IP 387/16 ASTM D2068-10

Determination of filter blocking tendency

0 Introduction IP 476, Petroleum liquids — Automatic pipeline

sampling (EN ISO 3171).
This test method covers 3 procedures using
different filter media. The result of any test is IP 367, Petroleum products — Determination of
dependent on the filter mandated in the procedure. application of precision data in relation to methods
If a specification requires a specific procedure of test (ISO 4259).
do not substitute a different procedure or filter
without agreement from the specifier. ISO 5636-5, Paper and board — Determination of
air permeance and air resistance (medium range)
1 Scope Part 5 Gurley method.

This standard specifies a method for the 3 Definitions

determination of the filter blocking tendency
(FBT) and filterability of middle distillate fuel oils For the purposes of this European Standard, the
and non-petroleum liquid fuels such as biodiesel, following terms and definitions apply.
where the end use demands an exceptional degree
of cleanliness. The method covers 3 procedures 3.1
and associated filter types, and is applicable to filter blocking tendency (FBT)
fuels within the viscosity range of 1,5 mm2/s to a calculated dimensionless value that defines
6,0 mm2/s at 40 °C. the filter blocking tendency of a fuel caused by
particulates. The value is calculated using the
A change in filtration performance after storage pressure across the filter or volume of fuel filtered
or pre-treatment, such as cold soaking, can be at the end of the test. Depending on the outcome
used to indicate potential filter blocking problems of the test, two different equations are applied.
or small changes in fuel condition. See section 9 Calculation.

WARNING — The use of this standard may involve 3.2

hazardous materials, operations and equipment. filterability
This standard does not purport to address all of the relationship between the volume of material
the safety problems associated with its use. It is passed through the filter and the measured
the responsibility of the user of this standard to pressure.
establish appropriate safety and health practices
and determine the applicability of regulatory NOTE The filterability of the fuel can be assessed by
limitations prior to use. recording the pressure when a specific volume of fuel
has passed through the filter. It can also be assessed by
evaluating a volume versus pressure graph. See Annex
2 Normative references B.

The following referenced documents are 3.3

indispensable for the application of this document. cold soak
For dated references, only the edition cited applies. the exposure of the test portion to a constant
For undated references, the latest edition of the reduced temperature for a period of time.
referenced document (including any amendments)
applies.

IP 475, Petroleum liquids — Manual sampling (EN

ISO 3170).

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4 Principle

A test portion of the fuel to be analysed, is passed

at a constant 20 ml/min rate of flow through a
specified filter medium. The pressure difference
across the filter and the volume of fuel passing
the filter are monitored until the pressure reaches
105 kPa or the volume of fuel passing through the
filter medium reaches 300 ml. The pressure (see
3.1) and flow are then used to calculate the filter
blocking tendency. The filterability of the fuel can
also be assessed by reporting the pressure when
a specified volume of fuel passes through the
filter or by reporting the volume of fuel passing
through the filter that causes a pressure of
105 kPa.
Figure 1 Assembly of Filter A
The filters specified for procedures A and B are
both 1,6 μm nominal pore diameter, however, the 5.2.2 Filter B (for procedure B)
filter for procedure B offers ease of use as it is
pre-assembled. 5.2.2.1 Filter housing, disposable polypropylene
‘syringe type’ with Luer and taper fittings, and
The pre-assembled filter specified for procedure C factory fitted filter media.
has a 5 μm nominal pore diameter.
The filter, as shown in Figure 2, is used with an
5 Apparatus 1 adaptor (5.9) to allow the test portion to input
through the taper fitting and exit from the Luer
fitting. The filter medium is supported by a coarse
5.1 General
glass fibre support pad as shown in Figure 2.
The apparatus as described in Annex A and shown Filters fitted with additional pre-filtration are not
in Figure A.1. permitted and can affect FBT results.

