided;
— Clause 7: the only acceptable way o f reporting particle size using this document is using the unit
o f µm(c);
— Table A.1: the median, upper and lower acceptable particle concentration limits have been updated
based on the results o f interlaboratory testing using RM 8632a test dust and calculated based upon
the logarithm o f the observed particle counts and 98 % confidence level;
— Table C.2: acceptable values for DQ are based upon the mean number o f particles counted rather
than particle concentration;
— F.2 : use of NIST RM 8631x, ISO MTD, or other test dust con forming to ISO 12103-1 for secondary
calibration suspensions is permitted and the maximum allowable concentration for secondary
suspensions is increased from 75 % to 100 times the coincidence error limit o f the sensor;
— F.4 and F.7: data are obtained from at least 16 di fferent particle sizes and reported in the certificate
o f analysis for the resultant secondary calibration suspensions;
— Annex G: this new annex specifies the method o f dilution for calibration suspension samples for use
in 6.6 for samples that would otherwise be in coincidence error;
— Annex H, Sample calculations, from ISO 11171:2016: deleted. Replaced by Annex H, Verification o f
particle size distribution o f calibration samples.
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing o f these bodies can be found at www.iso .org/members .html.

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Introduction
In hydraulic fluid power systems, power is transmitted and controlled through a liquid under pressure
within an enclosed circuit. The fluid is both a lubricant and a power-transmitting medium. Reliable
system per formance requires control o f the contaminants in the fluid. Qualitative and quantitative
determination o f the particulate contaminants in the fluid medium requires precision in obtaining
the sample and in determining the contaminant particle size distribution and concentration. Liquid
automatic particle counters (APC) are an accepted means o f determining the concentration and size
distribution o f the contaminant particles. Individual APC accuracy is established through calibration.
This document is a standard calibration procedure for APC that are used for determining particle sizes
and counts. The primary particle-sizing calibration is conducted using NIST SRM 2806x suspensions with
particle size distribution certified by the United States National Institute o f Standards and Technology
(NIST) for particle sizes 30 µm(c) and smaller, and using polystyrene latex spheres at larger sizes.
A secondary calibration method uses suspensions o f NIST RM 8631x, ISO MTD, or other test dust
con forming to ISO 12103-1, which are independently analysed using an APC calibrated by the primary
method. Minimum per formance specifications are established for the APC coe fficient o f variation (CV)
o f sample volume, CV o f flow rate, resolution and particle counting accuracy. The operating limits o f an
APC, including its threshold noise level, coincidence error limit and flow rate limits are determined.

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INTERNATIONAL STANDARD ISO 1 1 1 71 : 2 02 0(E)

Hydraulic fluid power — Calibration o f automatic particle

counters for liquids
1 Scope
This document specifies procedures for the following:
a) primary particle-sizing calibration for particle sizes 1 µm(c) and larger, sensor resolution and
counting per formance o f liquid automatic particle counters that are capable o f analysing bottle
samples;
b) secondary particle-sizing calibration using suspensions verified with a primary calibrated APC;
c) establishing acceptable operation and per formance limits;
d) veri fying particle sensor per formance using a test dust;
e) determining coincidence and flow rate limits.
This document is applicable for use with hydraulic fluids, aviation and diesel fuels, engine oil and
other petroleum-based fluids. This document is not applicable to particle-sizing calibration using
NIST SRM 2806b primary calibration suspensions.

2 Normative references
The following documents are re ferred to in the text in such a way that some or all o f their content
constitutes requirements o f this document. For dated re ferences, only the edition cited applies. For
undated re ferences, the latest edition o f the re ferenced document (including any amendments) applies.
ISO 3722, Hydraulic fluid power — Fluid sample containers — Qualifying and controlling cleaning methods
ISO 4787, Laboratory glassware — Volumetric instruments — Methods for testing o f capacity and for use
ISO 5598, Fluid power systems and components — Vocabulary
ISO 12103-1, Road vehicles — Test contaminants for filter evaluation — Part 1: Arizona test dust
ISO 16889, Hydraulic fluid power — Filters — Multi-pass method for evaluating filtration performance of
a filter element

3 Terms and definitions

For the purposes o f this document, the terms and definitions given in ISO 5598 and the following apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https://www.iso .org/obp
— IEC Electropedia: available at http://www.electropedia .org/
3 .1
automatic particle counter
APC
instrument that automatically:

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a) senses individual particles suspended in a controlled volume o f fluid using optical light extinction
or light scattering principles;
b) measures the size o f particles;
c) sorts or compiles particles into size ranges;
d) counts particles in each size range;
e) reports the number o f particles in each size range per unit volume; and
f ) acilitates instrument calibration according to this document.
f

Note 1 to entry: APC used for particle size (3.7) determination with hydraulic fluids, aviation and diesel fuels,
engine oil and other petroleum-based fluids shall be calibrated in accordance with Clause 5 of this document.
3.2
threshold noise level
minimum voltage setting o f an APC (3.1) at which the observed pulse-counting frequency does not
exceed 60 counts/min due to electrical noise in the absence o f flow in the sensing volume (3.3 )
Note 1 to entry: The Brownian motion o f any detectable particles in the sensing zone during per formance o f
subclause A.2 can result in erratic results.
3.3
sensing volume
portion o f the illuminated region o f the sensor through which the fluid stream passes and from which
the light is collected by the optical system
3 .4
resolution
measure o f the ability o f an APC (3.1) to distinguish between particles o f similar, but di fferent, sizes as
determined in accordance with Annex D of this document
3.5
coincidence error limit
highest concentration o f NIST RM 8632x that can be counted with an automatic particle counter (3.1)
with an error o f less than 5 % resulting from the presence o f more than one particle in the sensing
volume (3.3) at one time

3 .6
working flow rate
flow rate through the sensor used for sample analysis
3 .7
particle size
projected area equivalent diameter o f particles as determined by NIST using scanning electron
microscopy traceable to SI units through a NIST length standard or using a liquid optical single particle
APC (3.1) calibrated according to this document

Note 1 to entry: NIST uses scanning electron microscopy to determine the projected area equivalent diameter
o f particles in NIST standard re ference material 2806x, where x is the letter used by NIST to designate the batch
number o f the certified primary calibration (3.9 ) suspension.

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3.8
particle size distribution
cumulative number concentration o f particles larger than a specified size, expressed as a function o f
(3.7 )
particle size

Note 1 to entry: A certified particle size distribution is one provided by a producer o f primary (3.9 ) or secondary
calibration (3.10) suspensions, and certifies that the particle size distribution reported for the suspensions was
determined by NIST or determined according to Annex F o f this document. The particle size distribution o f SRM
2806x used for primary calibrations (3.9) shall consist o f the Diameter [µm(c)] and corresponding Number o f
Particles > Diameter (part/mL) given in columns 1 and 3 o f Table 3 o f the Certificate o f Analysis for Standard
Re ference Material® 2806x[5] .
Note 2 to entry: Verification o f particle size distribution o f calibration samples is detailed in Annex H of this
document.
3 .9
primary calibration
sizing calibration conducted according to the sizing calibration procedure specified in Clause 6 of this
document using NIST standard re ference material 2806x for particle sizes (3.7) 30 µm(c) and smaller,
and using polystyrene latex spheres at larger sizes
Note 1 to entry: For details o f NIST standard re ference material 2806x, see 4.4 .
3 .10
secondary calibration
sizing calibration conducted using secondary calibration suspensions
Note 1 to entry: The sizing calibration procedure is specified in Clause 6 and the preparation o f secondary
calibration suspensions is set out in Annex F.
3 .11
multi-channel analyser
MCA
electronic device capable o f sorting incoming electric pulses according to their amplitude

4 Materials and equipment

4.1 Polystyrene latex spheres that:
a) are in aqueous suspension;
b) have a nominal diameter o f:
1) 10 µm i f used for resolution determination in accordance with Annex D;
2) larger than 30 µm for particle size calibration in accordance with Clause 6 for particle sizes o f
larger than 30 µm;
c) have a coe fficient o f variation that is less than 5 % where the coe fficient o f variation is the ratio
o f the standard deviation o f the latex particle diameters in the suspension to their mean particle
diameter;
d) have a certificate o f analysis that indicates that the latex spheres mean particle diameter and
coe fficient o f variation were determined using techniques with traceability to national standards.
Once opened, suspensions o f polystyrene latex spheres shall be used within three months unless the
size distribution and cleanliness o f the suspension have been verified.
NOTE 1 The size distribution o f polystyrene latex spheres can be verified using the method described in D.14 .
NOTE 2 Polystyrene latex spheres in aqueous suspension have a limited shel f li fe. Shel f li fe is a function o f a
variety o f factors including temperature and microbial contamination o f the suspension.

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4.2 Clean diluent, consisting o f the test liquid used in ISO 16889 and containing:
a) an antistatic additive at such a concentration that resultant conductivity o f the clean diluent is
(2 500 ± 1 000) pS/m at room temperature; and
b) less than 0,5 % o f the number concentration o f particles equal to or larger than the smallest particle
size o f interest expected to be observed in the samples.

4.3 Clean aerosol OT diluent, for use in calibration for particle sizes greater than 30 µm(c) and to
determine sensor resolution in Annex D (the clean diluent specified in 4.2 is used for all other operations
in this document), which:
a) is prepared from a concentrate made by adding 120 g o f aerosol OT to each litre o f clean diluent
(4.2), which is:
1) heated to approximately 60 °C and stirred until no undissolved aerosol OT is visible to the
eye; and
2) diluted with clean diluent (4.2) to a final concentration o f 12 g o f aerosol OT per litre; and
b) meets the same cleanliness levels as the diluent specified in 4.2 .
Aerosol OT (dioctyl sul fosuccinate, sodium salt) is a waxy, hygroscopic solid. I f it appears damp, or has
absorbed water prior to use, dry it first for at least 18 h at approximately 150 °C.
NOTE In 4.3 a) 1), it is critical that all o f the aerosol OT be dissolved prior to proceeding to 4.3 a) 2).
Depending upon the local conditions, complete dissolution can require in excess o f 6 hours o f heating and stirring
as described.
WARNING — Follow the precautions for sa fe handling and usage described in the sa fety data
sheet (available from the supplier o f the aerosol OT).

4.4 NIST standard reference material 2806x (SRM 2806x) primary calibration suspension ,
where x is the letter used by NIST to designate the batch number o f the certified primary calibration
suspension available from NIST, for use in primary calibrations. SRM 2806b shall not be used for
calibrations according to this document.

