Iec 60865 1 PDF
Iec 60865 1 PDF
Iec 60865 1 PDF
STANDARD 4548-4
First edition
1997-12-01
A Reference number
ISO 4548-4:1997(E)
ISO 4548-4:1997(E)
Contents Page
3.8 Report of test results for life and cumulative efficiency ............ 18
Annexes
A Test parameters for initial particle retention efficiency test ....... 19
B Method for determining insolubles in test liquid samples for
initial particle retention efficiency .............................................. 20
C Test parameters for life and cumulative efficiency test ............. 24
D Method for determining insolubles in test liquid samples for
cumulative efficiency ................................................................. 25
E Details of equipment used in the mixing of test dust and liquid
slurry ......................................................................................... 28
F Bibliography .............................................................................. 30
© ISO 1997
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced
or utilized in any form or by any means, electronic or mechanical, including photocopying and
microfilm, without permission in writing from the publisher.
International Organization for Standardization
Case postale 56 CH-1211 Genève 20 Switzerland
Internet central@iso.ch
X.400 c=ch; a=400net; p=iso; o=isocs; s=central
Printed in Switzerland
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© ISO ISO 4548-4:1997(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide
federation of national standards bodies (ISO member bodies). The work of
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 of electrotechnical standardization.
ISO 4548 will consists of the following parts, under the general title Method
of test for full-flow lubricating oil filters for internal combustion engines:
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ISO 4548-4:1997(E) © ISO
Introduction
ISO 4548 establishes standard test procedures for measuring the
performance of full-flow lubricating oil filters for internal combustion
engines. It has been prepared in separate parts, each part relating to a
particular performance characteristic.
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INTERNATIONAL STANDARD © ISO ISO 4548-4:1997(E)
Section 1: General
1.1 Scope
This part of ISO 4548 specifies tests for determining the performance of full-flow lubricating oil filters for internal combustion
engines as follows.
Section 2: Initial particle retention efficiency. This gives the test procedures and parameters for the determination of the initial
particle retention efficiency of lubricating oil filter elements under defined test conditions. By reporting the results in
accordance with subclause 2.6, the probable retention efficiency for any particle size may be derived. The retention efficiency
is determined by the gravimetric method.
Section 3: Life and cumulative efficiency. This gives the test procedures and parameters for the determination of element life
and cumulative efficiency of lubricating oil filters. The cumulative efficiency is determined by the gravimetric method.
NOTE — By agreement between filter manufacturer and purchaser, tests on large filters can be conducted on the basis of tests carried out on
filters scaled-down in length. The relationship of the filter flow and test dust addition rate to the effective length of the filter medium should
be the same in the scaled-down tests as in the full size filter. For the purposes of this part of ISO 4548, a filter having a test flow rate
exceeding 100 l/min is considered large.
ISO 1219-1:1991, Fluid power systems and components — Graphic symbols and circuit diagrams — Part 1:
Graphic symbols.
ISO 4548-1:—1), Methods of test for full-flow lubricating oil filters for internal combustion engines — Part 1:
Differential pressure/flow characteristics.
ISO 11841-1:— 2), Road vehicles and internal combustion engines — Filter vocabulary — Part 1: Definitions of
filters and filter components.
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ISO 4548-4:1997(E) © ISO
ISO 11841-2:— 2), Road vehicles and internal combustion engines — Filter vocabulary — Part 2: Definitions
of characteristics of filters and their components.
ISO 12103-1:— 2), Road vehicles — Test dust for filter evaluation — Part 1: Arizona test dust.
ISO 12103-2:— 2), Road vehicles — Test dust for filter evaluation — Part 2: Aluminium oxide test dust.
1.3 Definitions
For the purposes of this part of ISO 4548, the definitions given in ISO 11841-1 and ISO 11841-2 apply.
2) To be published.
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© ISO ISO 4548-4:1997(E)
2.2.2 The sump shall be capable of holding a quantity of oil as given in annex A and shall be equipped with a
thermostatically controlled heater capable of maintaining the test temperature. The heater shall be arranged so that local
overheating of the oil is avoided. The by-pass return to the sump and the main filter outlet pipe shall terminate below the
surface of the oil in the sump when the oil is in circulation. The temperature shall be adjusted so that the stipulated test oil
viscosity is maintained within a limit of ± 3 mm2/s 3).
2.2.4 The two valves 3 and 8 (see figure 2) shall be used for the purpose of pressure and flow control. Needle valves or
diaphragm valves are recommended.
2.2.5 The flow-meter 4 shall be suitable for use with oil of 24 mm 2/s kinematic viscosity and shall register the flow in the
pipeline leading to the test filter with an accuracy of ± 2 %.
