ASTM D6217-98
(Test Method)Standard Test Method for Particulate Contamination in Middle Distillate Fuels by Laboratory Filtration
Standard Test Method for Particulate Contamination in Middle Distillate Fuels by Laboratory Filtration
SCOPE
1.1 This test method covers the determination of the mass of particulate contamination in a middle distillate fuel by filtration. This test method is suitable for all No. 1 and No. 2 grades in Specifications D 396, D 975, D 2880 and D 3699 and for grades DMA and DMB in Specification D 2069.
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Standards Content (Sample)
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An American National Standard
Designation: D 6217 – 98
Designation: 415/98
Standard Test Method for
Particulate Contamination in Middle Distillate Fuels by
Laboratory Filtration
This standard is issued under the fixed designation D 6217; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope D 975 Specification for Diesel Fuel Oils
D 1193 Specification for Reagent Water
1.1 This test method covers the determination of the mass of
D 1655 Specification for Aviation Turbine Fuels
particulate contamination in a middle distillate fuel by filtra-
D 2069 Specification for Marine Fuels
tion. This test method is suitable for all No. 1 and No. 2 grades
D 2276 Test Method for Particulate Contaminant in Avia-
in Specifications D 396, D 975, D 2880 and D 3699 and for
tion Fuel by Line Sampling
grades DMA and DMB in Specification D 2069.
D 2880 Specification for Gas Turbine Fuel Oils
1.2 This test method is not suitable for fuels whose flash
D 3699 Specification for Kerosine
point as determined by Test Methods D 56, D 93 or D 3828 is
D 3828 Test Methods for Flash Point by Small Scale Closed
less than 38°C.
Tester
NOTE 1—Middle distillate fuels with flash points less than 38°C have
D 4057 Practice for Manual Sampling of Petroleum and
been ignited by discharges of static electricity when the fuels have been
Petroleum Products
filtered through inadequately bonded or grounded membrane filter sys-
D 4865 Guide for Generation and Dissipation of Static
tems. See Test Methods D 2276 and D 5452 for means of determining
Electricity in Petroleum Fuel Systems
particulate contamination in Specification D 1655 aviation turbine fuels
D 5452 Test Method for Particulate Contamination in Avia-
and other similar aviation fuels. See Guide D 4865 for a more detailed
discussion of static electricity formation and discharge.
tion Fuels by Laboratory Filtration
1.3 The precision of this test method is applicable to
3. Terminology
particulate contaminant levels between 0 to 25 g/m provided
3.1 Definitions:
that 1 L samples are used and the 1 L is filtered completely.
3.1.1 membrane filter, n—a thin medium of closely con-
Higher levels of particulate contaminant can be measured, but
trolled pore size through which a liquid is passed and on which
are subject to uncertain precision.
particulate matter in suspension is retained.
1.4 The values stated in SI units are to be regarded as the
3.1.2 ground, v—to connect electrically with earth.
standard.
3.1.3 bond, v—to connect two parts of a system electrically
1.5 This standard does not purport to address all of the
by means of a conductive wire to eliminate voltage differences.
safety concerns, if any, associated with its use. It is the
3.2 Definitions of Terms Specific to This Standard:
responsibility of the user of this standard to establish appro-
3.2.1 control membrane, n—the lower of the two stacked
priate safety and health practices and determine the applica-
membrane filters used in this test method.
bility of regulatory limitations prior to use.
3.2.2 filtered flushing fluids, n—either of two solvents,
2. Referenced Documents
heptane or 2,2,4-trimethylpentane, filtered through a nominal
0.45 μm membrane filter.
2.1 ASTM Standards:
3.2.3 test membrane, n—the upper of the two stacked
D 56 Test Method for Flash Point by Tag Closed Tester
membrane filters used in this test method.
D 93 Test Methods for Flash Point by Pensky-Martens
Closed Tester
4. Summary of Test Method
D 396 Specification for Fuel Oils
4.1 A measured volume of about 1 L of fuel is vacuum
filtered through one or more sets of 0.8 μm membranes. Each
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.14on Stability and Cleanliness of Liquid Fuels. Annual Book of ASTM Standards, Vol 11.01.
Current edition approved Jan. 10, 1998. Published March 1998. Annual Book of ASTM Standards, Vol 05.02.