4.5 NIST re ference material 8631x (RM 8631x) dust, where x is the letter used by NIST to designate
the batch number o f the re ference material, available from NIST, prepared by drying the dust for at least
18 h at a temperature between 110 °C and 150 °C, for use i f secondary calibration is to be performed
(see 6.1 ).
4.6 ISO medium test dust (MTD) or other test dust con forming to ISO 12103-1, dried for at least
18 h at a temperature between 110 °C and 150 °C be fore use, for use i f secondary calibration is to be
performed (see 6.1 ).
4.7 NIST re ference material 8632x (RM 8632x) dust, where x is the letter used by NIST to designate
the batch number o f the re ference material, prepared by drying the dust for at least 18 h at a temperature
between 110 °C and 150 °C, be fore use, required for determination o f coincidence error limit and in
Annexes A, B, C and E.
NOTE The re ference materials specified in 4.4, 4.5, 4.6 and 4.7 can change as new batches are produced. Such
a change does not a ffect the particle sizing calibration (Clause 6), but the ability o f an APC to meet the counting
accuracy requirements o f E.9 can be a ffected i f the batch o f RM 8632 x used to prepare the samples di ffers from
the batch used to create Table A.1 .

4.8 Automatic particle counter for liquids , with bottle sampler with at least 8 channels that can be
set at various threshold settings.

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4.9 Clean sample containers , with closures (appropriate bottle caps, for example), and volumetric
glassware o f at least class B accuracy as defined in ISO 4787, with cleanliness levels lower than 0,5 % o f
the number o f concentration o f particles (larger than the smallest particle size o f interest) expected to be
observed in the samples, confirmed in accordance with ISO 3722.

4.10 Mechanical shaker, such as a paint or laboratory shaker, suitable for dispersing suspensions.

4.11 Ultrasonic bath, with a power density o f 3 000 W/m 2 to 10 000 W/m 2 o f bottom area.

4.12 Linear-linear graph paper or computer so ftware, for generating graphics.

4.13 Log-log graph paper or computer so ftware, for generating graphics.

4.14 Analytical or electronic balance, with the following minimum specifications:

a) readability: 0,01 mg;
b) accuracy (agreement with true mass): ±0,05 mg;
c) precision (repeatability): 0,05 mg;
d) ront or side doors and a covered top to eliminate the e ffect o f air currents.
f

4.15 Secondary calibration suspension , prepared according to Annex F for use in secondary
calibrations. Secondary calibration samples shall not be used for primary calibrations.

5 Sequence o f APC calibration procedures

5 .1 Conduct the procedures o f this Clause when a new APC is received or following the repair or re-
adjustment o f an APC or sensor as shown in Table 1 . See Figure 1 for a recommended sequence o f steps
to be followed when performing a full calibration on a new APC. Annexes A and B shall be performed
prior to proceeding to Clause 6. Proceed to Clause 6 if neither the APC nor the sensor has been repaired
or readjusted, i f no detectable change in the operating characteristics has occurred since the last sizing
calibration was performed, and i f the APC has been subjected to the procedures in Annexes A, B, C , D,
and E and the results have been documented. The specific order o f annexes and clauses given in Figure 1
and Table 1 are recommendations. The operator may follow a di fferent order, as long as all required
parts are performed.
Annexes A, B, C , D and E may be per formed by an individual laboratory or by the manu facturer o f the
APC prior to delivery. I f these are per formed prior to delivery, it is not always required to repeat these
annexes upon receipt o f the APC, depending upon the manu facturer's recommendations.
NOTE For the purposes o f this subclause, repair or readjustment o f an APC re fers to service or repair
procedures that a ffect the ability o f the APC to accurately size and count particles.

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Figure 1 — Recommended sequence o f APC calibration procedures

A change in the operating characteristics o f the APC can be detected by several di fferent methods,
including but not limited to the following:
a) using particle data from control samples collected over time and a statistical process control chart,
such as an individual moving range (IMR) chart, to detect significant changes in calibration;
b) comparing calibration curves reporting particle size in units o f µm(c) over time to detect a
significant change in calibration;
c) returning the APC to its manu facturer for evaluation and assessment o f the change in calibration;

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d) analysing a primary or secondary calibration suspension in accordance with 6.5 through 6.7, then
comparing the resulting particle concentration data to the corresponding particle size distribution
for the sample:

1) i f the results agree within the limits for the maximum allowable D Q (6.6 ) given in Table C.2, the
ability o f the APC to size and count particles has not been significantly a ffected;
2) i f the results do not agree, a significant change has occurred, so proceed as indicated in Table 1 .
e) determining the threshold noise level o f the APC in accordance with A.2 , then comparing the
resulting noise level to previously obtained results. I f the threshold noise level has increased by
more than 30 % since the last time it was determined, this can be an indication that the calibration
o f the APC has changed and the APC is in need o f repair. I f the threshold noise level has not changed,
this is not proo f that the APC's operating characteristics are unchanged.
I f the light source or any part o f the optics is adjusted, repaired or replaced, repeat the procedures o f
Clause 6 and Annexes A, B, D , and E.
I f the sensor or counting electronics is adjusted, repaired or replaced, repeat the procedures o f Clause 6
and Annexes A, B, C , D , and E.
I f the volume measurement system is repaired, replaced or re-adjusted, the procedures o f A.3 to A.9
and o f Annex C shall be per formed.
It is not necessary to repeat these procedures following normal cleaning procedures, the attachment o f
cables or peripheral equipment, the replacement o f plumbing lines or connections, or following other
operations that do not involve disassembly o f the APC, sensor or volume measurement system.

5 .2 Perform the preliminary APC check, which includes volume accuracy, in accordance with Annex A.

5 .3 Determine the coincidence error limits o f the APC in accordance with Annex B .

5 .4 Perform the sizing calibration procedure in accordance with Clause 6 .

5 .5 Determine the flow rate limits o f the APC in accordance with Annex C .

5 .6 Determine the APC resolution in accordance with Annex D .

5 .7 Veri fy the particle-counting accuracy in accordance with Annex E .

5 .8 In order to con form to the requirements o f this document, the APC shall:
a) be calibrated in accordance with 5.4;
b) meet the volume accuracy, resolution and sensor per formance specifications determined in 5.2, 5.6
and 5.7;
c) be operated using the calibration curve determined in accordance with 5.4 within the coincidence
error and flow rate limits determined in accordance with 5.3 and 5.5 .

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 Table 1 — Schedule o f APC calibration procedures
8

ISO 1 1 1 71 : 2 02 0(E)
Relevant clause or annex o f this document to be per formed
Clause 6 Annex A Annex B Annex C Annex D Annex E
APC status a Sizing
Preliminary Coincidence Flow rate
calibration Resolution Accuracy
APC check error limits limits
procedure
New APC or existing APC not calibrated to this Per form Per form Per form Per form Per form Per form
document procedure procedure procedure procedure procedure procedure
Last calibration was more than 6 m to 12 m ago Per form Not required Not required Not required Not required Not required
procedure
Suspicion that calibration has changed significantly Per form Not required Not required Not required Not required Not required
procedure
Optics (including light source) repaired or readjusted Per form Per form Per form Not required Per form Per form
procedure procedure procedure procedure procedure
Sensor or counting electronics repaired or readjusted Per form Per form Per form Per form Per form Per form
procedure procedure procedure procedure procedure procedure
Volume measurement components (e.g. flow meter, Not required Per form Not required Per form Not required Not required
burette, level detectors) repaired or readjusted procedure procedure
Sensor cleaned No action necessary
Cables or peripheral equipment attached No action necessary
Plumbing lines and connections replaced No action necessary
Operation per formed that does not involve disassembly No action necessary
o f APC, sensor or volume measurement system
a Repair or re-adjustment re fers only to service or repair procedures that a ffect the ability o f the APC to accurately size and count particles. In order to veri fy the ability o f
an APC to accurately size and count particles, analyse a primary or secondary calibration suspension in accordance with 6.5 through 6.7, then compare the resulting particle
concentration data to the corresponding particle size distribution for the sample. I f the results agree within the limits given for the maximum allowable D Q in Table C.2, the ability
o f the APC to size and count particles has not been significantly a ffected. I f the results do not agree, proceed as indicated in this Table.
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6 Sizing calibration procedure

6.1 Conduct the sizing calibration set out in Figure 2 every three to six months, when a new APC is
received, or after the repair or re-adjustment o f an APC or sensor. After a suitable calibration history
for an APC and sensor has been developed, the time interval between successive calibrations can be
increased, but shall not exceed one year. For particle sizes 30 µm(c) and smaller, use NIST calibration
suspensions (see 4.4) for primary calibrations or secondary calibration suspensions (4.15) prepared
in accordance with Annex F for secondary calibrations. For particle sizes larger than 30 µm(c), use
polystyrene latex spheres (see 4.1) for primary calibrations or use secondary calibration suspensions
prepared in accordance with Annex F for secondary calibrations.
Conduct all phases o f the calibration at the same working flow rate. Determine the flow rate limits o f
the APC in accordance with Annex C. Discard any data obtained at flow rates outside these limits and
repeat the corresponding part o f the procedure using the proper flow rate.
Conduct the sizing calibration using the same sample volume used in 5.2. I f a di fferent volume is used,
repeat the procedure in 5.2 using the new sample volume to avoid volume measurement errors.
Determine the threshold noise level o f the APC using the method in A.2 before proceeding to 6.2 .
Proceed to 6.2 to calibrate for particle sizes smaller than or equal to 30 μm(c) and for secondary
calibrations for particles larger than 30 μm(c) using samples prepared in full con formance with Annex F.
The procedure described in 6.2 through 6.10 shall not be used for primary calibration at particle sizes
larger than 30 μm(c). Proceed to 6.11 for primary calibration at particle sizes larger than 30 μm(c). The
procedure described in 6.11 through 6.14 shall not be used for particle sizes 30 μm(c) and smaller.
The procedure described in 6.2 to 6.15 assumes manual calibration of an APC with at least 8 channels
that can be set at various threshold settings. Alternatively, calibration can be per formed using a multi-
channel analyser (MCA) or so ftware that follows the same procedure. I f an MCA is used, the relationship
between the measured voltage o f the MCA and the APC threshold setting shall be established. In general,
so ftware and MCA methods tend to be faster and more accurate than manual methods.

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Figure 2 — Sizing calibration procedure

6.2 Choose at least 16 di fferent particle sizes from those listed in the certified particle size distribution
o f the calibration suspension samples. The smallest particle size chosen shall be the smallest particle size
o f interest and the largest particle size shall not exceed 30 μm(c) for primary calibrations and shall not
exceed the largest reported particle size that is in con formance with Annex F for secondary calibrations.
Record these particle sizes and their corresponding particle concentrations from the certified particle
size distribution in the corresponding columns o f the Particle Size Calibration Summary o f Table 4 .