2.2.6 The pressure tapping 14 shall be made at five internal pipe diameters upstream of the filter inlet port. The filter inlet
and outlet pipes shall be straight and free from obstruction for eight internal pipe diameters upstream and 13 internal pipe
diameters downstream of the filter inlet and outlet ports.
2.2.7 The filter shall be mounted vertically in the test rig (see figure 1) in accordance with the requirements of ISO 4548-1
to ensure consistency of tests to enable meaningful comparisons to be made.
3) 1 mm2/s = 1 cSt
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ISO 4548-4:1997(E) © ISO
2.3.1 The test liquid for these tests shall be a straight mineral oil of ISO VG 100 (SAE 30) grade or ISO VG 150 (SAE 40)
grade (see [2] and [3]).
2.3.2 The oil shall be used at a kinematic viscosity of 24 mm2/s ± 3 mm2/s, at approximately 74 °C with ISO VG 100
(SAE 30) or at approximately 83 °C with ISO VG 150 (SAE 40).
Key
1 Insulated sump with thermostatically controlled heater, conical bottom and smooth internal surfaces
2 Motor-driven pump
3 Pressure-regulating valve
4 Flow meter
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5 ON-OFF valve
6 Slurry addition reservoir with a capacity equivalent to half the volume of the test filter ± 25 % with bleed screw in removable
cover (see figure 3)
7 Test filter
8 Flow-regulating valve
9 Three-way valve
10 Filtrate receptacle with a capacity of four times the volume of the test filter
11 ON-OFF valve
12 Three-way valve
13 Drain cock
14 Inlet pressure gauge
15 Indicating temperature controller
Figure 2 — Diagrammatic arrangement of test rig for initial particle retention efficiency test
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© ISO ISO 4548-4:1997(E)
Dimensions in millimetres
4) Suitable fused aluminium oxide test dusts can be obtained from the Motor Industry Research Association, Lindley, Nuneaton,
Warwickshire, UK. This information is given for the convenience of users of this part of ISO 4548 and does not constitute an endorsement by
ISO of the product named. Equivalent products may be used if they can be shown to lead to the same results.
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ISO 4548-4:1997(E) © ISO
2.4.2.4 The contents of the beaker shall then be thoroughly mixed by means of a high speed stirrer (see annex E).
2.4.2.5 Mixing shall proceed for at least 1 h immediately prior to placing in the slurry addition reservoir and commencing the
test.
2.5.1 General
This test procedure specifies the method of determining the retention efficiency of a filter element where a test dust of a
particular mean particle size, suspended in a small quantity of oil, is injected into the main flow of oil being passed through the
test filter under controlled conditions of temperature, pressure and flow rate. The period of injection will vary according to the
size of the test filter and the test flow rate but for practical purposes the evaluation may be regarded as a measure of the
instantaneous or single-pass retention efficiency of the test filter at the mean particle size of the test dust being used.
NOTE — The retention efficiency is a function of time, so the instantaneous or single-pass retention efficiency during the life of the filter
element may differ from the initial value.
2.5.2.1 In order to achieve this degree of cleanliness, the following procedure is suggested. Fit a
new clean-up filter in place of the test filter and drain all fluids from the test rig.
Pour a sufficient quantity of suitable flushing fluid into the test rig sump such that the pump does not cavitate when running.
Circulate the flushing fluid through the complete test rig system, including the slurry addition by intermittent change-over of
the appropriate valves, for at least 30 min at a flow rate which allows the clean-up filter to function at maximum efficiency in
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WARNING — Do not switch on the heater when using highly volatile or inflammable liquids.
Drain the test rig and refill with a sufficient quantity of the specified test oil so that the pump does not cavitate when running.
With the heater switched on, circulate the oil until the temperature stabilizes at the required figure and run the test rig for at least
20 min.
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© ISO ISO 4548-4:1997(E)
2.5.2.2 The cleanliness of the rig shall be determined by the following procedure.
a) Fit a new clean-up filter and fill the test rig with the required quantity of oil as given in annex A. Record the relative
density of the oil used.
b) With the heater switched on, circulate the oil until the temperature stabilizes at the required figure and run the test rig for at
least 20 min.
c) Take a 50 ml sump oil sample and analyse for percentage contaminant content as described in B.6. The result of this
analysis and calculation shall be referred to as the rig blank, and these rig blank tests shall be carried out prior to each
retention test on any test filter. Where the total contaminant content of the test liquid exceeds 60 mg/l the rig cleaning
operation shall be repeated until the rig blank contamination level is below the maximum mass allowed. The final rig blank
test result shall be used for correction of particle retention values in 2.6.
d) Remove the clean-up filter and replace its oil content with an equal quantity of clean test oil added to the sump.
