ASTM D6217-98(2008)
(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
SIGNIFICANCE AND USE
This is the first ASTM standard test method for assessing the mass quantity of particulates in middle distillate fuels. Test Method D 5452 and its predecessor Test Method D 2276 were developed for aviation fuels and used 1 gal or 5 L of fuel sample. Using 1 gal of a middle distillate fuel, which can contain greater particulate levels, often required excessive time to complete the filtration. This test method used about a quarter of the volume used in the aviation fuel methods.
The mass of particulates present in a fuel is a significant factor, along with the size and nature of the individual particles, in the rapidity with which fuel system filters and other small orifices in fuel systems can become plugged. This test method provides a means of assessing the mass of particulates present in a fuel sample.
The test method can be used in specifications and purchase documents as a means of controlling particulate contamination levels in the fuels purchased. Maximum particulate levels are specified in several military fuel specifications.
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.
1.2 This test method is not suitable for fuels whose flash point as determined by Test Methods D 56, D 93 or D 3828 is less than 38°C.
Note 1—Middle distillate fuels with flash points less than 38°C have been ignited by discharges of static electricity when the fuels have been filtered through inadequately bonded or grounded membrane filter systems. See Test Methods D 2276 and D 5452 for means of determining particulate contamination in Specification D 1655 aviation turbine fuels and other similar aviation fuels. See Guide D 4865 for a more detailed discussion of static electricity formation and discharge.
1.3 The precision of this test method is applicable to particulate contaminant levels between 0 to 25 g/m3 provided that 1 L samples are used and the 1 L is filtered completely. Higher levels of particulate contaminant can be measured, but are subject to uncertain precision.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 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:D6217–98 (Reapproved 2008)
Designation: 415/98
Standard Test Method for
Particulate Contamination in Middle Distillate Fuels by
Laboratory Filtration
This standard is issued under the fixed designation D6217; 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 priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
1.1 Thistestmethodcoversthedeterminationofthemassof
particulate contamination in a middle distillate fuel by filtra-
2. Referenced Documents
tion.This test method is suitable for all No. 1 and No. 2 grades
2.1 ASTM Standards:
in Specifications D396, D975, D2880 and D3699 and for
D56 Test Method for Flash Point by Tag Closed Cup Tester
grades DMA and DMB in Specification D2069.
D93 Test Methods for Flash Point by Pensky-Martens
1.2 This test method is not suitable for fuels whose flash
Closed Cup Tester
point as determined by Test Methods D56, D93 or D3828 is
D396 Specification for Fuel Oils
less than 38°C.
D975 Specification for Diesel Fuel Oils
NOTE 1—Middle distillate fuels with flash points less than 38°C have
D1193 Specification for Reagent Water
been ignited by discharges of static electricity when the fuels have been
D1655 Specification for Aviation Turbine Fuels
filtered through inadequately bonded or grounded membrane filter sys-
D2069 Specification for Marine Fuels
tems. See Test Methods D2276 and D5452 for means of determining
D2276 Test Method for Particulate Contaminant inAviation
particulate contamination in Specification D1655 aviation turbine fuels
Fuel by Line Sampling
and other similar aviation fuels. See Guide D4865 for a more detailed
discussion of static electricity formation and discharge.
D2880 Specification for Gas Turbine Fuel Oils
D3699 Specification for Kerosine
1.3 The precision of this test method is applicable to
D3828 Test Methods for Flash Point by Small Scale Closed
particulate contaminant levels between 0 to 25 g/m provided
Cup Tester
that 1 L samples are used and the 1 L is filtered completely.
D4057 Practice for Manual Sampling of Petroleum and
Higher levels of particulate contaminant can be measured, but
Petroleum Products
are subject to uncertain precision.
D4865 Guide for Generation and Dissipation of Static
1.4 The values stated in SI units are to be regarded as
Electricity in Petroleum Fuel Systems
standard. No other units of measurement are included in this
D5452 Test Method for Particulate Contamination in Avia-
standard.
tion Fuels by Laboratory Filtration
1.5 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
3. Terminology
responsibility of the user of this standard to establish appro-
3.1 Definitions:
1 2
This test method is under the jurisdiction of ASTM Committee D02 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
D02.14 on Stability and Cleanliness of Liquid Fuels. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Dec. 1, 2008. Published February 2009. Originally the ASTM website.
´1 3
approved in 1998. Last previous edition approved in 2003 as D6217–98(2003) . Withdrawn. The last approved version of this historical standard is referenced
DOI: 10.1520/D6217-98R08. on www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D6217–98 (2008)
FIG. 1 Schematic of Filtration System
3.1.1 bond, v—to connect two parts of a system electrically test method provides a means of assessing the mass of
bymeansofaconductivewiretoeliminatevoltagedifferences. particulates present in a fuel sample.