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6.3 Determine a minimum o f 12 di fferent threshold settings to use in constructing a calibration curve.
The first (lowest) threshold setting, J, shall be 1,5 times the threshold noise level o f the APC. The highest
threshold setting, H, shall correspond to a particle size o f approximately 30 μm(c) or less for primary
calibrations and shall correspond to a size that does not exceed the largest reported particle size that
is in con formance with Annex F for secondary calibrations. The value o f constant K shall be calculated
using Formula (1) :
K = 10( log H−log J )/( G−1 ) (1)
where G is the number o f threshold settings to be used to construct the calibration curve. Intermediate
threshold settings between J and H shall be determined such that the value of each intermediate
threshold setting shall be equal to the value o f its preceding channel times K. It is permissible to round
o ff the values o f all threshold settings to the nearest value attainable by the APC, but the values o f
consecutive channels shall not be the same. Record the values determined for the threshold settings in
the first column o f Table 3 .

6.4 Set the APC to the cumulative mode. Using at least eight di fferent channels, set the channels such
that the threshold settings are arranged in order o f increasing voltage. The settings for these channels
shall be selected from the list o f threshold settings previously determined (6.3) and shall be distributed
over this range o f settings.

6.5 Prepare a calibration suspension sample for analysis. Shake the sample vigorously by hand. Agitate
the sample ultrasonically for at least 30 s then shake it on a mechanical shaker for at least 1 min to
disperse the dust in the liquid. Continue shaking the sample until it is to be analysed. De-gas the sample
under vacuum or ultrasonically until no surfacing bubbles are observed then analyse immediately. Obtain
five consecutive particle counts, each consisting o f at least 10 mL and 10 000 particles at the smallest
threshold setting. Record the particle concentrations obtained for each threshold setting for each o f the
five counts in the appropriate cells o f Table 2 .

6.6 Calculate the mean observed number o f particles counted, X, using Formula (2) :
X = X ⋅V (2)
where
X is the mean particle concentration, in particles per millilitre, o f all acceptable counts from the
sample for a particular channel;
V is the sample volume, in millilitres, for a single count.
Calculate the total number, N, o f particles counted for each channel using Formula (3) :
N= 5 X (3)

The value o f N shall be greater than or equal to 1 000 in order to ensure statistically significant results
for that particular channel. The value o f X shall not exceed the coincidence error limit o f the APC (5.3 ).
I f the value o f X exceeds the coincidence error limit, prepare dilutions o f the calibration samples as in
accordance with Annex G and analyse them as described in 6.5 .

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ISO 1 1 1 71 : 2 02 0(E)

Calculate D Q , which is the di fference expressed as a percentage between the minimum, Xmin , and
maximum, Xmax, observed particle concentration for each channel in particles per millilitre, using
Formula (4) :
X max − Xmin
DQ = × 100 (4)
X
Record the threshold voltage setting, particle concentration data, X , and DQ for each channel in the
calibration suspension worksheet in Table 2 for the appropriate sample.
Using Table C.2, find the maximum allowable DQ corresponding to the value of X for each channel. I f the
value o f DQ is less than the maximum, then the value o f X for that channel is acceptable for use. I f there
are at least eight channels with acceptable data, proceed to 6.7. I f not, examine the results o f any
unacceptable channels as follows.
Calculate D0 using Formula (5) :
Xmax − Xmin
D0 = (5)
X0 − XN
where
D0 is the outlier test parameter;
X0 is the observed particle concentration o f the suspected outlier (either Xmax or Xmin) in particles
per millilitre;
XN is the observed particle concentration closest in value to X0 in particles per millilitre.
If D0 for a particular channel is less than 1,44, discard the related outlier data point, X0 , from Table 2,
then recalculate X using the remaining four data points, and use the recalculated value o f X for
calibration purposes. I f D0 for a particular channel is greater than 1,44, all data from this channel are
not acceptable and shall be discarded. I f there are at least eight channels o f acceptable data (using the
DQ and D 0 criteria), proceed to 6.7. I f not, take appropriate corrective action and repeat 6.5 to 6.6 .
If N is less than 1 000 for any channel, do not use the data for that channel. I f su fficient numbers of
particles counted is the only quality criterion that is not met, change the threshold setting to correspond
to a smaller particle size that yields su fficient counts, or repeat 6.5 to 6.6 using a larger sample volume.
Do not collect and re-use primary and secondary calibration samples. Avoid the use o f magnetic stirrers.
NOTE Other failures to meet the quality criteria can arise from a number o f sources, including contaminated
diluent or glassware, volumetric errors, calculation errors, operating too closely to the threshold noise level o f
the APC, or bubbles in the samples. Flow rate variability due to counting while the sample chamber is being
pressurized or due to other sources, also leads to problems. Particle settling can occur. Excessive agitation or
turbulence introduces bubbles into samples.

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 ISO 1 1 1 71 : 2 02 0(E)

Table 2 — APC particle sizing calibration worksheet (see 6 .6)

APC Model Date
Serial number Operator
Sensor type Model Noise level mV
Serial number Flow rate mL/min

First calibration suspension worksheet

First calibration suspension identification number
Channel Channel Channel Channel Channel Channel Channel Channel
1 2 3 4 5 6 7 8

Threshold setting (mV )

Count 1 (particles/mL)
Count 2 (particles/mL)
Count 3 (particles/mL)
Count 4 (particles/mL)
Count 5 (particles/mL)
X (particles/mL)
DQ
XN (particles/mL)
Second calibration suspension worksheet
Second calibration suspension identification number
Channel Channel Channel Channel Channel Channel Channel Channel
1 2 3 4 5 6 7 8

Threshold setting (mV )

Count 1 (particles/mL)
Count 2 (particles/mL)
Count 3 (particles/mL)
Count 4 (particles/mL)
Count 5 (particles/mL)
X (particles/mL)
DQ
XN (particles/mL)

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ISO 1 1 1 71 : 2 02 0(E)

Table 2 — APC particle sizing calibration worksheet (continued)

Third calibration suspension worksheet

Third calibration suspension identification number
Channel Channel Channel Channel Channel Channel Channel Channel
1 2 3 4 5 6 7 8

Threshold setting ( ) mV

C ou nt 1 ( p a r ticle s/m L)

C ou nt 2 ( p a r ticle s/m L)

C ou nt 3 ( p a r ticle s/m L)

C ou nt 4 ( p a r ticle s/m L)

C ou nt 5 ( p a r ticle s/m L)

X ( p a r ticle s/m L)

DQ
XN ( p a r ticle s/m L)

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 ISO 1 1 1 71 : 2 02 0(E)

Table 3 — Calibration curve worksheet

Threshold Standard
XN Mean
setting NC
( p a r ticle s/m L)
uncertainty
( p a r ticle s/m L)
mV Sample 1 Sample 2 Sample 3 ( p ar ticle s/m L)

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ISO 1 1 1 71 : 2 02 0(E)

6.7 Normalize the values for X recorded in Table 2 for each channel for a particular sample, using
Formula (6) :
XN = X ⋅ DR (6)

where
XN is the mean normalized particle concentration, in particles per millilitre, o f the undiluted
calibration suspension sample for a particular channel;
X is the mean particle concentration, in particles per millilitre, o f all acceptable counts from
the sample for a particular channel (6.6);
DR is the actual dilution ratio for the sample (G.8 ).
I f the sample was not diluted, the value o f DR is 1. I f the sample was diluted according to Annex G, use
the value o f DR for the sample obtained in G.8. Record the value o f XN for each channel in the appropriate
cells in Tables 2 and 3 .
6.8 Repeat 6.4 to 6.7 two more times using di fferent calibration suspension samples and approximately
the same DR as the first sample. Choose threshold settings for each sample such that at least two di fferent
samples are analysed for each o f the threshold settings listed in Table 3 (6.3 ).
Note that a di fferent undiluted calibration sample shall be used each time 6.4 to 6.7 is repeated to ensure
that the APC calibration curve is based on data from 3 di fferent primary or secondary calibration
samples.

6.9 Define the relationship between particle size and threshold voltage setting using the constrained
cubic spline technique. A spreadsheet to carry out this interpolation is provided at the following URN:
http://standards .iso.org/iso/11171/ed-4/en.
To use the spreadsheet, open the worksheet labelled 6.9 and enter the threshold voltage settings and
corresponding values o f XN for each calibration suspension sample taken from the first four columns
of Table 3 (6.7) in the white data cells o f columns A, B, C and D in order of decreasing value of threshold
voltage setting. Enter only values o f XN in cells for threshold settings that were actually used for a
given sample. Leave all other cells empty. Record in the fi fth column o f Table 3 the mean XN for each
threshold setting which is displayed in column E o f the 6.9 worksheet. Calculate the standard deviation
o f all acceptable counts for all the samples listed in Table 2 (6.6) for each threshold setting. Calculate
the standard uncertainty for each threshold setting, using Formula (7) :

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 ISO 1 1 1 71 : 2 02 0(E)

sDR
sN = (7)
NC
where
sN is the standard uncertainty in normalized particle concentration, in particles per millilitre, o f
the undiluted calibration suspension sample for a particular channel;
s is the standard deviation, in particles per millilitre, o f all acceptable counts from all the sam-
ples (6.6) obtained from a particular channel;
DR is the actual dilution ratio for the sample (G.8);
NC is the total number o f acceptable particle counts from all samples for a particular channel
(i.e. 8 to 15).
Record in the appropriate cells o f Table 3, the values o f NC and sN for each threshold setting.
NOTE Failure to enter the threshold voltage settings in the subclause 6.9 worksheet in the proper order
results in error. The worksheet will display values o f 0 for the interpolated threshold voltage settings in column
H i f the threshold voltage settings in column A are not consecutive or not in order o f decreasing voltage. A value
o f 0 for the interpolated threshold voltage setting will also be displayed for any particle concentration that falls
outside the range o f the data in column E.

6.1 0 Determine the threshold voltage settings that correspond to the particle concentrations for each
size selected in 6.2 using the same subclause 6.9 worksheet. Enter, in order o f increasing particle size,
the size and corresponding particle concentrations from Table 4 in the blue data cells o f column F and G.
The worksheet displays the interpolated threshold voltage setting corresponding to each size in yellow
column H. The values o f extrapolated points are displayed as “0”. Record the interpolated threshold
voltage settings for each o f these sizes in the right column o f the Particle Size Calibration Summary
of Table 4 that corresponds to this size. The use o f extrapolated data is forbidden. Proceed to 6.11 to
continue calibration for particle sizes larger than 30 μm(c) for primary calibrations or for particle sizes
greater than the largest size listed on the certificate o f analysis for secondary calibrations. I f the APC is
not to be calibrated for larger particle sizes, proceed to 6.15 .