2.5.3.1 Prepare the test rig as described in 2.5.2 and necessary dust increments as in 2.4.1 and 2.4.2.
2.5.3.2 The filter for test shall be installed vertically in the test rig as shown in figure 2 and the element by-pass component
shall remain operative. Care shall be taken to ensure that the test filter housing and any additional pipe- work are clean before
installation.
NOTE — The filter for test may be tested for fabrication integrity in accordance with ISO 2942 [2] prior to installation unless it is impractical
to disassemble the filter assembly.
2.5.3.3 The test oil shall be circulated through the test rig system via the by-pass pipe only. Valve 5 is closed. No liquid shall
pass through the test filter at this stage. The heater is switched on and the thermostat adjusted to a test temperature which
provides the specified oil viscosity shown in annex A. Allow temperature to stabilize. The viscosity of the test oil shall be
maintained within the defined limits for the duration of the test.
2.5.3.4 When the temperature has stabilized, the test oil shall be allowed to flow through the test filter while by- passing the
slurry addition reservoir.
2.5.3.5
5).
The flow through the test filter shall be adjusted to the required figure with the inlet pressure at a minimum of 40 kPa
2.5.3.6 Slurry, containing one of the test dusts, shall be added to the slurry addition reservoir. The test dusts are specified in
2.4.1 and the quantity of test dust and preparation of the slurry shall be in accordance with 2.4.2.
2.5.3.7 By the simultaneous operation of valves 11, 12 and 9, flow shall be directed through the slurry addition reservoir and
the effluent collected in the pre-cleaned receptacle 10. The volume of effluent collected shall be approximately four times the
volume of the test filter.
2.5.3.8 Reset valves 9 and 12 and close valve 11, allowing the test liquid to flow directly through the filter into the sump.
The test liquid flow shall then be stopped by closing valve 5 and opening valve 3.
2.5.3.9 Collect the dust not offered to the test filter as follows: place the beaker used for mixing the slurry beneath the drain
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cock 13 of the reservoir 6 and drain the reservoir by opening the cock and the top cover bleed screw.
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ISO 4548-4:1997(E) © ISO
2.5.3.10 Rinse all internal surfaces of the reservoir with 100 ml of petroleum spirit, collecting the rinsings in the beaker
referred to in 2.5.3.9.
2.5.3.11 The test dust content of the filter effluent shall be determined in accordance with annex B and the amount of test
dust in drainings and rinsings from 2.5.3.9 and 2.5.3.10 shall be determined in the same manner, except that all the rinsings
shall be used and finally washed through the membrane with 100 ml of petroleum spirit.
2.5.3.12 The filter bowl and test element shall be removed and the element discarded. In the case of sealed unit type filters,
the filter shall be discarded.
2.5.3.13 The retention efficiency of the test filter relative to the particular grade of test dust used shall be calculated as
defined in clause 2.6.
2.5.3.14 The test rig shall be prepared as in 2.5.2 before repeating the test as in 2.5.3.1 to 2.5.3.13 using the remaining grades
of test dust. A clean element shall be used for each separate test.
where
m1 is the mass of test dust transmitted after correction, in grams:
m1 = m – m0
in which
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6) For spin-on filters with a screwed adaptor block, a screw-on cap of minimum volume connecting the inlet with outlet may be used.
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© ISO ISO 4548-4:1997(E)
Grade Supplier 50 % mean particle size Batch No. Filter retention efficiency
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ISO 4548-4:1997(E)
curve
Figure 4 — Typical initial particle retention efficiency
ISO
© ISO ISO 4548-4:1997(E)
3.2.4 The two valves (3 and 10 in figure 5) shall be used for the purpose of pressure and flow control in conjunction with
the variable speed control for the motor-driven pump. Needle valves or diaphragm type valves are recommended.
3.2.5 The flow meter 5 shall be suitable for use with oil of 24 mm 2/s kinematic viscosity and shall register the flow in the
pipeline leading to the filter with an accuracy of ± 2 %.
NOTE — To be suitable for use with the tests specified in other parts of ISO 4548, the flow meter should also be capable of use with oil of
500 mm2/s kinematic viscosity, and cope with the abrasive material used in this test without undue wear.
3.2.6 The filter shall be mounted vertically in the test rig in accordance with the requirements of ISO 4548-1 to ensure
consistency of tests to enable meaningful comparisons to be made.
