Standard Test Method for Sizing and Counting Particles in Light and Middle Distillate Fuels, by Automatic Particle Counter <a href="#fn00005"></a>
SIGNIFICANCE AND USE
This test method is intended for use in the laboratory or in the field for evaluating the cleanliness of distillate fuels, and liquid bio fuels. It is not applicable to on or in-line applications.
This test method offers advantage over traditional filtration methods in that it is a precise rapid test, and advantage over visual methods as it is not subjective.
An increase in particle counts can indicate a change in the fuel condition caused by storage or transfer for example.
High levels of particles can cause filter blockages and have a serious impact on the life of pumps, injectors, pistons and other moving parts. Knowledge of particle size in relation to the metallurgy can provide vital information especially if the hardness of particles is also known from other sources.
This test method specifies a minimum requirement for reporting measurements in particle size bands (see A1.1.2). Some specific applications may require measurements in other particle size bands.
Obtaining a representative sample and following the recommended sample and test specimen preparation procedures and timescales is particularly important with particle counting methods. (See Sections 8, 10, 14.1.4 and Note 10.)
SCOPE
1.1 This test method uses a specific automatic particle counter (APC) to count and measure the size of dispersed dirt particles, water droplets and other particles, in light and middle distillate fuel, and bio fuels such as biodiesel and biodiesel blends, in the overall range from 4 µm(c) to 100 µm(c) and in the size bands ≥4 µm(c), ≥6 µm(c), and ≥14 µm(c).
Note 1—ASTM specification fuels falling within the scope of this test method include Specifications: D975 grades 1D and 2D, D3699, D4814 (see 14.1.1.1), D6751, D6985, D7467 and distillate grades of D396 and D2880.
Note 2—For the purposes of this test method, water droplets are counted as particles, and agglomerated particles are detected and counted as a single larger particle. Dirt includes biological particles. Although the projected area of a particle is measured, this is expressed as the diameter of a sphere for the purposes of this test method.
Note 3—The notation (c), used with particle sizes, is used to denote that the apparatus has been calibrated in accordance with ISO 11171. Strictly this only applies to particles up to 50 µm.
Note 4—This test method may be used for particle sizes bands up to 100 µm(c), however the precision has only been determined for the size bands ≥4 µm(c), ≥6 µm(c), and ≥14 µm(c).
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D7619–10
Standard Test Method for
Sizing and Counting Particles in Light and Middle Distillate
,
1 2
Fuels, byAutomatic Particle Counter
This standard is issued under the fixed designation D7619; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 2. Referenced Documents
1.1 This test method uses a specific automatic particle 2.1 ASTM Standards:
counter (APC) to count and measure the size of dispersed dirt D396 Specification for Fuel Oils
particles,waterdropletsandotherparticles,inlightandmiddle D975 Specification for Diesel Fuel Oils
distillate fuel, and bio fuels such as biodiesel and biodiesel D2880 Specification for Gas Turbine Fuel Oils
blends, in the overall range from 4 µm(c) to 100 µm(c) and in D3699 Specification for Kerosine
the size bands$4 µm(c),$6 µm(c), and$14 µm(c). D4057 Practice for Manual Sampling of Petroleum and
Petroleum Products
NOTE 1—ASTM specification fuels falling within the scope of this test
D4177 Practice for Automatic Sampling of Petroleum and
method include Specifications: D975 grades 1D and 2D, D3699, D4814
Petroleum Products
(see 14.1.1.1), D6751, D6985, D7467 and distillate grades of D396 and
D2880. D4814 Specification for Automotive Spark-Ignition Engine
NOTE 2—For the purposes of this test method, water droplets are
Fuel
counted as particles, and agglomerated particles are detected and counted
D5854 PracticeforMixingandHandlingofLiquidSamples
as a single larger particle. Dirt includes biological particles.Although the
of Petroleum and Petroleum Products
projected area of a particle is measured, this is expressed as the diameter
D6300 Practice for Determination of Precision and Bias
of a sphere for the purposes of this test method.