6.1 1 Obtain polystyrene latex spheres (4.1) with nominal diameters larger than 30 µm and spanning the
particle size range o f interest. The particle size o f the smallest polystyrene latex sphere (4.1) chosen shall
be between 35 µm and 45 µm. The particle size o f the next largest latex spheres shall be approximately
equal to the size o f the smallest latex sphere times a constant with a value between 1,1 and 1,5.
Subsequent larger latex particle sizes shall be approximately equal to the largest preceding latex particle
size times a constant with a value between 1,1 and 1,5. Prepare the polystyrene latex suspensions for
each size o f latex spheres as described in D.2.

6.1 2 Set the APC to the di fferential mode and set the first four channels o f the APC at threshold settings,
as follows:
a) set the first channel to 1,5 times the threshold noise level o f the APC;
b) set the third channel to the threshold voltage setting expected to correspond to the polystyrene
latex sphere size;
c) set the second channel to the threshold voltage setting corresponding to 0,72 times the threshold
voltage setting o f the third channel;
d) set the fourth channel to the threshold voltage setting corresponding to 1,32 times the threshold
voltage setting o f the third channel.

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ISO 1 1 1 71 : 2 02 0(E)

Use only the di fferential particle counts o f the second and third channels determined in 6.13 through
6.15 to determine the threshold setting corresponding to the polystyrene latex sphere size.

6.1 3 Prepare and analyse the diluted polystyrene latex sphere sample as described in 6.5, but obtain at
least 2 500 particles in the second channel, instead o f 10 000 particles at the smallest threshold setting.
Evaluate the particle count data using the criteria described in 6.6 . If DQ is less than the appropriate
value shown in Table C.2 for the second and third channels, proceed to 6.14. I f not, discard the data and
suspect an error in the analytical technique. Repeat 6.11 to 6.13 after taking appropriate corrective
action (see NOTE in 6.6 ).
NOTE To determine the hal f-count setting more rapidly, it may be desirable to per form 6.12 to 6.14, but
obtain only one count (instead o f five as indicated in 6.13) o f at least 500 particles in the second channel. Readjust
the channels as necessary and repeat the process until the hal f-count condition described in 6.14 is achieved.
Following this, repeat 6.12 to 6.14 using five counts as described in 6.13 .

6.1 4Calculate the di fference in observed particle counts, D, expressed as a percentage, between the
second and third channels using Formula (8) :
 N2 
D = 1−  × 100 (8)
 N3 
where
N2 is the mean number o f particles counted for the second channel;
N3 is the mean number o f particles counted for the third channel.
I f the absolute value o f D is less than or equal to 3 %, the threshold setting o f the third channel corresponds
to the size o f the polystyrene latex sphere. I f not, and i f the value o f D is negative, the threshold settings
selected in 6.12 are too high. I f D is positive, the threshold settings selected in 6.12 are too low. Re-
adjust the second, third and fourth channel settings while maintaining the relationship among these
three channels as described in 6.12. Repeat 6.12 to 6.14 using the re-adjusted threshold settings. I f no
threshold setting yields an absolute value for D less than 3 %, the threshold setting o f the third channel
yielding the minimum absolute value o f D corresponds to the size o f the polystyrene latex sphere.
For each latex sphere size, record the mean latex particle diameter in the particle size column and the
corresponding mean threshold setting in the threshold setting column o f the Particle Size Calibration
Summary o f Table 4. Do not record a particle concentration and leave this data cell empty.
Repeat 6.12 to 6.14 using the next size o f latex spheres until all latex samples prepared in 6.11 have
been analysed and then proceed to 6.15 .

6.1 5 Define the APC calibration curve by interpolation o f the particle size data and corresponding mean
threshold voltage settings listed in the Particle Size Calibration Summary o f Table 4 using the constrained
cubic spline technique. A spreadsheet to carry out this interpolation is provided at the following URN:
http://standards .iso.org/iso/11171/ed-4/en.
To use the spreadsheet, open the 6.15 worksheet and enter all o f the particle sizes and corresponding
mean threshold settings from Table 4 into the white data cells o f column A and B in order o f increasing
particle size. Enter the values for all particle sizes o f interest into the blue data cells o f column C o f
the worksheet in order o f increasing size. The worksheet displays the interpolated threshold setting
corresponding to each size in yellow column D and the actual calibration curve. Extrapolation is
forbidden and the spreadsheet displays extrapolated value as "0".

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Table 4 — APC Calibration summary

APC Model __________________________ Date ________________________________________
Serial Number ________________ Operator ___________________________________
Sensor Model __________________________ Calibration type (primary or secondary) _____________________
Serial Number _________________ Calibration sample identification numbers ___________________
Noise level (Annex A) _________________mV Coincidence error limit (Annex B) ______________ particles/mL
Sample volume (Annex A) ____________mL Working flow rate (Annex C ) ___________________ mL/min
C v, vol (Annex A) _______________________ % Flow rate range (Annex C ) ______________________ mL/min
Resolution (Annex D)
SR _________________ µm R R ________________________________ %
SL _________________ µm R L ________________________________ %
d _________________ µm R _________________________________ %

Verification o f Particle Counting Particle Size Calibration Summary

Accuracy (Annex E ) (Clause 6 )

Expected Observed
Particle Particle Particle Threshold
particle particle
Size Size Concentration Setting
concentration concentration
µm(c) Particles/mL Particles/mL µm(c) Particles/mL mV

7 Data presentation
7.1 Report all particle sizes obtained using an APC calibrated in accordance with this document
as “µm(c)”, where the sizes were obtained through the use o f an APC calibrated in accordance with
ISO 11171 using calibration samples traceable to NIST SRM 2806x.

7.2 Retain completed Table 2, Table 3, Table 4, Table B.1 and Table C.1 on file for inspection.

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ISO 1 1 1 71 : 2 02 0(E)

8 Identification statement
Use the following statement in test reports, catalogues and sales literature when an APC is calibrated in
accordance with this document:
“Calibration o f liquid automatic particle counter con forms to ISO 11171, Hydraulic fluid power —
Calibration of automatic particle counters for liquids.”

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 ISO 1 1 1 71 : 2 02 0(E)

Annex A
(normative)
Preliminary APC check

A.1 Conduct the preliminary APC check as set out in the flow chart in Figure A.1 when a new APC is
received, following the repair or re-adjustment o f an APC or sensor.

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ISO 1 1 1 71 : 2 02 0(E)

Figure A.1 — Preliminary APC check procedure

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 ISO 1 1 1 71 : 2 02 0(E)

A.2 Determine the threshold noise level o f the APC under no-flow conditions with clean diluent (4.2 )
in the sensor. Ensure that the noise levels do not di ffer significantly for all the channels o f the APC. I f
significant di fferences occur, re-adjust the APC. Record the APC and sensor model and serial number, the
date, operator and the threshold noise level o f the first channel in Tables 2, 4, B.1, C.1 and F.1.
For APCs that use pulse height analysers (as opposed to comparator circuits), determine only the
first-channel threshold noise level. Contact the APC manu facturer in order to determine the type o f APC
being used (pulse height analyser or comparator circuit type).
NOTE The APC manu facturer can provide guidance on how to determine the threshold noise level.

A.3 Determine the sample volume actually measured during a particle-counting run using a method
with traceability to a national or ISO standard. Record this value in Table 4 and use it to calculate particle
concentrations in all subsequent work.
Contact the APC manu facturer in order to determine an appropriate method o f determining the
sample volume.
A.4 Prepare an RM 8632x concentrate o f approximately 100 mg/L as follows:
a) accurately weigh out the required amount o f dry RM 8632x (±0,1 mg) and trans fer it to a clean
sample bottle; and
b) fill the bottle approximately 75 % full with an accurately measured amount (±1 mL) o f clean diluent.
Calculate the mass concentration o f dust, γA , in milligrams per litre, in the concentrate using
Formula (A.1) :

γA = 1 000 m (A.1)
V0
where
m is the mass, in milligrams, of RM 8632x;
V0 is the volume, in millilitres, of clean diluent.
The RM 8632x concentrate, prepared in accordance with this subclause, is used to determine the
coincidence error limit (Annex B) and flow rate limits (Annex C) o f the APC, as well as to veri fy particle-
counting accuracy (Annex E). Take special care in determining the dust concentration o f the concentrate
and ensure that the concentrate is not contaminated. Failure to do so can cause an otherwise suitable
APC to be deemed unacceptable for use.

A.5 Cover the bottle with a clean closure and vigorously shake the concentrate by hand. Disperse the
RM 8632x concentrate ultrasonically for at least 30 s and then shake it on a mechanical shaker for at
least 60 s to disperse the dust. De-gas the concentrate under vacuum or ultrasonically until no surfacing
bubbles are observed and proceed immediately to A.6 .

A.6 Calculate the amount o f concentrate required to prepare a dilution that is about 25 % o f the
coincidence error limit for the sensor recommended by the manu facturer. Estimate the number
concentration corresponding to a particular mass concentration using Table A.1 .
Add accurately the required amount o f concentrate and clean diluent (4.2) to a clean sample container
in order to obtain the correct total volume o f diluted RM 8632x suspension. Put a particle- free closure
on the sample container.

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ISO 1 1 1 71 : 2 02 0(E)

Table A.1 — Particle size distribution for sensor per formance verification
(see A.6, B.4, E .4 and E .9) a
Median particle Particle concentration (particles/mL greater than indicated
concentration (particles/ size for a 1,00 mg/L sample o f RM 8632x) shall be
Particle size mL
µm(c) greater than indicated
size for a 1,00 mg/L greater than or equal to less than
sample o f RM 8632x)
2 20 210 14 180 28 820
3 10 700 7 928 14 440
4 6 300 4 553 8 713
5 3 475 2 330 5 183
6 1 631 938,2 2 834
7 769,8 413,6 1 433
8 379,1 179,7 799,5
9 196,2 76,57 502,6
10 88,90 27,89 283,4
a The particle concentrations in Table A.1 are for RM 8632a and can change i f a di fferent batch o f RM 8632x is used.