3.2.7 Tappings for the measurement of differential pressure across the complete filter shall be made at five internal pipe
diameters upstream of the filter inlet port and 10 internal pipe diameters downstream from the filter outlet port. The inlet and
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outlet pipes shall be straight and free from obstruction for eight internal pipe diameters upstream and 13 internal pipe diameters
downstream of the filter inlet and outlet ports.
7) 1 mm2/s = 1 cSt
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ISO 4548-4:1997(E) © ISO
3.4.1 The test liquid for these tests shall be a straight mineral oil of ISO VG 100 (SAE 30) grade or ISO VG 150 (SAE 40)
grade with addition of anti-static additive (see annex C)
3.4.2 The oil shall be used at a kinematic viscosity of 24 mm2/s ± 3 mm2/s, at approximately 74 °C with ISO VG 100
(SAE 30) or at approximately 83 °C with ISO VG 150 (SAE 40).
Key
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1 Sump (preferably insulated) incorporating a thermostatically controlled heater, and cooler if required
2 Motor-driven pump with variable speed control
3 Pressure-regulating by-pass valve
4 ON-OFF valve
5 Flow meter
6 Filter under test
7 Thermocouple connected to a temperature indicator
8 Pressure gauge
9 Differential pressure gauge, to measure the pressure drop across the filter1)
10 Flow-regulating valve
11 Sampling cock
1) For cases where mercury manometer(s) is (are) used in place of item 9, it will be necessary to fit isolating valve(s) in the high-pressure leg(s) of the
manometer pipework.
Figure 5 — Diagrammatic arrangement of test rig for life and cumulative efficiency test
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© ISO ISO 4548-4:1997(E)
3.5.2.1 A sufficient quantity of ISO 12103-A2 dust to complete the test shall be dried in an oven at a temperature of 105 °C ±
5 °C for at least 1 h. The dried dust shall then be stored ready for use in a desiccator.
3.5.2.2 When required for use in the test rig a quantity of ISO 12103-A2 test dust shall be weighed into a clean beaker and to
it shall be added a volume of test liquid to make a total volume of one litre. The mass of dust shall be within ± 10 mg of the
calculated quantity given in annex C.
The contents of the beaker shall then be thoroughly mixed by means of a high speed stirrer and ultrasonic probe (see annex E
for equipment details).
Mixing shall be carried out by first placing the stirrer blades close to the bottom of the beaker and stirring at a speed of
approximately 2 000 r/min. The ultrasonic probe shall then be immersed into the liquid to a depth of 30 mm from the tip end
and the power adjusted to produce an amplitude of 6 µm, peak to peak.
The combined mechanical stirring and ultrasonic dispersion of the dust shall proceed for one hour immediately prior to adding
to the sump.
NOTES
1 Test dust is normally supplied in different size jars. This dust, in storage, will tend to precipitate and quantities removed from the top of
the jar will not be representative of the original particulate distribution. To ensure that the test dust used meets the requirements of 3.5.1, the
test dust must be thoroughly mixed before individual increments are removed for weighing.
2 It is essential that the test be completed without interruption.
Before commencing particle retention efficiency tests, it is essential that the test rig be cleaned such that the results obtained
are not influenced by residual contaminant in the test rig circuit. The total contaminant content of the test fluid shall not exceed
60 mg/l.
3.6.2.1 In order to achieve this degree of cleanliness, the following procedure is suggested. Fit a
new clean-up filter in place of the test filter and drain all fluids from the test rig.
Pour sufficient quantity of suitable flushing fluid into the test rig sump such that the pump does not cavitate when running.
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ISO 4548-4:1997(E) © ISO
Circulate the flushing fluid through the complete test rig system, including the slurry addition reservoir by intermittent
changeover of the appropriate valves, for at least 30 min at a flow rate which allows the clean-up filter to function at maximum
efficiency in removing residual contaminant.
WARNING — Do not switch on the heater when using highly volatile or inflammable liquids.
Drain the test rig and refill with a sufficient quantity of the specified test oil so that the pump does not cavitate when running.
With the heater switched on, circulate the oil until the temperature stabilizes at the required figure and run the test rig for at
least 20 min.
Drain the test rig and remove the clean-up filter.
3.6.2.2 The cleanliness of the rig shall be determined by the following procedure.
a) Fit a new clean-up filter and fill the test rig with the required quantity of oil as given in annex C. Record the relative
density of the oil used.
b) With the heater switched on, circulate the oil until the temperature stabilizes at the required figure and run the test rig for at
least 20 min.
c) Take a sump oil sample and analyse for contaminant content. This figure shall be less than 0,007 % by mass
(approximately 60 mg/l) before proceeding further. If necessary, repeat cleaning operations using clean-up filter until the
contaminant level is below the maximum specified.
d) Remove the clean-up filter and replace its oil content with an equal quantity of clean test oil added to the sump.
during the transfer period, using the stirrer at a speed of approximately 1 000 r/min.