Data for Use in Test Methods for Petroleum Products and
NOTE 3—The notation (c), used with particle sizes, is used to denote
Lubricants
that the apparatus has been calibrated in accordance with ISO 11171.
Strictly this only applies to particles up to 50 µm. D6751 Specification for Biodiesel Fuel Blend Stock (B100)
NOTE 4—This test method may be used for particle sizes bands up to
for Middle Distillate Fuels
100 µm(c), however the precision has only been determined for the size
D6985 Specification for Middle Distillate Fuel Oil—
bands$4 µm(c),$6 µm(c), and$14 µm(c).
Military Marine Applications
1.2 The values stated in SI units are to be regarded as
D7467 Specification for Diesel Fuel Oil, Biodiesel Blend
standard. No other units of measurement are included in this
(B6 to B20)
standard.
2.2 ASTM Adjuncts:
1.3 This standard does not purport to address all of the
ADJ6300 D2PP Determination of Precision and Bias data
safety concerns, if any, associated with its use. It is the
for Use in Test Methods for Petroleum Products
responsibility of the user of this standard to establish appro-
2.3 ISO Standards:
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
This test method is under the jurisdiction of ASTM Committee D02 on Standards volume information, refer to the standard’s Document Summary page on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee the ASTM website.
D02.14 on Stability and Cleanliness of Liquid Fuels. Withdrawn. The last approved version of this historical standard is referenced
Current edition approved May 1, 2010. Published August 2010. on www.astm.org.
2 5
The following equipment, as listed in RR:D02-1696, Seta-Avcount 91700-0 For referenced ASTM adjuncts contact ASTM Customer Service at
available from Stanhope-Seta, London Street, Chertsey, Surrey KT16 8AP UK was service@astm.org.
used to develop the precision statement. This listing is not an endorsement or Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
certification by ASTM International. 4th Floor, New York, NY 10036, http://www.ansi.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D7619–10
ISO 11171 Hydraulic Fluid Power—Calibration of Auto- surement is then repeated. If the size band$4 µm(c), per mL,
matic Particle Counters for Liquids measurements agree within either 10 % or 200 counts, the
ISO 4406 Hydraulic Fluid Power—Fluids—Method for measurements for each of the size bands are averaged for each
Coding Level of Contamination by Solid Particles size band to give results, per mL, for each size band.
ISO 12103-A1 Specification for Ultra Fine Test Dust
(UFTD) 5. Significance and Use
ISO 12103-A3 Specification for Medium Test Dust (MTD)
5.1 This test method is intended for use in the laboratory or
in the field for evaluating the cleanliness of distillate fuels, and
3. Terminology
liquidbiofuels.Itisnotapplicabletoonorin-lineapplications.
3.1 Definitions of Terms Specific to This Standard:
5.2 This test method offers advantage over traditional filtra-
3.1.1 particles, n—solid particles and dispersed water drop-
tion methods in that it is a precise rapid test, and advantage
lets which are detected and counted by this test method.
over visual methods as it is not subjective.
3.1.2 particle count, n—the sum of the number of solid
5.3 An increase in particle counts can indicate a change in
particles and dispersed water droplets.
the fuel condition caused by storage or transfer for example.
3.1.3 particle size, µm(c), n—the projected area equivalent
5.4 High levels of particles can cause filter blockages and
diameter of spherical particles passing through the detecting
have a serious impact on the life of pumps, injectors, pistons
cell in accordance with ISO 11171.
and other moving parts. Knowledge of particle size in relation
3.1.4 particle size cumulative count, n—the total number of
tothemetallurgycanprovidevitalinformationespeciallyifthe
particles per mL, in size bands,$4 µm(c),$6 µm(c), and$14
hardness of particles is also known from other sources.