A.7 Set the APC to the cumulative mode. Set the lowest threshold setting o f the APC to 1,5 times the
threshold noise level o f the APC. Using clean diluent, adjust the flow rate to the working flow rate. Record
the flow rate in Tables 2, 4, B.1, C.1 , and F.1.
Conduct all o f the procedures at the same flow rate. Determine the flow rate limits o f the APC in
accordance with Annex C. Discard any data obtained at flow rates outside these limits and repeat the
corresponding part o f the procedure using the appropriate flow rate.
A.8 Prepare and analyse the diluted RM 8632x suspension sample prepared in A.6 as described in 6.5 .
Calculate the coe fficient o f variation for volume measurement, CV,vol, using Formula (A.2) :
NC 2
 NC 
∑
NC X −  Xi  2
i
 i=1 ∑
100 i =1  
CV ,vol =
X NC ( NC − 1 )
(A.2)
where
NC is the number o f consecutive particle counts per formed on the sample (i.e. five);
X is the mean particle concentration, in particles per millilitre, for the five counts;
Xi is the particle concentration, in particles per millilitre, observed for count i.
A.9 The V,vol shall be 3 % or less in order for the APC to be acceptable. Record the V,vol in Table 4.
C C

Although the V,vol is considered to be a measure of the ability of the bottle sampler to reproducibly
C

deliver the indicated volume o f fluid, other sources o f variability, including sample handling and the
counting accuracy o f the APC, are also included. Regardless o f the source o f variability, only proceed
with the calibration where the CV,vol is 3 % or less.

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 ISO 1 1 1 71 : 2 02 0(E)

Annex B
(normative)
Coincidence error procedure

B.1 Determine the coincidence error limit as set out in Figure B.1 when a new APC is received or after
the repair or re-adjustment o f an APC or sensor.
The magnitude o f the coincidence error at a given particle number concentration is governed by the
physical dimensions o f the sensing volume, as well as the particle size distribution o f the sample,
including those particles too small to be counted. The coincidence error limit determined in this annex
shall be regarded as a benchmark indicator that is use ful for routine analyses. For work requiring a
higher degree o f accuracy, analyse multiple dilutions o f a sample to establish that the particle size
distribution o f the sample does not yield a particle number concentration significantly di fferent from
that determined using this annex.
B.2 Set the APC to the cumulative mode. Choose a threshold setting corresponding to 1,5 times the
threshold noise level o f the APC or corresponding to the smallest particle size o f interest i f it is greater
than 1,5 times the threshold noise level. Only data from this channel is used in this annex. Set the
remaining channels to higher settings arranged in ascending order.

B.3 Adjust the flow through the sensor to the working flow rate (see A.7 ) using clean diluent (see 4.2 ).
Flush the sensor with at least two 150 mL batches o f clean diluent.

B.4 Prepare dilutions o f the concentration (see A.4) which are 10 %, 20 %, 30 % to 150 % o f the
particle number concentration limit recommended by the manu facturer for the sensor. Table A.1 can be
used to estimate the mass concentrate o f RM 8632x necessary to obtain the required particle number
concentration. Calculate the required amount o f concentrate, V1 , in millilitres, needed for each dilution
using Formula (B.1) :
XM VS L
V1 = (B.1)
100 XA

where
XM is the particle number concentration limit, in particles per millilitre, recommended by the
manu facturer;
VS is the final volume, in millilitres, o f the diluted sample;
L is the percentage o f the limit recommended by the manu facturer;
XA is the particle number concentration, in particles per millilitre, o f the concentrate.
Disperse the RM 8632x concentrate in accordance with A.5. Accurately add the required amounts
o f concentrate, V1 , and clean diluent (4.2) to the sample container in order to attain the correct total
volume. Put particle- free closures on the sample containers.

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ISO 1 1 1 71 : 2 02 0(E)

Figure B.1 — Coincidence error determination procedure

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B.5 Analyse the samples prepared in B.4 as described in 6.5 in order o f increasing particle number
concentration.
Evaluate the particle count data using the criteria described in 6.6 . If DQ is acceptable, record in
Table B.1 the mass concentration, in milligrams per litre, o f the diluted sample, the corresponding
observed particle number concentrations for each o f the five counts, and the mean particle number
concentration, X , be fore proceeding to B.6 . If DQ is too large, discard the data and suspect an error in
the analytical technique. In this case, repeat B.4 and B.5 a fter taking appropriate corrective action (see
NOTE to 6.6).
B.6 Flush the sensor with the next sample to be counted using at least three times the sample volume
determined in A.3. Repeat B.5 and B.6 for all required dilutions.
B.7 Plot the mean particle number concentration, X , as a function o f the mass concentration o f
RM 8632x, γ, on a linear-graph. Determine the linear regression line for the results from the 10 % to
40 % particle number concentration samples using the least squares method with the intercept set to 0.
The regression equation shall pass through the origin and be o f the form given in Formula (B.2) :
X = a⋅γ (B.2)

where a is the slope of the regression line.

Plot the regression line just determined on the graph for particle number concentrations ranging
from 0 % to 150 % o f the limit recommended by the manu facturer. This line defines the theoretical
relationship between the number concentration o f particles and the mass concentration. Record in
Table B.1 the slope, a, and correlation coe fficient, r, obtained by regression analysis.

B.8 Use the regression equation obtained in B.7 to calculate the theoretical number o f particles for
each mass concentration, Xt. Record the value o f Xt for each mass concentration in the appropriate cell in
Table B.1 .

B.9 Calculate the di fference, E, expressed as a percentage, between the theoretical, Xt, and mean, X ,
particle number concentration for each dilution using Formula (B.3) :
X−X
E= × 100t
(B.3)
X t

Record the value o f E for each mass concentration in Table B.1 .

B.10 Determine the coincidence error limit o f the sensor by plotting a line passing through the origin
with a slope o f 95 % o f the theoretical relationship (see B.7). The lowest particle number concentration,
in particles per millilitre, at which the data line (B.7) crosses the 95 % line is the coincidence error
limit o f the sensor. I f the data line does not cross the 95 % line, report the limit recommended by the
manufacturer as the coincidence error limit o f the sensor and use this value for all subsequent work.
Record the coincidence error limit, in particles per millilitre, o f the sensor in Table 4 and Table B.1 .

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 Table B.1 — Coincidence error data sheet
28

ISO 1 1 1 71 : 2 02 0(E)
Pa r ticle cou nter Model D ate S er ia l no . O p erator Sensor Model S eri a l no .

Noise level F low rate C h a n nel s e tti ng F low rate l i m its

C o ncentratio n

(mg/L)
Count 1
( p a r ticle s/m L)

Count 2
( p a r ticle s/m L)

C o u nt 3

( p a r ticle s/m L)

C o u nt 4

( p a r ticle s/m L)

C o u nt 5

( p a r ticle s/m L)

X ( p a r ticle s/m L)

Xt ( p a r ticle s/L)
E
C oi nc idence er ror l i m it ( p a r ticle cou nts/m L) =

Xt =aγ
a=
r=
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 ISO 1 1 1 71 : 2 02 0(E)

Annex C
(normative)
Flow rate limit determination

C.1 Perform the flow rate limit determination, as set out in Figure C.1 , when a new APC is received or
ollowing the repair, or re-adjustment o f an APC or sensor.
f

IMPORTANT — It is essential that the flow rate limits determined in accordance within this
annex are followed in all APC calibration and sample analysis work. APC calibration is sensitive
to flow rate. At high flow rates, the electronics may not determine the size o f the particle
correctly. The time interval separating successive particles can be so small that the electronics
are unable to distinguish them as individual particles.

© ISO 2020 – All rights reserved 29

ISO 1 1 1 71 : 2 02 0(E)

Figure C.1 — Flow rate limit determination procedure

C.2 Record the date, operator, APC and sensor model and serial numbers in Table C.1 . Determine
whether the flow rate o f the APC bottle sampler can be adjusted by the operator (adjustable flow rate
type) or is designed to deliver the sample at a fixed flow rate (fixed flow rate type).

C.3 I f the APC is o f the adjustable flow rate type, proceed to C.4. I f it is o f the fixed flow rate type,
proceed to C.14.

30 © ISO 2020 – All rights reserved

 ISO 1 1 1 71 : 2 02 0(E)

C.4 Set the APC to the cumulative mode. Use the calibration curve determined in 6.15 to set the first
channel to 1,5 times the threshold noise level o f the APC or the smallest particle size o f interest. Ignore
the data from other channels during the flow rate limit determination. Let the flow rate number, n fr = 1.
NOTE All channels to be in order o f increasing threshold setting, unless otherwise recommended by the APC
manu facturer.

C.5 Calculate the flow rate, q , in millilitres per minute, to be used according to Formula (C.1) :
nfr qm
q=
5 (C.1)
where
n fr is the flow rate number;
qm is the working flow rate, in millilitres per minute.
Using clean diluent, establish a flow rate approximately equal to q.

C.6 Prepare a sample o f RM 8632x in clean diluent as specified in A.4 to A.6 .

C.7 Prepare and analyse the RM 8632x sample prepared in C.6 as described in 6.5 .

C.8 Record the flow rate and the number o f particles observed at the channel corresponding to
1,5 times the threshold noise level o f the APC or the smallest particle size o f interest for each count in the
appropriate column in Table C.1 .

C.9 Evaluate the particle count data using the criteria described in 6.6 . If DQ is less than or equal to the
appropriate value shown in Table C.2, proceed to C.10. If DQ is greater than the appropriate value shown
in Table C.2, discard the data and suspect an error in the analytical technique. Repeat C.6 to C.9 after
taking appropriate corrective action (see NOTE to 6.6 ).

© ISO 2020 – All rights reserved 31

ISO 1 1 1 71 : 2 02 0(E)

Table C.1 — Flow rate limit worksheet

APC Mode Date
Serial no. Operator
Sensor Model
Serial no.

Noise level
Working flow rate
Flow rate limits

Particle counts (C.8 and C.10)

n fr 1 2 3 4 5 6 7 8
Flow rate
Count 1
Count 2
Count 3
Count 4
Count 5
X

Particle counts (C.14 and C.15 )

Count 1 Count 2 Count 3 Count 4 Count 5 X
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Mean — — — — —
Standard — — — — —
deviation
CV — — — — —

32 © ISO 2020 – All rights reserved

 ISO 1 1 1 71 : 2 02 0(E)

Table C.2 — Maximum allowable di fferences, expressed as percentages, in particle counts

between runs (see 6 .6 , 6 .13 , B.5, C.9, D.4, D.9, E .6 , E .9, F. 5 and F.6)
I f X (mean observed Use these values for the Use these values for the maximum
number o f particles maximum allowable D Q for an allowable CV when the number o f
counted) is individual sample samples analysed is (see E .9 and F.6)
greater than but less than (see 6.6, 6.13, B.5, C.9, D.4, D.9 N= 3 N= 6 = 10 = 20 N = 40
or equal to E.6 and F.5 ) N N

10 000 11,0 7,8 5,3 4,0 2,7 1,8

5 000 10 000 11,3 7,8 5,3 4,0 2,7 1,9
2 000 5 000 11,9 7,9 5,4 4,1 2,9 2,1
1 000 2 000 13,4 8,0 5,6 4,3 3,1 2,4
500 1 000 15,6 8,2 5,9 4,7 3,6 2,9
200 500 19,3 8,9 6,8 5,7 4,7 4,1
100 200 27,5 10,0 8,0 7,0 6,1 5,5

C.10 Calculate the mean observed particle concentration, X , in particles per millilitre, and record this
result in Table C.1 .
C.11 If n fr ≥ 8, proceed to C.12 . I f not, increase n fr by 1, and repeat C.5 to C.10.
C.12 Plot the mean observed particle concentration, X , in particles per millilitre, as a function o f the
flow rate on a linear-linear graph and connect the data points by a smooth curve.