2 5
Annual Book of ASTM Standards, Vol 05.01. Annual Book of ASTM Standards, Vol 05.03.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D 6217 – 98
operation of the filtration apparatus and flask can be used. If the filtrate is
membrane set consists of a tared nylon test membrane and a
to be subsequently tested for stability it is advisable not to use copper as
tared nylon control membrane. When the level of particulate
copper ions catalyze gum formation during the stability test.
contamination is low, a single set will usually suffice; when the
contamination is high or of a nature that induces slow filtration 6.1.3 Receiving Flask, 1.5 L or larger borosilicate glass
vacuum filter flask, which the filtration apparatus fits into,
rates, two or more sets may be required to complete filtration
in a reasonable time. equipped with a sidearm to connect to the safety flask.
6.1.4 Safety Flask, 1.5 L or larger borosilicate glass vacuum
4.2 After the filtration has been completed, the membranes
are washed with solvent, dried, and weighed. The particulate filter flask equipped with a sidearm to connect the vacuum
system. A fuel and solvent resistance rubber hose through
contamination level is determined from the increase in the
mass of the test membranes relative to the control membranes, which the grounding wire passes shall connect the sidearm of
the receiving flask to the tube passing through the rubber
and is reported in units of g/m or its equivalent mg/L.
stopper in the top of the safety flask.
5. Significance and Use
6.1.5 Vacuum System, either a water aspirated or a mechani-
cal vacuum pump may be used if capable of producing a
5.1 This is the first ASTM standard test method for assess-
vacuum of 1 to 100 kPa below atmospheric pressure when
ing the mass quantity of particulates in middle distillate fuels.
measured at the receiving flask.
Test Method D 5452 and its predecessor Test Method D 2276
6.2 Other Apparatus:
were developed for aviation fuels and used 1 gal or 5 L of fuel
6.2.1 Air Ionizer, for the balance case. Air ionizers shall be
sample. Using 1 gal of a middle distillate fuel, which can
replaced within one year of manufacture.
contain greater particulate levels, often required excessive time
to complete the filtration. This test method used about a quarter
NOTE 3—When using a solid-pan balance, the air ionizer may be
of the volume used in the aviation fuel methods.
omitted provided that, when weighing a membrane filter, it is placed on
5.2 The mass of particulates present in a fuel is a significant the pan so that no part protrudes over the edge of the pan.
factor, along with the size and nature of the individual
6.2.2 Analytical Balance, single- or double-pan, the preci-
particles, in the rapidity with which fuel system filters and
sion standard deviation of which must be 0.07 mg or less.
other small orifices in fuel systems can become plugged. This
6.2.3 Crucible Tongs, for handling clean sample container
test method provides a means of assessing the mass of
lids.
particulates present in a fuel sample.
6.2.4 Drying Oven, naturally convected (without fan-
5.3 The test method can be used in specifications and
assisted air circulation), controlling to 90 6 5°C.
purchase documents as a means of controlling particulate
6.2.5 Flushing Fluid Dispenser, an apparatus for dispensing
contamination levels in the fuels purchased. Maximum particu- 6
flushing fluid through a nominal 0.45 μm membrane filter.
late levels are specified in several military fuel specifications.
NOTE 4—An apparatus such as pictured in Fig. 2 has been found
suitable for this task. A standard laboratory wash bottle can also be used
6. Apparatus
provided the flushing fluid is pre-filtered through a 0.45-μm pore size
6.1 Filtration System—Arrange the following components
membrane filter and precautions are taken to maintain appropriate
as shown in Fig. 1.
cleanliness of the interior of the wash bottle
6.1.1 Funnel and Funnel Base, with filter support for a 47
6.2.6 Forceps, approximately 12 cm long, flat-bladed, with
mm diameter membrane, and locking ring or spring action clip.
non-serrated, non-pointed tips.
6.1.2 Ground/Bond Wire, 0.912-2.59 mm (No. 10 thru No.
6.2.7 Graduated Cylinders, to contain at least 1 L of fluid
19) bare stranded flexible, stainless steel or copper installed in
and marked at 10 mL intervals. 100 mL graduated cylinders
the flasks and grounded as shown in Fig. 1.
NOTE 2—The electrical bonding apparatus described in Test Method D
A membrane approval procedure may be obtained from ASTM Headquarters.
5452 or other suitable means of electrical grounding which ensure safe
Request RR:D02-1012.
FIG. 1 Schematic of Filtration System
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D 6217 – 98
FIG. 2 Apparatus for Filtering and Dispensing Flushing Fluid
may be required for samples which filter slowly. Specification D 1193.