µm(c),
5.5 This test method specifies a minimum requirement for
3.1.4.1 Discussion—Automatic particle counters may also
reporting measurements in particle size bands (see A1.1.2).
count the total number of particles per mL, in size bands, in
Some specific applications may require measurements in other
addition to those in 3.1.4,upto$100 µm.
particle size bands.
3.1.5 ISO Codes, n—a standard method for coding the level
5.6 Obtaining a representative sample and following the
of contamination by particles.
recommended sample and test specimen preparation proce-
3.1.5.1 Discussion—Results are expressed by ISO Codes as
dures and timescales is particularly important with particle
specified by ISO 4406. These codes are written in the form of
counting methods. (See Sections 8, 10, 14.1.4 and Note 10.)
x/y/z, where x, y and z are ISO Codes equivalent to the
cumulative counts, per mL, for particle size bands$4 µm(c),
6. Apparatus
$6 µm(c), and$14 µm(c) respectively. An example of this is
given in Appendix X1.
6.1 Automatic Particle Counter (APC) —Operating on the
laser light obscuration principle, comprising an optical mea-
NOTE 5—All particle counts are per mL.
surement cell, bi-directional double pump, electronics and
3.1.6 coincidence error limit, n—the highest concentration
softwaretoanalyzethetestspecimen,anddisplayandprintthe
of ISO ultrafine test dust (ISO 12103-A1 or ISO UFTD) that
particle measurement data. (See Annex A1.)
can be counted with an automatic particle counter with less
6.2 Test Specimen Container, cylindrical, made of glass or
than 5 % error resulting from the presence of more than one
other suitable material, of at least 125 mL volume with
particle in the sensor/laser optical path at a time.
provision for holding the test specimen input tube at least
3.1.7 test specimen, n—an aliquot of the test sample. (See
10 mm above the bottom of the container, and a cap with a
Section 10.)
suitable inert internal seal.
4. Summary of Test Method
NOTE 6—It is recommended that glass test specimen containers should
be used to avoid any potential problems with particles adhering to the
4.1 The optical measurement cell comprises a light source
insides of the containers due to static electricity that could occur with
and an optical sensor. The principle of operation is the
some samples or some specimen containers.
measurement of laser light obscuration. Particles/droplets en-
trained within the test specimen cast shadows on the optical 6.3 Waste Container, for collecting the tested test specimen.
sensor causing a reduction of the output voltage of the sensor.
6.4 Filter Apparatus, general purpose for filtering heptane
The voltage drop is a function of the particle/droplet size. Each
or other solvents.
detected particle is counted, sized and recorded. Upon comple-
6.4.1 Filters, cellulose, glass fiber or polycarbonate
tion of the test the software calculates and displays the number
0.45 µm.
of obscuration events for each of the predetermined size bands.
6.5 Printer, to record details of the measurements and
4.2 The test specimen is mixed in its container to suspend
results.
the particles. Upon initiation of a test, the automatic particle
counter (APC) draws the test specimen directly from a test
specimen container (see Fig. A1.1). The test sequence com-
mences by flushing the optical measurement cell and pipework
with 30 mLof the test specimen. This is immediately followed
by the test of a 10 mLtest specimen where particles in each of
the specified size bands are counted. This flushing and mea-
D7619–10
7. Reagents and Materials the measurement cell and the inside of the connecting tubing
before testing other test specimens.
7.1 Verification and Calibration Fluids —Containing ISO
Medium Test Dust (MTD) as specified in specification
10. Test Specimen Preparation
ISO 12103-A3.
7.2 Heptane—Reagent grade filtered down to 0.45 µm.
10.1 Gently shake the sample in its container, for at least a
7.2.1 Prepare the heptane by filtering through a 0.45 µm minute, sufficiently to ensure that a representative test speci-
filter (see 6.4.1) contained in a filter apparatus (see 6.4) See
men can be drawn into the test specimen container.