C.13 Determine the flow rates above and below the working flow rate that yield counts that di ffer by
more than 5 % from those observed at the working flow rate. These are the flow rate limits o f the APC.
Record the flow rate limits in Table 4, Table B.1 and Table C.1 .

C.14 Establish a flow rate equal to the working flow rate. Prepare and analyse five samples as specified
in C.6 to C.9. Record the number o f counts observed at the channel corresponding to 1,5 times the
threshold noise level o f the APC or the smallest particle size o f interest for each count o f each sample in
Table C.1. Calculate the mean observed particle concentration, X , in particles per millilitre, for each
sample and record this result in Table C.1 .

C.15 Calculate and record, in Table C.1, the mean, standard deviation and coe fficient o f variation o f the
five X for the samples analysed in C.14. I f the coe fficient o f variation is less than or equal to 3 %, then the
APC meets the flow rate specifications o f this document. I f the coe fficient o f variation is greater than 3 %,
the APC is unacceptable and requires servicing or replacement.
Ideally, always use the APC at the working flow rate. Calibrate APCs at each flow rate for which they are
used. Always use the APC within the flow rate limits determined in accordance with C.2 to C.13. I f any
o f the data used for size calibration was obtained using flow rates outside these limits, repeat the size
calibration within these flow rate limits.

© ISO 2020 – All rights reserved 33

ISO 1 1 1 71 : 2 02 0(E)

Annex D
(normative)
Resolution determination

D.1 Perform the resolution determination as set out in Figure D.1 when a new APC is received or
ollowing the repair or re-adjustment o f an APC or sensor.
f

Figure D.1 — Resolution determination procedure

34 © ISO 2020 – All rights reserved

 ISO 1 1 1 71 : 2 02 0(E)

Determine resolution using a polystyrene latex sphere suspension with a nominal particle size o f 10 µm
(4.1). Measure the resolution at not less than 2,1 times the threshold noise level o f the APC (see Annex A).
Use the calibration curve determined in Clause 6 to determine the corresponding size as specified in
D.3. Be aware that optical arte facts can occur that yield poor resolution results. I f poor resolution is
obtained contact the APC manu facturer to determine the reason and discuss the appropriate action.
Note that the procedures may be carried out manually or by the use o f appropriate so ftware for those
APCs with microprocessor controls. Alternatively, resolution may be determined through use o f an
MCA. Such practice is acceptable, provided the relationship between the measured voltage o f the MCA
and the APC threshold setting is established. In general, an MCA provides faster, more accurate results
than the di fferential hal f-count method.
D.2 Prepare a sample o f polystyrene latex sphere suspension as follows:
a) Calculate the volume o f polystyrene latex sphere concentrate (4.1), V0 , in millilitres, that needs to
be added to clean aerosol OT diluent (4.3) to achieve a particle concentration that is approximately
25 % o f the coincidence error limit for the sensor using Formula (D.1) :
VS XL π dL3
V0 = (D.1)
6 ×1010 × ws
where
VS is the final volume, in millilitres, o f the polystyrene latex sphere suspension;
XL is the desired particle concentration, in particles per millilitre;
dL is the mean diameter, in micrometres, o f the polystyrene latex spheres indicated on its
certificate o f analysis (see 4.1);
ws is the solids content, expressed as a percentage mass fraction, o f the polystyrene latex
sphere concentrate (this value is typically supplied by the manu facturer o f the polysty-
rene latex spheres).
b) Shake polystyrene latex sphere concentrate vigorously by hand, then disperse it ultrasonically for
30 s and finally shake it mechanically for at least 1 min to suspend the polystyrene latex spheres;
c) Prepare a suspension o f polystyrene latex spheres by adding the required amount o f polystyrene
latex sphere concentrate, V0 , to a sample container approximately 75 % full o f clean aerosol OT
diluent (4.3) and dispersing the sample by mechanical shaking for at least 1 min.
The final dilution o f the polystyrene latex sphere suspension, which is counted, shall be clear in
appearance. Be fore proceeding, correct any cloudiness in the sample, which indicates insu fficient
dilution.
D.3 Set the APC to the di fferential mode. Use the calibration curve (see Clause 6) to estimate the
threshold setting that corresponds to the polystyrene latex sphere size, as follows:
a) Set the first channel to 1,5 times the threshold noise level o f the APC;
b) Set the third channel to the threshold voltage setting corresponding to the polystyrene latex
sphere size;
c) Set the second channel to the threshold voltage setting corresponding to 0,72 times the threshold
voltage setting o f the third channel;
d) Set the fourth channel to the threshold voltage setting corresponding to 1,32 times the threshold
voltage setting o f the third channel.

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ISO 1 1 1 71 : 2 02 0(E)

Use only the di fferential particle counts o f the second and third channels to determine the threshold
setting corresponding to the polystyrene latex sphere size.
Due to di fferences in the optical properties o f the polystyrene latex spheres and the calibration
dust (4.4), the apparent particle size obtained using an APC calibrated in accordance with Clauses 5 and
6 di ffers from the size stated by the supplier o f the polystyrene latex spheres. As a first approximation,
choose a particle size that is 10 % to 50 % larger than the particle size stated by the supplier o f the
polystyrene latex spheres.
NOTE 1 D.3, D.4 and D.5 speci fy the moving-window di fferential hal f-count method for determining the
threshold setting that corresponds to the mean polystyrene latex sphere size. These data are critical to
determining sensor resolution. Inaccurate determination o f the threshold setting corresponding to the mean
polystyrene latex sphere size can result in apparently poor sensor resolution and failure o f the APC to pass the
sensor per formance specification.
NOTE 2 To determine the hal f-count setting more rapidly, some labs first per form D.3 to D.5, but obtain only
one count (instead o f five as indicated in D.4) o f at least 500 particles in the second channel, and then re-adjust the
channels as necessary and repeat the process until the hal f-count condition described in D.5 achieved. Following
this, they repeat D.3 to D.6 using five counts as described in D.4 .

D.4 Prepare and analyse the diluted polystyrene latex sphere sample as described in 6.5, but obtain at
least 2 500 particles in the second channel, instead o f 10 000 particles at the smallest threshold setting.
Evaluate the particle count data using the criteria described in 6.6 . If DQ is less than the appropriate value
shown in Table C.2 for the second and third channels, proceed to D.5. I f not, discard the data and suspect
an error in the analytical technique. Repeat D.2 to D.4 after taking appropriate corrective action (see
NOTE in 6.6).
D.5 Calculate the difference in observed particle counts, D, expressed as a percentage, between the
second and third channels using Formula (D.2) :
 N2 
D = 1−
N3 
× 100 (D.2)

where
N2 is the mean number o f particles counted for the second channel;
N3 is the mean number o f particles counted for the third channel.
I f the absolute value o f D is less than or equal to 3 %, the threshold setting o f the third channel
corresponds to the size o f the polystyrene latex sphere. In this case, proceed to D.6. I f not, and i f the
value o f D is negative, the threshold settings in D.3 are too high. I f D is positive, the threshold settings
in D.3 are too low. Re-adjust the second, third and fourth channel settings while maintaining the
relationship among these three channels as described in D.3. Repeat D.3 to D.5 using threshold settings
for the second, third and fourth channel which have been re-adjusted. I f no threshold setting yields
an absolute value for D less than 3 %, the threshold setting o f the third channel yielding the minimum
absolute value o f D corresponds to the size o f the polystyrene latex sphere.

D.6 Using the calibration curve obtained in 6.15, determine the particle size that corresponds to the
threshold setting o f the third channel. Using the calibration curve obtained in 6.15, determine the sizes
and threshold settings that correspond to 0,9 and 1,1 times this size.

D.7 Set the first five channels o f the APC as follows:

a) Set channel A, the first channel, to the threshold voltage setting corresponding to 0,72 times the
threshold setting o f the third channel, channel C;
b) Set channel B, the second channel, to the threshold voltage setting corresponding to a size 0,9 times
the size o f the polystyrene latex sphere determined in D.6;

36 © ISO 2020 – All rights reserved

 ISO 1 1 1 71 : 2 02 0(E)

c) Keep channel C, the third channel, at the threshold voltage setting corresponding to the size o f the
polystyrene latex sphere determined in D.6;
d) Set channel D, the fourth channel, to the threshold voltage setting corresponding to a size 1,1 times
the size o f the polystyrene latex sphere determined in D.6;
e) Set channel E, the fi fth channel, to the threshold voltage setting corresponding to 1,32 times the
threshold setting o f channel C.
Use only di fferential counts to determine resolution.

D.8 Prepare and analyse the diluted polystyrene latex sphere sample as described in 6.5, but obtain at
least 2 500 particles in the second channel, instead o f 10 000 particles at the smallest threshold setting.

D.9 Evaluate the particle count data using the criteria described in 6.6 . If DQ is less than the appropriate
value shown in Table C.2 for the second and third channels, proceed to D.10 . I f not, discard the data
and suspect an error in the analytical technique. Repeat D.8 after taking appropriate corrective action
(see NOTE in 6.6).
D.10 Calculate the mean differential particle concentration for each channel.
D.11 Calculate the apparent standard deviation o f the APC using Formulae (D.3) and (D.4) :

sL = d (D.3)
6 ln [1 + 2 ( NB / NA ) ]

sR = d (D.4)
6 ln 1 + 2 ( NC / ND ) 

where
sL is the apparent le ft or negative-side standard deviation, in µm;
sR is the apparent right or positive-side standard deviation, in µm;
d is the apparent polystyrene latex sphere size, in micrometres, obtained using the calibration
curve obtained in 6.15 for the threshold setting o f the third channel;
NA is the mean number o f particles counted for channel A;
NB is the mean number o f particles counted for channel B;
NC is the mean number o f particles counted for channel C;
ND is the mean number o f particles counted for channel D.

D.12 Calculate the positive and negative-side resolution (RR and RL, respectively) using Formulae (D.5)
and (D.6) :
100 sL2 − sI2
RL = (D.5)
d
100 sR2 − sI2
RR = (D.6)
d
where sl is the standard deviation of the polystyrene latex sphere size, in micrometres, stated by the
supplier.
© ISO 2020 – All rights reserved 37
ISO 1 1 1 71 : 2 02 0(E)

The APC resolution, R, is RR or RL , whichever is greater. Record d, sR, sL , RR, RL , and R in Table 4 .