5.2 Filter media and assemblies

5.2.1 Filter A (for procedure A)

5.2.1.1 Filter housing, stainless steel, 13 mm

diameter with a Luer fitting at the top where it
connects with the filtration apparatus. Figure 1
shows the assembly.

5.2.1.2 Filter media, glass fibre grade GF/A,

1,6 μm nominal pore diameter, 13 mm diameter
and with an effective filtration area of 63,6 mm2
– 78,6 mm2. Filter media shall be batch selected
to have a Gurley time (ISO 5636-5) of between Figure 2 Filter B
12,5 s and 13,4 s for 300 ml.
5.2.2.2 Filter media, glass fibre grade GF/A,
NOTE The effective filtration area was determined by 1,6 μm nominal pore diameter and effective
measuring the diameter of the patch of sediment in the filtration area of 95,0 mm2 – 113,1 mm2. The
centre of the filter media. filters shall be batch selected and quality controlled
(using ISO 5636-5 for example) for equivalence
with the assembled filter A.

NOTE The effective filtration area was determined by

1 A list of suppliers is obtainable from the Energy measuring the diameter of the patch of sediment in the
Institute. centre of the filter media.

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5.2.3 Filter C (for procedure C) 5.9 Adaptor, only for use with procedure B,
to convert the Luer fitting on the apparatus to a
5.2.3.1 Filter housing, disposable polypropylene fitting compatible with the tapered fitting on Filter
‘syringe type’ filter housing, as shown in Figure B.
3, which has Luer and taper fittings, and factory
fitted filter media. The test portion inputs via the 5.10 Anti splash tubing, nylon or silicone
Luer fitting. rubber, approximately 4 mm inner diameter for
Filters A and C, and 6 mm inner diameter for Filter
The filter medium is held above concentric/ B.
segmented ribbed channels and the exit port is
recessed and segmented to eliminate localized 6 Preparation of apparatus
filter blocking.
6.1 Verification
5.2.3.2 Filter media, nylon, 5 μm nominal pore
diameter and effective filtration area of 143,2 mm2 6.1.1 Pressure and temperature
– 165,2 mm2. The filters shall be batch selected
and quality controlled.
Follow the manufacturer’s instructions for
verifying that the pressure and temperature
NOTE The effective filtration area was determined by
readings are in accordance with the tolerances
measuring the diameter of the patch of sediment in the
centre of the filter media. given in A.1.3 and 5.6 respectively. Verify the
pressure reading at least every 6 months or if the
apparatus has not been used for the previous 3
months. Verify the temperature reading at least
every 12 months. If the readings do not meet the
specified tolerances, calibrate the sensors (6.2.1).

6.1.2 Flow rate

Follow the manufacturer’s instructions for

verifying that the flow rate is 20 ml/min ± 1 ml/
min through a filter assembly.

Figure 3 Filter C Verify the flow rate, by measuring the volume

pumped during a 15 min period, at least once a
5.3 Measuring cylinder, polypropylene or month, using a suitable measuring cylinder. The
glass with a capacity of 25 ml with graduations volume should be between 285 ml and 315 ml.
every 0,5 ml.
More frequent checks on the flow rate can be
5.4 Measuring cylinder, polypropylene or made by measuring the volume during a 1 min
glass with a capacity of at least 500 ml with period using a 25 ml measuring cylinder. The
graduations every 5 ml. volume should be between 19 ml and 21 ml.