3.6.3.8 Take 50 ml samples every 20 min for a period of 2 hours. At each sample interval adjust the volume of oil in the
sump to its original value, as specified in annex C.
3.6.3.9 Analyse oil samples as in annex D.
9) For spin-on filters with a screwed adaptor block, a screw-on cap of minimum volume connecting the inlet with outlet may be used.
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© ISO ISO 4548-4:1997(E)
3.6.3.10 Plot percentage contaminant in samples against contaminant added, in grams. This curve should be linear.
3.6.3.11 The graph drawn should not deviate more than ± 5 % from theoretical concentration, based on total mass of oil and
contaminant added to the sump, at any point on the graph. A typical calibration graph is shown in figure 6. Where results are
outside the specified limits, it will be necessary to modify the test rig system until the requirements are satisfied.
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ISO 4548-4:1997(E) © ISO
3.6.4.2 Prepare the test rig as detailed in 3.6.2 and install the test filter.
The filter for test shall be installed vertically in the test rig as shown in figure 5 and the element by-pass component shall
remain operative. Care shall be taken to ensure that the test filter housing and any additional pipe- work are clean before
installation.
NOTE — The filter for test may be tested for fabrication integrity in accordance with ISO 2942 prior to installation, unless it is impractical to
disassemble the filter assembly.
3.6.4.3 Prepare sufficient test dust as detailed in 3.5.2.1 and sufficient clean oil sample containers (100 ml capacity) to cover
the test requirements.
3.6.4.4 Open by-pass valve 3 (see figure 5), close on-off valve 4, set the heater control to the required temperature and run
the pump at low speed.
3.6.4.5 When the required oil temperature has been attained, open valve 4, close by-pass valve 3 and adjust the flow rate
through the test filter to 50 % of the test flow rate (annex C) by increasing the pump speed.
3.6.4.6 Allow the temperature to stabilize and adjust the pump speed to obtain 125 % of the test flow rate (annex C) through
the test filter.
3.6.4.7 Gradually open by-pass valve 3, until the flow through the test filter is set to the test flow rate (annex C).
3.6.4.8 Set the oil sample line flow to approximately 0,5 l/min by adjusting valve 11 and, when stabilized, re-adjust pump
speed to correct the flow through the test filter to the test flow rate (annex C). This flow rate shall be maintained constant
throughout the test by further adjustments to by-pass valve 3.
3.6.4.9 Take a 50 ml sample from the sample line and replace with 50 ml of clean test oil, added to the sump.
3.6.4.10 Transfer the previously prepared slurry which is contained in the beaker (see 3.5.2.2) to the sump via a peristaltic
pump. Precalibrate the transfer rate to give the required rate of contaminant addition (see annex C). Continuously stir the slurry
during the transfer period, using the stirrer at a speed of approximately 1 000 r/min. Continuously add the slurry until the test
terminating pressure across the filter attains the value specified in annex C.
3.6.4.11 Take 50 ml samples from the sample line every 20 min thereafter and at the test end point. At each sample interval
adjust the volume of oil in the sump to its original value, as specified in annex C.
3.6.4.12 Record the temperature, and the pressure differential across the test filter, immediately prior to each 50 ml sample.
3.6.4.13 Take a final 50 ml sample at test end point (see annex C).
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3.6.4.14 Record the total mass of dust added to the sump before analysing the oil samples as detailed in annex D.
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© ISO ISO 4548-4:1997(E)
mi is the initial mass of insolubles in the sump plus the mass of cumulative solids added;
ms is the volume of oil in the sump times the volumic mass of the oil.
A graph as shown in figure 7 may be drawn, plotting cumulative efficiency against grams of contaminant added.
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ISO 4548-4:1997(E) © ISO
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© ISO ISO 4548-4:1997(E)
Annex A
(normative)
Test liquid: Straight mineral oil of ISO VG 100 (SAE 30) grade or ISO VG 150 (SAE 40) grade.
Test oil operating kinematic viscosity: 24 mm2/s ± 3 mm2/s, at approximately 74 °C with ISO VG 100 (SAE 30), or
approximately 83 °C with ISO VG 150 (SAE 40).
The test flow rate (through the filter), qV, in litres per second, shall be as specified by the customer or the manufacturer of the
filter. In the absence of such a specification, the test flow rate shall be 1,5 l/s per square metre of filter media area.