6.2.8 Petri Dishes, approximately 12.5 cm in diameter, with
7.3 Flushing Fluids:
removable glass supports for membrane filters.
7.3.1 Heptane (Warning—See Note 6)
7.3.2 2,2,4-trimethylpentane (isoctane) (Warning—See
NOTE 5—Small watch glasses, approximately 5 to 7 cm in diameter,
Note 6)
have also been found suitable to support the membrane filters.
7.4 Propan-2-ol (2-propanol; isopropyl alcohol),
7. Reagents and Materials
(Warning—See Note 6.)
7.1 Purity of Reagents—Reagent grade chemicals shall be
NOTE 6—Warning—Flammable
used in all tests. Unless otherwise indicated, it is intended that
all reagents shall conform to the specifications of the Commit-
7.5 Liquid or Powder Detergent, water-soluble, for cleaning
tee on Analytical Reagents of the American Chemical Society,
glassware.
where such specifications are available. Other grades may be
7.6 Nylon Test Membrane Filters, plain, 47-mm diameter,
used, provided it is first ascertained that the reagent is of
nominal pore size 0.8-μm.
sufficient purity to permit its use without lessening the accu-
7.7 Nylon Control Membrane Filters (see Note 7), 47-mm
racy of the determination.
diameter, nominal pore size 0.8-μm.
7.2 Purity of Water— Unless otherwise indicated, refer-
NOTE 7—Membrane filters with a grid imprinted on their surface, may
ences to water mean reagent water as defined by Type III of
be used as control membrane filters for identification.
7.8 Protective Cover, polyethylene film or clean aluminum
Reagent Chemicals, American Chemical Society Specifications, American
foil.
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole Dorset, U.K., and the United States Pharmacopeia and
8. Preparation of Apparatus and Sample Containers
National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
MD. 8.1 Clean all components of the filtration apparatus, sample
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D 6217 – 98
containers, their caps and petri dishes as described in 8.1.1- inside the container. Fill the sample container 95 volume %
8.1.7. full, leaving space for vapor expansion. Protect the fuel sample
8.1.1 Remove any labels, tags, and so forth. from prolonged exposure to light by wrapping the container in
8.1.2 Wash with warm tap water containing detergent. aluminum foil or storing it in the dark to reduce the possibility
8.1.3 Rinse thoroughly with warm tap water. of particulate formation by light-promoted reactions. Do not
8.1.4 Rinse thoroughly with reagent water. Container caps transfer the fuel sample from its original sample container into
should be handled only externally with clean laboratory an intermediate storage container. If the original sample
crucible tongs during this and subsequent washings. container or damaged or leaking, then a new sample must be
8.1.5 Rinse thoroughly with propan-2-ol that has been obtained.
filtered through a 0.45 μm membrane filter. 9.5 Analyze fuel samples as soon as possible after sampling.
8.1.6 Rinse thoroughly with filtered flushing fluid and dry. When a fuel cannot be analyzed within one day, blanket it with
8.1.7 Keep a clean protective cover (the cover may be rinsed an inert gas such as oxygen-free nitrogen, argon, or helium and
with filtered flushing fluid), over the top of the sample store it at a temperature no higher than 10°C (50°F), except for
container until the cap is installed. Similarly protect the funnel samples with cloud points above 10°C which are to be stored
opening of the assembled filtration apparatus with a clean at a temperature 2°C above their cloud point.
protective cover until ready for use.
10. Preparation of Membrane Filters
9. Sampling
10.1 Each set of test filters consists of one test membrane
NOTE 8—Caution—It is important to note that the entire contents of filter and one control membrane filter. For fuels containing
the sample container are filtered during the conduct of this test method.
little particulate materials, only one set of filters is required. If
This includes not only all of the fuel but also all rinsings of the interior of
the fuel highly contaminated, more than one set of filters may
the container with flushing fluid. Because of this, take care to protect the
be required (see Section 11). The two membrane filters used for
sample from any external contamination.
each individual test shall be identified by marking the petri
9.1 The sample container shall be 1 L (6 0.15 L) in volume
dishes used to hold and transport the filters. Clean all glassware
and have a screw on cap. Glass containers are preferred to
used in preparation of membrane filters as described in 8.1.
facilitate a visual inspection of the contents and the container
10.1.1 Using forceps place the test and control membrane
before and after filling. Glass containers also allow for visual
filters side by side in a clean petri dish. To facilitate handling,
inspection of the container, after the sample is emptied, to
the membrane filters should rest on clean glass support rods, or
confirm complete
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