5.5 Stopwatch, (optional) capable of If the flow rate is incorrect calibrate the pump
measuring to the nearest 0,2s, required if timing (6.2.2).
not automated.
6.2 Calibration
5.6 Thermometer, IP 15C. Alternative
electronic or liquid in glass type thermometers 6.2.1 Pressure and temperature
with a range of at least 15 °C to 25 °C and an
accuracy of ± 0,5 °C or better are suitable. Follow the manufacturer’s instructions to calibrate
the pressure and temperature measuring devices.
5.7 Forceps, spade ended, for use with Filter
A. 6.2.2 Flow rate

5.8 Spanners, plastic or metal, for use with 6.2.2.1 Follow the manufacturer’s instructions
Filter A.
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to set and lock the mechanical flow adjustment 7 Samples and sample preparation
control on the pump.
7.1 Unless otherwise specified or required in
6.2.2.2 A filter assembly shall be fitted when the 7.2, samples shall be obtained by the procedures
flow rate is calibrated. described in IP 475 or IP 476 and be prepared as
described in 7.1.1 to 7.1.5.
6.3 Apparatus assembly
7.1.1 Obtain at least 400 ml of a representative
Assemble the apparatus as shown in Figure A.1, aliquot of the sample to be tested in an epoxy-lined
without the filter unit connected. can or dark glass bottle of at least 500 ml capacity.
The containers shall have been previously flushed
6.4 Filter assembly three times with the product to be sampled.

Assemble the filter appropriate to the test 7.1.2 Measure the temperature (5.6) of the fuel
procedure specified. in the container and adjust to 15 °C to 25 °C, if
appropriate.
6.4.1 Filter A (for procedure A)
7.1.3 Shake the fuel container vigorously
for 120 s ± 5 s, and then allow to stand on a
Assemble the filter as shown in Figure 1 using a
vibration-free surface for 300 s.
new filter medium handled with the forceps (5.7)
taking care not to damage the filter medium. Place
the medium into the holder with the face marked 7.1.4 Place at least 350 ml of the sample
with a grid pattern uppermost. The spanners into the fuel reservoir beaker and check that
(5.8) may be used to assist in assembling or the temperature (5.6) is still within the range of
disassembling the housing. Attach a suitable 15 °C to 25 °C. Record the actual temperature.
length (typically 80 mm to 90 mm) of anti splash If any undissolved water is apparent in the fuel
tubing (5.10) to the outlet of the filter assembly at this stage, abandon the test and report the
if required. presence of water.

NOTE 1 It is most important that the filter unit 7.1.5 Place the pump suction pipe into the
components are assembled in the exact configuration reservoir beaker and run the pump. Flush the
shown in Figure 1. system through with the sample by allowing
approximately 20 ml of the sample to flow into
NOTE 2 Over or under tightening of the Filter A the receiver beaker. Stop the pump and discard
assembly can lead to erroneous results. any fuel from the fuel receiver beaker.

6.4.2 Filter B (for procedure B) 7.2 Samples subject to specific pretreatment,

such as specified in cold soak methods, shall
6.4.2.1 Attach a suitable length (typically 80 mm follow the prescribed instructions particularly
to 90 mm) of anti splash tubing (5.10) to the the temperature requirements, sample mixing
outlet of the filter assembly if required. and positioning of the pump suction pipe during
flushing of the system.
6.4.2.2 Attach the adaptor (5.9) to the Luer fitting
on the outlet of the apparatus. 8 Procedures A, B and C

6.4.3 Filter C (for procedure C) 8.1 General

Attach a suitable length (typically 80 mm to 90 Test fuels having an extremely high blocking
mm) of anti splash tubing (5.10) to the outlet of tendency may cause the pressure reading to rise
the filter assembly if required. so rapidly at the beginning of the test that the
initial pressure requirement cannot be met. If this
6.5 Rinse the fuel reservoir beaker with some is evidently found to be the case after checking
of the product to be tested. the pump and filter units, the requirement can
be ignored, and this fact reported in the form
6.6 Remove the adaptor if procedures A or C described in 10.2.
are to be used.

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8.2 Procedure A 8.3.5 When 300 ml of sample has been pumped

without the pressure rising to 105 kPa, record the
8.2.1 Attach the assembled Filter A assembly to pressure reached at the end of the test (see 3.1),
the Luer fitting on the system. to the nearest 5 kPa, and discontinue the test.