NOTE — In the following the volume of test oil (litres) and the mass of test dust (grammes) are proportional to the test flow rate ( qV), and
they are numerically equal to the product of a factor and the flow rate.
Volume of test oil: 15 × qV, in litres. The minimum volume shall be 6 l. Test
dust: Grades M2, M3, M4 and M5 (see 2.4.1).
Mass of dust to be injected: (8 × qV) ± 0,002 g.
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ISO 4548-4:1997(E) © ISO
Annex B
(normative)
Method for determining insolubles in test liquid samples for initial particle
retention efficiency
B.1 Introduction
This annex describes the method used for determining the mass-to-mass concentration of insolubles in test liquid samples for
the initial particle10)retention efficiency test. The petroleum distillate insolubles are separated from the oil by vacuum filtration.
Two membranes are used for each sample analysed: one is used for filtering the sample and the other as a control so that a
correction can be made for any change in mass of the sample filtering membrane that may result from changes in humidity,
temperature, etc.
B.2 Equipment
The following equipment is typical of that for filtering the sample (see figure B.1). Any suitable apparatus which can
accommodate the particular membranes specified by b in figure B.1 may be used.
B.4.1 Wash the filter holder, and sufficient Petri dishes to cover the test requirements
11) in warm water to which a little
detergent has been added. Remove the filter holder and the Petri dishes from the bath and assemble the filter holder
components, but do not tighten.
10) Suitable membrane discs can be obtained from Millipore Corp., Bedford, Massachussets 01730, USA, and from Sartorius Membranfilter
GmbH, Göttingen, Germany. This information is given for the convenience of users of this part of ISO 4548 and does not constitute an
endorsement by ISO of the product named. Equivalent products may be used if they can be shown to lead to the same results.
11) Each oil sample to be analysed requires the use of two membranes: one for filtering the sample, the other to be placed beneath the
filtering membrane as a control membrane, to enable corrections to be made for humidity, temperature, etc., when weighing.
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© ISO ISO 4548-4:1997(E)
B.4.2 Hold the filter holder and the Petri dishes with clean tongs and rinse thoroughly with acetone delivered from a force-
feed bottle. The holder and the Petri dishes should be handled with tongs for the remainder of the determination.
B.4.3 Place the filter holder and the Petri dishes in an oven at a temperature of 105 °C ± 5 °C for at least 1 h.
B.4.4 Remove the filter holder from the oven and place it in a desiccator to cool for a minimum period of 1 h.
B.4.5 Remove the Petri dishes from the oven and place them in a desiccator to cool for a minimum period of 1 h.
Key
a Filter holder
b Two cellulose acetate, nitrate or ester membranes, pore size 0,8 µm; 47 mm or 60 mm diameter according to equipment available
c Spring-loaded clamp
d Earth terminal for connecting a wire to discharge static charges to earth e
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Figure B.1 — Typical fixation apparatus — Membrane filter holder assembled on vacuum flask
B.4.6 Remove the Petri dishes from the desiccator, place the filter membranes as indicated by b in figure B.1 in each Petri
dish, and replace them in the oven for at least 1 h.
B.4.7 Remove the Petri dishes with membranes from the oven, and place in a desiccator to cool for at least 1 h. Remove
from the desiccator and stand in atmosphere for at least 1 h, then remove each membrane in turn and weigh it to the nearest 0,1
mg. Record the mass and replace in a Petri dish until required. Label and mark each Petri dish as appropriate.
NOTE — The Petri dishes and membranes may be weighed together directly from the desiccator, provided the balance pan is enclosed and the
weighing chamber contains a desiccant.
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ISO 4548-4:1997(E) © ISO
B.4.8 Remove the filter holder from the desiccator, place the appropriate pre-weighed control membrane, and sample
filtering membrane, with the control membrane beneath filtering membrane, and assemble the filter holder. Install on suitable
vacuum flask, ensure that a filter holder is suitably earthed, and apply a vacuum of 65 kPa.
B.4.9 Weigh the receptacle containing the effluent and determine the mass of the test liquid to the nearest 0,1 g by
subtracting the initial clean receptacle mass.
B.4.10 Take approximately 10 % of the effluent sample, after thorough mixing to ensure that it is representative, and
determine its mass to the nearest 0,1 g in a clean pre-weighed measuring cylinder. Mix, by shaking, with an equal volume of
petroleum distillate. Pour slowly on to the clamped membranes and wash through with a similar volume of petroleum distillate
as before, assisted by a vacuum of not more than 65 kPa.
B.4.11 During filtration, wash the inside of the filter holder with petroleum distillate until clean and free from oil, allowing
the washings to pass on to the membranes.