D.13 If R is less than 15 % for polystyrene latex spheres with a nominal size of 10 µm (see 4.1) and the
absolute value o f the di fference between RR and RL is less than or equal to 5 %, the resolution o f the
sensor is acceptable. I f R equals or exceeds 15 %, or the absolute value o f the di fference between RR and
RL is greater than 5 %, the APC is unacceptable and requires servicing or replacement. Alternatively,
there might be an error in the procedure used to prepare or analyse the polystyrene latex sphere sample,
or the polystyrene latex spheres themselves might not meet the requirements o f 4.1. In this case, identi fy
and correct the error, and repeat the resolution determination procedure specified in D.2 to D.12.
NOTE Cleaning the liquid-wetted portions o f the APC system in accordance with the instructions o f the
manu facturer can help improve resolution.

D.14 I f the APC fails to meet the resolution requirements o f D.13, check the polystyrene latex sphere size
distribution using an MCA or APC in the cumulative mode as follows:
a) Determine the size range corresponding to 0,55 and 1,45 times the size o f the polystyrene latex
spheres as determined in D.6. Divide the size range into at least 10 equal size increments and
determine the corresponding threshold settings using the calibration curve obtained in 6.15 . Set
the channels to as many o f these threshold settings as possible;
b) Prepare and analyse a polystyrene latex sphere sample as described in D.2 and D.4, but with the
APC set to the cumulative mode. Repeat the analysis at di fferent threshold settings until su fficient
numbers o f particles are obtained for all o f the size increments. When repeating the analysis, do
not change the channel corresponding to the smallest size;
c) Normalize the results o f each run by expressing the number o f counts in each channel as a
percentage o f the total counts observed in the smallest channel for the same run. Compile the
normalized results in order o f ascending size in a table. For each size, calculate the di fferential
percentage by subtracting the cumulative results for each size from the cumulative results for the
next largest size;
d) Plot the di fferential results versus size and fit a smooth curve through the data.
The curve plotted in item d) should be Gaussian (bell-shaped) in appearance with no secondary peaks
and the di fferential percentages at the smallest and largest sizes should approach zero. I f observed and
the APC failed the resolution requirements o f D.13, the APC needs to be repaired or serviced or else a
larger number o f size increments are needed to veri fy the polystyrene latex sphere size distribution.
I f not observed, suspect a problem with the polystyrene latex spheres or with the sample preparation.
Regardless o f why the APC failed, obtain an acceptable resolution for the APC as defined in D.13 . If
resolution cannot be obtained, then the APC cannot be calibrated in accordance with this document.

38 © ISO 2020 – All rights reserved

 ISO 1 1 1 71 : 2 02 0(E)

Annex E
(normative)
Verification o f particle-counting accuracy

E.1 Veri fy sensor particle-counting accuracy as set out in Figure E.1 when a new APC is received, or
ollowing the repair or re-adjustment o f an APC or sensor.
f

E.2 Prepare three identical samples containing 1,00 mg/L o f RM 8632x (4.7) suspended in clean
diluent (4.2 ).
IMPORTANT — It is critical that the dust concentration in this sample is accurate, because the
results obtained by analysis are compared to the values given in Table A.1. Inaccuracies in sample
preparation or counting can contribute to deviations from the values in Table A.1, which could
result in rejection o f an otherwise acceptable sensor. The three 1,00 mg/L RM 8632x samples
may be prepared in accordance with A.4 through A.6. When this method is used, be careful to
avoid errors introduced by weighing, volume measurement and settling. Alternatively, consider
purchasing 1,00 mg/L RM8632x samples from a reliable source that certifies its work.

E.3 Disperse the sample ultrasonically for at least 30 s and then shake it on a mechanical shaker for at
least 1 min to disperse the dust. Keep shaking the sample until it is to be analysed.

E.4 Set the APC to the cumulative mode and set the threshold voltage settings to at least six di fferent
sizes selected from those particle sizes listed in Table A.1. These settings shall be greater than 1,5 times
the threshold noise level o f the APC and shall include the smallest particle size o f interest as well as
4 μm(c), 6 μm(c) and 10 μm(c). Use the calibration curve previously determined in 6.15 to determine the
threshold voltage settings corresponding to these sizes. I f the sensor is incapable o f counting at one or
more o f these sizes, choose alternative sizes within the range o f sizes listed in Table A.1 .

E.5 Adjust the flow rate to the working flow rate.

E.6 Analyse the samples as described in 6.5. I f the data meet the quality criteria specified in 6.6,
proceed to E.8. I f they do not, discard the data and suspect an error in the analytical technique.
E.7 Repeat E.2 to E.6 after taking appropriate corrective action (see NOTE to 6.6 ).

© ISO 2020 – All rights reserved 39

ISO 1 1 1 71 : 2 02 0(E)

E.8 Rep eat E . 3 to E . 6 until three s amp les have b een analys ed.

Figure E.1 — Verification o f particle-counting accuracy

E.9 Fo r each p article s ize, calculate the glo b al mean p article co ncentratio n fo r all three s amp les , X,
and the co e fficient o f variatio n, CV
, exp res s ed as a p ercentage, fo r the three s amp les us ing Fo rmula (E . 1 ) :

40 © ISO 2020 – All rights reserved

 ISO 1 1 1 71 : 2 02 0(E)

N 2
N 
100
∑
N Xi2 −  Xi  ∑
CV = i=1  i=1  (E.1)
X N( N − 1 )
where
X
i is the mean particle concentration at a particular size for sample " i";
N is the total number o f samples analysed.
If theCV for any particle size is smaller than the corresponding values in Table C.2, compare the mean

for each size to the appropriate limits given in Table A.1 . If X falls within the particle concentration
limits given in the third and fourth columns o f Table A.1 for all six sizes, sensor per formance is verified.
Report the range o f expected particle concentrations and the mean particle concentration for each size
in Table 4.
If theCV for any particle size is larger than the corresponding values in Table C.2 discard the data

and suspect an error in the sample preparation or analytical technique. Repeat E.2 to E.9 a fter taking
,

appropriate corrective action.

If X for any particle size falls outside the corresponding limits given in Table A.1, then the APC system

is unacceptable and requires servicing or replacement. Alternatively, there might be an error in the
procedure used to prepare or analyse the verification samples in the calibration. In the latter case,
identi fy and correct the error and repeat the procedure in E.2 to E.9 .

© ISO 2020 – All rights reserved 41

ISO 1 1 1 71 : 2 02 0(E)

Annex F
(normative)
Preparation and verification o f bottles o f secondary calibration
suspensions

F.1 Prepare and veri fy secondary calibration suspensions as set out in Figure F.1 when, for economic
or other reasons, it is desirable to utilize secondary calibration suspensions instead o f NIST calibration
suspensions. For example, i f more than one APC needs to be calibrated, the use o f secondary calibration
suspensions can be more practical.
To prepare secondary calibration suspensions, calibrate one APC for re ference using NIST primary
calibration suspensions that con form to Clauses 5 and 6. Calibration o f the re ference APC with
secondary calibration samples is prohibited. Bottles o f secondary calibration suspensions, prepared
in accordance with this annex, may be used for sizing calibration instead o f NIST primary calibration
suspensions.

Figure F.1 — Procedure for preparation and verification o f secondary calibration suspensions

42 © ISO 2020 – All rights reserved

 ISO 1 1 1 71 : 2 02 0(E)

F.2 Prepare a minimum o f 30 bottles o f secondary calibration samples using a properly validated
multipass test system in accordance with ISO 16889 or a similar system, capable o f mixing a total volume
o f suspension o f at least 8 L.
Use NIST RM 8631x (4.5), ISO MTD (4.6), or other test dust con forming to ISO 12103-1 (4.6) to prepare
the samples. Use clean diluent (4.2) as the fluid. The dust concentration shall be such that the particle
concentration does not exceed 100 times the coincidence error limit for the sensor. Collect and store
samples prepared in this manner in clean, sealed containers with closures (4.9 ). The shelf life of the
secondary calibration samples shall not exceed that o f the NIST primary calibration suspensions.
NOTE The use o f NIST RM 8631x is recommended due to possible batch-to-batch variability in test dusts.
Secondary calibration samples prepared at concentrations exceeding the coincidence error limit o f the sensor
will be in coincidence error at small particle sizes, unless diluted as described in Annex G .

F.3 Calibrate an APC in accordance with Clause 5 and Clause 6 using NIST primary calibration
suspensions (4.4).
The APC used to veri fy the bottles o f secondary calibration suspension samples shall meet all APC
per formance specifications described in this document. Where a choice o f APCs is available, use the
APC with the best per formance, in terms o f coincidence error limit (B.10), threshold noise level (A.2 ),
resolution (D.12 ), flow rate coefficient o f variation (C.15), etc.
F.4 Select at least 16 di fferent particle sizes and corresponding threshold voltage settings using the
primary calibration curve determined in 6.15, such that:
a) the lowest threshold setting shall be at least 1,5 times the threshold noise level o f the APC;
b) the highest threshold setting shall be within the threshold voltage range covered by the
calibration curve;
c) intermediate threshold settings shall be chosen between the lowest and highest threshold settings
to correspond to particle sizes o f interest.
F.5 Prepare and analyse in accordance with 6.5 every fi fth sample bottle prepared in F.2.
Evaluate the particle count data for each sample bottle using the criteria described in 6.6 . If DQ is less
than the appropriate value shown in Table C.2 consider the data from that sample to be acceptable and
record the mean particle concentration for each threshold setting in Table F.1 . If DQ is greater than the
,

appropriate value shown in Table C.2, suspect an error in the analytical technique, discard the data and
analyse the next consecutive sample bottle only a fter taking appropriate corrective action (see NOTE
to 6.6).
For each threshold setting, calculate the global mean particle concentration, standard deviation and
coe fficient o f variation o f the samples using Formula (E.1) .

F.6 If the CV for each threshold setting is less than the corresponding value taken from Table C.2 then
,

the global mean particle concentrations, X , and corresponding particle sizes define the certified particle
size distribution for these secondary calibration suspensions, and can be used for secondary calibration
o f other APCs. Complete Table F.1 with the required data. I f the CV for a threshold setting is greater than
the corresponding value taken from Table C.2, re-evaluate the sample preparation procedure, take
appropriate corrective action and repeat F.2 to F.5 .
Do not collect and re-use primary and secondary calibration samples.

F.7 Producers o f secondary calibration suspensions shall retain completed Table F.1 on file for
inspection. The certificate o f analysis for these secondary calibration suspensions shall report the
particle size and corresponding values for X listed in Table F.1 .