8.2.2 Re-start the pump and after 20s, record 8.4 Procedure C
the pressure gauge reading, which should be
within the range 7 kPa to 40 kPa. If the pressure 8.4.1 Attach Filter C to the Luer fitting on the
gauge reading is not within the correct range, system.
stop the pump and check the apparatus for faults.
8.4.2 Re-start the pump and after 20 s, record
NOTE A pressure reading of greater than 21 kPa may the pressure gauge reading, which should be
indicate an incorrect installation of the filter media. within the range 7 kPa to 40 kPa. If the pressure
gauge reading is not within the correct range,
8.2.3 Observe the pressure gauge reading stop the pump and check the apparatus for faults.
as pumping continues. If the pressure rises to
105 kPa, stop the pump immediately. Measure 8.4.3 Observe the pressure gauge reading
and record the volume of the fuel in the receiver as pumping continues. If the pressure rises to
beaker, rounding off the figure to the nearest 105 kPa, stop the pump immediately. Measure
10 ml. and record the volume of the fuel in the receiver
beaker, rounding off the figure to the nearest
8.2.4 When 300 ml of sample has been pumped 10 ml.
without the pressure rising to 105 kPa, record the
pressure reached at the end of the test (see 3.1), 8.4.4 When 300 ml of sample has been pumped
to the nearest 5 kPa, and discontinue the test. without the pressure rising to 105 kPa, record the
pressure reached at the end of the test (see 3.1),
8.2.5 Disassemble the filter unit and inspect the to the nearest 5 kPa, and discontinue the test.
filter medium. The patch of sediment in the centre
shall be 9,0 mm to 10,0 mm in diameter. Repeat 8.5 All procedures
the test if this condition is not met.
8.5.1 If for specification compliance purposes
8.3 Procedure B the test is stopped manually after a specific
volume of fuel, other than 300 ml, has been
8.3.1 Follow the manufacturer’s instructions to pumped through the filter, record and report the
attach the adaptor (5.9) to the Luer fitting on the pressure and volume. Do not use equations [1]
system. and [2].

8.3.2 Attach the tapered end of Filter B to the 8.5.2 If during any test the pressure rises to
adaptor. 105 kPa or if a sample is known to be severely
contaminated with particulates, follow the
NOTE Procedure B uses a syringe filter in an upside manufacturer’s instructions to clean the pulse
down orientation. damper assembly before commencing the next
test.
8.3.3 Re-start the pump and after 20 s, record
the pressure gauge reading, which should be 9 Calculation
within the range 7 kPa to 40 kPa. If the pressure
gauge reading is not within the correct range, Calculate the filter blocking tendency (FBT)
stop the pump and check the apparatus for faults. using one of the equations below. Equation 1
applies when 300 ml of fuel have passed through
8.3.4 Observe the pressure gauge reading the filter medium at a pressure below 105 kPa
as pumping continues. If the pressure rises to and equation 2 applies when the test has been
105 kPa, stop the pump immediately. Measure discontinued when the pressure reached 105 kPa.
and record the volume of the fuel in the receiver
beaker, rounding off the figure to the nearest 2
10 ml. =
FBT 1+ ( (
P
105
(1)

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2 10.4 If the condition of 8.1.5 applies, report

=
FBT 1+( (
300
v
(2)
‘high initial pressure’ appended to the FBT result.

where
11 Precision
P is the pressure reading at the end of the
test (see 3.1) obtained for 300 ml of fuel 11.1 General
to pass the filter, in kPa.
The precision, derived from statistical analysis
v is the volume of fuel in ml, passed prior to by IP 367 of the results of interlaboratory testing
the pressure rising to 105 kPa. is given in 11.1 and 11.2. Table 1 shows the
precision in tabular form.
10 Expression of results NOTE 1 An evaluation of a sub-set of the round robin
samples used to derive the precision and comprising
10.1 If undissolved water is observed (see biodiesel, biodiesel blend (B10) and automotive diesel,
7.1.4), report as ‘undissolved water present, test showed that the precision of these samples using
not carried out’. Procedure B was not significantly different from the
precision quoted in 11.1.2 and 11.2.2.
10.2 For all completed tests, record the
following: NOTE 2 The viscosity range of the samples used to
determine the precision was 2,0 mm2/s to 4,6 mm2/s.