B.4.12 When the liquid has passed through the membranes, continue the washing process until a further 200 ml has been
used.
B.4.13 Dismantle the filter holder and remove the membranes with care, keeping them horizontal so that no insolubles are
lost, and return the membranes to their appropriate Perti dishes and replace them in an oven set at 105 °C ± 5 °C for at least 1
h.
B.4.14 Remove the Petri dishes and membranes from the oven and place them in a desiccator to cool for at least 1 h.
B.4.15 Remove the Petri dishes and membranes from the desiccator and stand in atmosphere for at least 1 h. Remove each
membrane in turn, weigh to the nearest 0,1 mg, and record its mass.
NOTE — The Petri dishes and membranes may be weighed together directly from the desiccator, provided the balance pan is enclosed and
the weighing chamber contains a desiccant.
B.4.16 The mass of insolubles present in the weighed oil sample shall then be determined as indicated in
B.4.16.1 and B.4.16.2.
B.4.16.1 Correct the clean filtering membrane mass by applying the difference in mass occurring on the control membrane
after filtering (i.e. add the difference if an increase occurs or subtract the difference if a decrease occurs).
B.4.16.2 Deduct the corrected mass of clean filtering membrane from the mass of used filtering membrane to obtain the
corrected increase in membrane mass due to solids from the oil sample.
B.4.17 Express results as total mass of insolubles present in the complete effluent sample by using the multiplication factor
obtained from the masses recorded in B.4.9 and B.4.10.
The amount of test dust in the drainings and rinsings from the mixing beaker and slurry addition reservoir (2.5.3.9 and
2.5.3.10) shall be determined as described in B.4.1 to B.4.16 except that all the rinsings shall be used and finally washed
through the membrane with 100 ml of petroleum distillate. The final result shall be used for correction in the calculations
detailed in subclause 2.6.
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© ISO ISO 4548-4:1997(E)
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ISO 4548-4:1997(E) © ISO
Annex C
(normative)
Test liquid: Straight mineral oil of ISO VG 100 (SAE 30) grade or ISO VG 150 (SAE 40) grade with the addition of anti-static
additive12) in the concentration of 0,25 ml per 10 litres.
Test oil operating kinematic viscosity: 24 mm2/s ± 3 mm2/s at approximately 74 °C with ISO VG 100 (SAE 30), or at
approximately 83 °C with ISO VG 150 (SAE 40).
Test flow rate (through the filter), qV, in litres per second, shall be as specified by the customer or the manufacturer of the filter.
In the absence of such a specification, the test flow rate should be 1,5 l/s per square metre of filter media area.
Volume of test oil: 15 × qV, in litres (minimum 6 l).
Test rig by-pass flow: approximately 25 % times qV, in litres per second.
Contaminant: ISO 12103-A2 (ISO Fine — see 3.5.1).
Contaminant add rate: 10 × qV, in grams per hour.
Test end point: 50 kPa increase above initial pressure drop.
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12) A suitable anti-static additive is STADIS 450, available from Du Pont Petroleum Additives, Wilmington, DE 19898, USA. This
information is given for the convenience of users of this part of ISO 4548 and does not constitute an endorsement by ISO of the product
named. Equivalent products may be used if they can be shown to lead to the same results.
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© ISO ISO 4548-4:1997(E)
Annex D
(normative)
D.1 Introduction
This annex describes the method used for determining the mass-to-mass concentration of insolubles in test liquid samples for
the cumulative efficiency test. The petroleum distillate insolubles are separated from the oil by vacuum filtration. Two
membranes are used for each sample analysed: one is used for filtering the sample and the other as a control so that a
correction can be made for any change in mass of the sample filtering membrane that may result from changes in humidity,
temperature, etc.
D.2 Equipment
The equipment shall be as given in B.2
D.4.4 Remove the filter holder from the oven and place it in a desiccator to cool until required for further use.
D.4.5 Remove the sample containers from the oven and place them in a suitable covered glass beaker to cool to room
temperature.
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D.4.6 When cooled, label and weigh the sample containers to the nearest 0,1 mg, record the mass and replace them in a
beaker. (These sample containers will then be used for sampling purposes.)
D.4.7 Remove the Petri dishes from the oven, and place them in a desiccator to cool for a minimum period of 1 h.
D.4.8 Remove the Petri dishes from the desiccator, place a filter membrane as indicated by b in figure B.1 in each Petri
dish, and replace in the oven for at least 1 h.
13) Each oil sample to be analysed requires the use of two membranes: one for filtering the sample, the other to be placed beneath the
filtering membrane as a control membrane, to enable corrections to be made for humidity, temperature, etc., when weighing.