Note 8. Store in a container prepared in accordance with 10.2. 10.1.1 It is essential to take a representative test specimen,
(Warning—Extremely flammable, health hazard.)
but avoid power mixing or vigorous mixing as this can modify
the particles, break up agglomerated particles and entrain air.
8. Sampling
(See 14.1.4 and Note 17.)
8.1 Unless otherwise specified, take a sample of at least 100
NOTE 7—To achieve a consistent agitation, equivalent to “gentle
mL in accordance with Practices D4057, D5854, D4177,or
shaking”ofthesample,itisrecommendedtoeither: (a)tumblethesample
other comparable sampling practices.
container, by hand or using a suitable automated mechanical tumbler, end
over end for a minimum of 60 revolutions at approximately 1 revolution
8.2 It is essential to take a representative sample, but avoid
per second; (b) invert the sample container back and forth for a minimum
power mixing as this can modify the particles, break up
of 60 times at approximately 1 cycle per second; or (c) use a barrel roller
agglomeratedparticlesandentrainair.(See14.1.4andNote7.)
and roll for a minimum of 60 rotations.
8.3 Use sample containers that are capable of transporting
Other ways of gently shaking the sample may be used, provided a
the sample without contamination. Examples of these are fully
representative test specimen is achieved.
epoxy-lined metal or amber colored glass containers with a
10.2 Use a clean test specimen container, or flush a test
threaded cap, fitted with an inert liner, forming a seal with the
specimen container by rinsing the inside of the container three
container.
times with the sample to be tested. Each rinse shall use product
8.4 Prior to taking the sample, rinse the sample containers
equal to 10 to 20 % of the container volume. A rinse shall
with the product to be sampled at least three times. Each rinse
include closing and shaking the container for a minimum of 5
shall use product equal to 10 to 20 % of the container volume.
sandthendrainingtheproduct.Alternatively,thetestspecimen
A rinse shall include closing and shaking the container for a
container may be cleaned by washing thoroughly with filtered
minimum of 5 s and then draining the product.
heptane (see 7.2) and then allowed to dry in a clean environ-
8.5 Do not fill the sample container more than 90 % full.
ment.
Overfilling affects the preparation of the test specimen as
specified in 10.1.
NOTE 8—The efficacy of cleaning of the test specimen container may
8.6 Ensure that any aliquots or sub-division of the sample
be checked by testing a sample of filtered heptane (see 7.2), in the cleaned
results in representative samples being taken and remaining in
test specimen container; this should give a count of less than 50 counts for
the original sample container. Note 7 and 10.1 recommend the$4 µm(c) measurement.
suitable procedures regarding this particle counting test
10.3 Immediately after gently shaking, pour the mixed
method.
sample into the test specimen container and fit a clean cap.
Ensure that the test specimen container is less than 90 % full.
9. Preparation of Apparatus
2 NOTE 9—Over shaken or mechanically stirred samples can result in
9.1 Ensure that the APC is set up according to the instru-
finely dispersed micro bubbles forming that will be counted as solid
ment manufacturer’s operating instructions and the verification
particles. Test specimens given ultrasonic treatment can result in the
and calibration requirements stated in both Section 11 and
break-up of aglomerated particles into smaller ones that can affect the
A1.1.4.
particle counts.
9.2 Ensure that the mode of operation, specified for this test
method by the manufacturer, is selected. 11. Apparatus Verification and Calibration
9.3 Clean the outside of the test specimen input tube before
11.1 Verification:
each test sequence, by washing the outside in clean heptane or
11.1.1 Verify the correct operation of theAPC at least every
another filtered solvent.
6 months or more frequently if required by local quality
9.4 At the start of any daily testing regime, initiate a test
controls, by using the verification fluid (see 7.1) in accordance
sequence using filtered heptane.
with11.1.1.1andSection12.Theresultobtainedshallbeequal
9.5 If a te
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