(i) the value of FBT, rounded to the nearest

NOTE 3 For the precision of this test method when
0,01, as the filter blocking tendency; using sample pre-treatment such as specified in cold
(ii) the volume of fuel pumped, in ml; soak test methods, refer to the applicable test method.
(iii) the pressure at the end of the test, in kPa;
(iv) the initial pressure, in kPa;
(v) the sample temperature (see 7.1.4), in °C;
(vi) the procedure followed (A or B or C).

10.3 If the test is stopped manually when a

specified volume of fuel has been pumped, report:
volume pumped and final pressure.

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Table 1 Tabulated precision

Procedure A Procedure A Procedure B Procedure B Procedure C Procedure C

FBT r R r R r R
1,1 0,1 0,3 0,1 0,1 0,1 0,2
1,2 0,1 0,3 0,1 0,1 0,1 0,2
1,4 0,2 0,4 0,1 0,1 0,2 0,2
1,6 0,2 0,5 0,2 0,2 0,2 0,3
1,8 0,3 0,6 0,2 0,2 0,2 0,4
2 0,3 0,7 0,3 0,2 0,3 0,5
2,5 0,4 1,0 0,4 0,4 0,4 0,7
3 0,6 1,3 0,6 0,6 0,6 1,0
3,5 0,7 1,7 0,9 0,8 0,8 1,3
4 0,9 2,1 1,1 1,0 1,0 1,6
4,5 1,1 2,6 1,4 1,2 1,3 2,0
5 1,3 3,0 1,7 1,5 1,5 2,4
5,5 1,5 3,5 2,1 1,9 1,8 2,9
6 1,8 4,1 2,5 2,2 2,1 3,4
6,5 2,0 4,6 2,9 2,6 2,4 3,9
7 2,3 5,2 3,4 3,0 2,8 4,4
7,5 2,5 5,8 3,9 3,5 3,2 5,0
8 2,8 6,5 4,5 3,9 3,6 5,6
8,5 5,0 4,5 4,0 6,3
9 5,7 5,0 4,4 7,0
9,5 6,3 5,6 4,8 7,7
10 7,0 6,2 5,3 8,4
11 8,4 7,5
12 10,1 8,9
13 11,8 10,4
14 13,7 12,1
15 15,7 13,9

11.2 Repeatability, r 11.2.3 Procedure C

The difference between two test results, obtained r = 0,0842 x1,8

by the same operator with the same apparatus
under constant operating conditions on identical Where x is the average of results being compared.
test material would in the long run, in the normal
and correct operation of the test method, exceed 11.3 Reproducibility, R
the following value in absolute value in only one
case in twenty.
The difference between two single and independent
test results, obtained by different operators
11.2.1 Procedure A working in different laboratories on identical test
r = 0,1009 x1,6 material, would in the long run, in the normal and
correct operation of the test method, exceed the
following value in only one case in twenty.
11.2.2 Procedure B

r = 0,0698 x2

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11.3.1 Procedure A 12 Test report

R = 0,2318 x1,6 The test report shall contain at least the following
information:
11.3.2 Procedure B
a) a reference to this Standard;
R = 0,0616 x 2

b) the procedure used (A, B or C);

11.3.3 Procedure C
c) the type and complete identification of
R = 0,1337 x 1,8 the product tested;

Where x is the average of results being compared. d) the result of the test (see 10);

11.4 Relative bias between procedures e) any deviation, by agreement or otherwise,

from the procedure specified;
See Annex C.
f) the date of the test.