25
ISO 4548-4:1997(E) © ISO
D.4.9 Remove the Petri dishes with membranes from the oven, and place in a desiccator to cool for at least 1 h. Remove
from the desiccator and stand in atmosphere for at least 1 h, then remove each membrane in turn and weigh it to the nearest 0,1
mg. Record its mass, and replace it in the Petri dish until required. Label and mark each Petri dish as appropriate.
NOTE — The Petri dishes and membranes may be weighed together directly from the desiccator, provided the balance pan is enclosed and
the weighing chamber contains a desiccant.
D.4.10 Remove a pre-weighed sample container and collect approximately 50 ml of the oil to be analysed, taken from the
test rig sample point. Weigh it to the nearest 0,1 mg and record its mass.
D.4.11 Subtract the mass of the sample container from the total mass, to obtain the mass of the oil sample.
D.4.12 Remove the filter holder from the desiccator, place the appropriate pre-weighed control membrane, and sample
filtering membrane, into the filter holder, with control membrane beneath the filtering membrane, and assemble the filter
holder. Install on a suitable vacuum flask, ensure that filter holder is suitably earthed, and apply a vacuum of approximately 65
kPa.
D.4.13 Pour the oil sample (i.e. 50 ml) on to the membrane 14) and simultaneously wash through with 250 ml petroleum
distillate delivered from a force-feed wash-bottle. Continue to wash the oil sample container until clean and free from traces of
oil, allowing oil washings to pass through the membranes.
NOTE — It is important that the minimum amount of petroleum distillate be used
D.4.14 Continue washing oil through the membrane until a total of 500 ml petroleum distillate has been used. There should
be no traces of oil after this operation.
D.4.15 The filter holder shall then be dismantled, and the filtering membrane and control membrane returned to their
appropriate Petri dishes and replaced in an oven set at 105 °C ± 5 °C for at least 1 h.
D.4.16 Repeat the procedure from D.4.10 to D.4.15 for each oil sample to be analysed in conjunction with the remaining
pre-weighed membranes, prepared filter holder, etc.
D.4.17 Remove the Petri dishes containing membranes from the oven and place them in a desiccator to cool for a minimum
period of 1 h.
D.4.18 Remove the Petri dishes containing membranes from the desiccator and stand in atmosphere for at least 1 h, then
remove each membrane in turn and weigh to the nearest 0,1 mg and record its mass.
NOTE — The Petri dishes and membranes may be weighed together directly from the desiccator, provided the balance pan is enclosed and
the weighing chamber contains a desiccant.
D.4.19 The mass of insolubles present in the weighed oil samples shall then be determined as indicated in
D.4.19.1 and D.4.19.2.
D.4.19.1 Correct the clean filtering membrane mass by applying the difference in mass occurring on the control membrane
after filtering (i.e. add the difference if an increase occurs, or subtract the difference if a decrease occurs).
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14) Filtering the sample is usually enhanced by adding approximately 50 ml petroleum distillate to the sample container and mixing by hand
before pouring the sample on to the membrane.
26
© ISO ISO 4548-4:1997(E)
D.4.19.2 Deduct the corrected mass of clean filtering membrane from the mass of used filtering membrane to obtain the
corrected increase in membrane mass due to solids from the oil sample.
D.4.20 Express results as total mass of insolubles present in the sump oil prevailing at the time of removing the sample for
substitution in formula for calculating cumulative efficiency (see 3.7.2).
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ISO 4548-4:1997(E) © ISO
Annex E
(normative)
Details of equipment used in the mixing of test dust and liquid slurry
15) Kerry Ultrasonics Ltd, Hunting Gate, Wilbury Way, Hitchin, Hertfordshire, SG14 0TQ, U.K..
16) Park Products Ltd, Ordnance Street, Blackburn, Lancashire, BB1 3BN, U.K.
This information is given for the convenience of users of this part of ISO 4548 and does not constitute an endorsement by ISO of the
companies named. Equivalent products may be used if they can be shown to lead to the same results.
28
© ISO ISO 4548-4:1997(E)
Figure E.1 — Ultrasonic probe dimensions Figure E.2 — Stirrer paddle dimensions
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ISO 4548-4:1997(E) © ISO
Annex F
(informative)
Bibliography
[1] ISO 2942:1994, Hydraulic fluid power — Filter elements — Verification of fabrication integrity and
determination of the first bubble point.
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ISO 4548-4:1997(E) © ISO
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ICS 27.020
Descriptors: internal combustion engines, lubrification systems, oil filters, tests, performance tests, determination, efficiency.