© ISO 2020 – All rights reserved 43

 Table F.1 — Secondary calibration suspension validation data sheet
44

ISO 1 1 1 71 : 2 02 0(E)
APC Model Date
Serial no. Operator
Sensor Model Contaminant
Serial no. Lot no.
Noise level Flow rate Concentration
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17
Particle
size, µm(c)
Threshold
setting
Mean particle concentration for indicated sample bottle (particles/mL)
Sample
bottle 1
Sample
bottle 6
Sample
bottle 11
Sample
bottle 16
Sample
bottle 21
Sample
bottle 26
Sample
bottle 31
© ISO 2020 – All rights reserved

Sample
bottle 36
Sample
bottle 41
Sample
bottle 46
Sample
bottle 51
 Table F.1 (continued)
© ISO 2020 – All rights reserved

S a mp le

b o ttle 5 6

S a mp le

b o ttle 61

S a mp le

b o ttle 6 6

S a mp le

bottle 71
S a mp le

b o ttle 76

S a mp le

b o ttle 8 1

S a mp le

b o ttle 8 6

S a mp le

b o ttle 9 1

S a mp le

b o ttle 9 6

S a mp le

bottle 101

X ( p a r ticle s/

mL)
Sta nda rd

de viation

C V

ISO 1 1 1 71 : 2 02 0(E)
45
ISO 1 1 1 71 : 2 02 0(E)

Annex G
(normative)
Dilution o f calibration suspension samples

G.1 This annex shall be used to prepare samples for size calibration according to Clause 6 when the
particle concentration at the smallest threshold setting in 6.3 is in excess o f the coincidence error limit o f
the APC (B.10 ).

G.2 Determine the number concentration o f particles larger than the smallest particle size o f interest
in particles per millilitre expected to be observed in the diluted samples, XD , using Formula (G.1) :
XA
XD = (G.1)
1 ,3

where XA the coincidence error limit in particles per millilitre of the APC (B.10).
G.3 Determine the required dilution ratio for the calibration suspensions, DRR, using Formula (G.2) :
XC
DRR = (G.2)
XD
where XC is the number concentration of particles larger than the smallest size o f interest in particles
per millilitre obtained from the certificate o f analysis for the calibration suspension sample.
G.4 Veri fy that the glassware to be used for preparation and counting o f diluted calibration suspensions
meets the requirement o f 4.9 and that the diluent meets the required cleanliness o f 4.2 as follows:
a) fill a clean sample container (4.9) with clean diluent (4.2) to approximately 75 % o f its volume and
cover the container with a clean closure;
b) shake the sample vigorously by hand. Agitate the sample ultrasonically for at least 30 s then shake
it on a mechanical shaker for at least 1 min. Continue shaking the sample until it is to be analysed;
c) de-gas the sample under vacuum or ultrasonically until no sur facing bubbles are observed then
analyse immediately;
d) obtain five consecutive particle counts, each consisting o f at least 10 mL;
e) calculate the mean particle concentration, X , in particles per millilitre, for the five counts at the
channel setting corresponding to 1,5 times the threshold noise level o f the APC or the smallest
particle size o f interest.
If X is less than 0,005 XD then the clean diluent and glassware meet the requirements for use with this
annex. I f not, the glassware or the diluent or both, are insu fficiently clean for use with this annex and
G.4 shall be repeated a fter taking appropriate corrective action.

G.5 Three diluted calibration suspension samples shall be prepared using clean glassware (4.9) and
clean diluent (4.2) at an approximate dilution ratio o f DRR (G.3 ) using the volumetric dilution method
described in G.6 or the mass dilution method described in G.7. One o f these diluted samples shall be
analysed in 6.5. The other samples may be used i f the results o f the first diluted sample fail to meet the
data quality criteria o f 6.6 .

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G.6 Volumetric dilution method

a) Measure out the volume o f clean diluent, V0, necessary to achieve DRR into an empty, clean sample
container. Trans fer approximately 50 % o f the diluent into an empty, clean sample container.
b) Shake a primary or secondary calibration suspension sample vigorously by hand. Agitate the
sample ultrasonically for at least 30 s then shake it on a mechanical shaker for at least 1 min until
the sample is ready for use. De-gas the sample under vacuum or ultrasonically until no sur facing
bubbles are observed then, immediately, measure the sample volume, Vs, required to achieve DRR .
c) Trans fer the entire measured volume o f calibration suspension to the sample container containing
diluent [G.6 a)].
d) Rinse the container used to measure the calibration suspension sample [G.6 b)] with the remaining
clean diluent and trans fer all o f the liquid to the sample container containing diluent and sample
[G.6 a)].
e) Calculate the actual dilution ratio D R, using Formula (G.3) :
v0 + vS
DR = (G.3)
v0
f ) Proceed to G.8 .
G.7 Mass dilution method
a) Place an empty, clean sample container on the balance and either tare the balance or record the
mass o f the clean sample container.
b) Shake a primary or secondary calibration suspension sample vigorously by hand. Agitate the
sample ultrasonically for at least 30 s then shake it on a mechanical shaker for at least 1 min until
the sample is ready for use.
c) Estimate the volume o f calibration sample required to achieve DRR . De-gas the calibration
suspension sample under vacuum or ultrasonically until no sur facing bubbles are observed
then, using a pre-cleaned pipette (see 4.9), immediately extract that volume from the calibration
suspension sample and trans fer it into the clean sample container [G.7 a)], weigh and record the
mass o f the sample in the sample container as Ms .
d) Add the amount o f clean diluent to the sample container [G.7 c)] needed to obtain DRR and record
the total mass o f the sample plus diluent, Mt.
e) Determine and record the density o f the sample, ρ s , and the diluent, ρ d .
f ) Calculate the actual dilution ratio, DR, using Formula (G.4) :
 Mt − MS MS 
 + 
 ρd ρs 
DR = (G.4)
MS
ρs
g) Proceed to G.8 .

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ISO 1 1 1 71 : 2 02 0(E)

G.8 Record DR.

Figure G.1 — Procedure for dilution o f calibration suspension samples

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Annex H
(informative)
Verification o f particle size distribution o f calibration samples

H.1 Background
In order to calibrate automatic particle counters, Clause 6 requires that valid primary or secondary
calibration samples be used. In order to veri fy particle-counting accuracy, NIST RM8632x samples are
used in Annex E. Whether primary calibration sample, secondary calibration sample, or NIST RM8632x
sample, it is critical that the particle size distribution o f the sample is representative o f the specified
contaminant. Even though the specified contaminant was used to prepare the samples, the size
distribution can have been altered by sample preparation methodology, deterioration o f the samples
over time, contamination, or other causes. This annex provides guidance on how the particle size
distribution o f samples used in conjunction with this document can be verified.

H.2 Procedure
H.2 .1 Calibrate an APC in accordance with Clauses 5 and 6 using NIST primary calibration suspension
samples (4.4 ).

H.2 .2 Choose particle sizes and corresponding threshold voltage settings using the criteria
described in 6.2 .
H.2 .3 Prepare and analyse samples in accordance with 6.5 and 6.6 .

H.2 .4Calculate Rd, the ratio o f the mean particle concentration for each particle size to the re ference
mean particle concentration, using Formula (H.1) :
Xd
Rd =
Xd
,S

(H.1)
,R

where
Xd,S is the mean particle concentration for the sample at particle size d.
Xd,R is the mean particle concentration for the re ference at the same particle size.
For primary and secondary calibration samples, take Xd,R from the NIST SRM 2806x or secondary
sample certificate o f analysis, whichever is appropriate. For RM 8632x samples, Xd,R is the median
particle concentration for each size is given in Table A.1 .

H.2 .5 Plot Rd for each size as a function o f particle size d and connect the data points. I f the result is
a near horizontal line, this suggests that the size distribution o f the sample approximates that o f the
re ference suspension. I f the result is not horizontal or exhibits significant deviations from horizontal at
one or more sizes, this suggests that the sample is not representative o f the re ference suspensions and
should not be used.

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ISO 1 1 1 71 : 2 02 0(E)

H.2 .6 C alculate the ratio , Td , of the mean p article co ncentratio n fo r each p article s ize to the

co rres p o nding mean p article co ncentratio n fo r the s ame s amp le at 1 0 µm(c) us ing Fo rmula (H . 2 ) :
Xd ,S
Td =
X10 ,S
(H.2)
where
Xd ,S
i s the me an p ar ticle concentration for the s a mple at p a r ticle s i z e d.
X 10 , S
i s the me an p ar ticle concentration for the s a me s a mple at 10 µm(c) .

H.2 .7 Repeat H . 2 . 6 fo r the re ference s amp le.

H.2 .8 Plo t Td as a functio n of df o r the s amp le and fo r the re ference. C o nnect the s amp le data p o ints

and the re ference data p o ints to fo rm two lines . I f the two lines exhib it es s entially p arallel b ehavio ur, this

s ugges ts that the s ize dis trib utio n o f the s amp le ap p roximates that o f the re ference s us p ens io n and any

s ep aratio n b etween the two lines is the res ult o f co ncentratio n di fferences . I f no t, this s ugges ts that the

s amp le is no t rep res entative o f the re ference s us p ens io ns and s ho uld no t b e us ed.

H.2 .9 I f the s amp le p as s es the accep tance criteria given in H . 2 . 5 and H . 2 . 8 , then the s amp les are

accep tab le fo r us e in this do cument. I f no t, rep lace o r remake the s amp les a fter co rrecting the underlying

problem.

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 ISO 1 1 1 71 : 2 02 0(E)

Bibliography

[1 ] ISO 21501-3, Determination of particle size distribution — Single particle light interaction
methods — Part 3: Light extinction liquid-borne particle counter
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[3 ] ISO/TR 4808 :— 1) , Hydraulic fluid power — Interpolation method for particle count and filter
test data

[4] ISO/TR 4813:—2) , Hydraulic fluid power — Background, impact and use o f ISO 11171:2020 on
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[1 3 ] Verdegan B.M., Schwandt B.W., H olm C.E.,, Development o f a traceable particle counter
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1) Under preparation. Stage at the time o f publication: ISO/CD TR 4808:2020.

2) Under preparation. Stage at the time o f publication: ISO/DTR 4813:2020.
3) https://www.nist.gov/srm
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5) https://www.nist.gov/srm
6) https://doi.org/10 .6028/jres .121 .025
© ISO 2020 – All rights reserved 51
ISO 1 1 1 71 : 2 02 0(E)

[16] Kruger C.J.C., Constrained Cubic Spline Interpolation for Chemical Engineering Applications 7)

7) https://pages .uoregon.edu/dgavin/so ftware/spline.pdf

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