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Annex A
(normative)

Filtration apparatus

A.1 Apparatus A.1.5 Pressure relief valve, located on the front

of the arm holding the filter assembly. Used to
The apparatus, as shown diagrammatically relieve the pressure if the filter becomes blocked
in Figure A.1, is available as a complete and during verification and calibration of the
unit comprising pressure and temperature pressure sensor in automated apparatus.
measurement, automated calculation of filter
blocking tendency and a graphical representation A.1.6 Fuel beakers, made of glass, polypropylene
of filterability. It can also be constructed from the or other suitable materials, with a capacity of at
individual components described below, however, least 400 ml with 10 ml graduations.
the precision of the method may be affected.
NOTE Fuel reservoir beakers made of plastic type
A.1.1 Piston pump, capable of delivering fuel materials can cause particulates to adhere to the walls
at a constant rate of 20 ml/min ± 1 ml/min and of the beaker due to static effects and can affect the
result.
incorpo-rating a mechanical means of adjusting
and calibrating the flow. The flow adjustment
shall have a locking mechanism. A.1.7 Printer, optional with automated apparatus
to record results and graphically represent the
A.1.2 Pulse damper, a mechanism to produce pressure/flow characteristics (see Annex B).
smooth flow of fuel to the filter unit.
A.1.8 Input suction tube, for drawing up the test
A.1.3 Pressure gauge, calibrated and graduated portion from the fuel reservoir beaker. The top of
covering the range 0 kPa to 105 kPa gauge the input aperture is nominally 5 mm from the
pressure, with an accuracy of± 1 kPa. bottom of the liquid.

A.1.4 Over pressure sensor, fitted to automated A.1.9 Fuel input and output assemblies, shall be
apparatus between the pump and the damper to directly earthed (grounded) to avoid the build up
stop the pump if the pressure exceeds 200 kPa. of static electricity.

Pressure gauge or
transducer

THERMOMETER
Pump Pulse
Filter unit and pressure
damper
relief valve

Fuel Fuel
reservoir receiver
beaker beaker

Figure A.1 Flow diagram of filtration test apparatus

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Annex B
(informative)

Results format (optional)

Figure B.1 Typical results format

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Annex C
(informative)

Relative bias

C.1 General C.3 Relative bias between procedures A/B and C

This Annex provides relative bias information The filters used for these procedures have different
between procedures A and B, as well as porosity and hence no reliable bias statement is
equivalence between procedure C and ASTM possible.
D6426 [1]. This information was obtained, from
the round robin used to estimate the precision of C.4 Relative bias between procedure C and
IP 387, using the ASTM D2PP [2], IP 367 and ASTM D6426
D6708 [3], statistical software.
The filters used in procedure C have been shown
C.2 Relative bias between IP 387 procedures statistically to be equivalent to those specified in
A and B ASTM D6426.

FBTA = 1,097 FBTB The results using the single D6426 apparatus
showed general equivalence with the IP 387
Where an equivalent procedure A result (FBTA) can apparatus, for the samples tested.
be derived from the result obtained by procedure
B (FBTB).

This bias equation may not be suitable for all

types of sample, and users are advised to confirm
its suitability before use.

It is not possible to calculate a procedure B result

from a procedure A test.

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Bibliography

[1] ASTM D6426, Standard test method for [3] ASTM D6708, Standard practice for
determining filterability of middle distillate statistical assessment and improvement
fuel oils. of the expected agreement between two
test methods that purport to measure the
[2] D2PP, Adjunct to ASTM D6300. same property of a material.

Summary of changes

The location of selected changes made to this standard since the last version, that may impact the use
of this standard, are:

a) 5.2.2.1 addition of filter requirements.

b) Annex C - C.2 Bias equation may not be suitable for all sample types. Statement added to confirm it
is not possible to calculate a procedure B result from a procedure A test.

387.12