3.1.2 ground, v—to connect electrically with earth. 5.3 The test method can be used in specifications and
3.1.3 membrane filter, n—a thin medium of closely con-
purchase documents as a means of controlling particulate
trolled pore size through which a liquid is passed and on which contaminationlevelsinthefuelspurchased.Maximumparticu-
particulate matter in suspension is retained.
late levels are specified in several military fuel specifications.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 control membrane, n—the lower of the two stacked
6. Apparatus
membrane filters used in this test method.
6.1 Filtration System—Arrange the following components
3.2.2 filtered flushing fluids, n—either of two solvents,
as shown in Fig. 1.
heptane or 2,2,4-trimethylpentane, filtered through a nominal
6.1.1 Funnel and Funnel Base, with filter support for a 47
0.45 µm membrane filter.
mmdiametermembrane,andlockingringorspringactionclip.
3.2.3 test membrane, n—the upper of the two stacked
6.1.2 Ground/Bond Wire, 0.912-2.59 mm (No. 10 through
membrane filters used in this test method.
No. 19) bare stranded flexible, stainless steel or copper
installed in the flasks and grounded as shown in Fig. 1.
4. Summary of Test Method
4.1 A measured volume of about 1 L of fuel is vacuum
NOTE 2—The electrical bonding apparatus described in Test Method
D5452 or other suitable means of electrical grounding which ensure safe
filtered through one or more sets of 0.8 µm membranes. Each
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
rates, two or more sets may be required to complete filtration vacuum filter flask, which the filtration apparatus fits into,
in a reasonable time.
equipped with a sidearm to connect to the safety flask.
4.2 After the filtration has been completed, the membranes
6.1.4 Safety Flask, 1.5 Lor larger borosilicate glass vacuum
are washed with solvent, dried, and weighed. The particulate
filter flask equipped with a sidearm to connect the vacuum
contamination level is determined from the increase in the
system. A fuel and solvent resistance rubber hose through
mass of the test membranes relative to the control membranes,
which the grounding wire passes shall connect the sidearm of
and is reported in units of g/m or its equivalent mg/L.
the receiving flask to the tube passing through the rubber
stopper in the top of the safety flask.
5. Significance and Use
6.1.5 Vacuum System, either a water aspirated or a mechani-
5.1 This is the first ASTM standard test method for assess-
cal vacuum pump may be used if capable of producing a
ing the mass quantity of particulates in middle distillate fuels.
vacuum of 1 to 100 kPa below atmospheric pressure when
Test Method D5452 and its predecessor Test Method D2276
measured at the receiving flask.
were developed for aviation fuels and used 1 gal or 5 Lof fuel
6.2 Other Apparatus:
sample. Using 1 gal of a middle distillate fuel, which can
6.2.1 Air Ionizer, for the balance case. Air ionizers shall be
contain greater particulate levels, often required excessive time
replaced within one year of manufacture.
tocompletethefiltration.Thistestmethodusedaboutaquarter
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
particles, in the rapidity with which fuel system filters and 6.2.2 Analytical Balance, single- or double-pan, the preci-
other small orifices in fuel systems can become plugged. This sion standard deviation of which must be 0.07 mg or less.
D6217–98 (2008)
FIG. 2 Apparatus for Filtering and Dispensing Flushing Fluid
NOTE 5—Small watch glasses, approximately 5 to 7 cm in diameter,
6.2.3 Crucible Tongs, for handling clean sample container
have also been found suitable to support the membrane filters.
lids.
6.2.4 Drying Oven, naturally convected (without fan-
7. Reagents and Materials
assisted air circulation), controlling to 90 6 5°C.
7.1 Purity of Reagents—Reagent grade chemicals shall be
6.2.5 Flushing Fluid Dispenser, an apparatus for dispensing
used in all tests. Unless otherwise indicated, it is intended that
flushing fluid through a nominal 0.45 µm membrane filter.
all reagents shall conform to the specifications of the Commit-
NOTE 4—An apparatus such as pictured in Fig. 2 has been found
tee onAnalytical Reagents of theAmerican Chemical Society,
suitable for this task. A standard laboratory wash bottle can also be used 5
where such specifications are available. Other grades may be
provided the flushing fluid is pre-filtered through a 0.45-µm pore size
used, provided it is first ascertained that the reagent is of
membrane filter and precautions are taken to maintain appropriate
sufficient purity to permit its use without lessening the accu-
cleanliness of the interior of the wash bottle
racy of the determination.
6.2.6 Forceps, approximately 12 cm long, flat-bladed, with
7.2 Purity of Water— Unless otherwise indicated, refer-
non-serrated, non-pointed tips.
ences to water mean reagent water as defined by Type III of
6.2.7 Graduated Cylinders, to contain at least 1 L of fluid
Specification D1193.
and marked at 10 mL intervals. 100 mL graduated cylinders
7.3 Flushing Fluids:
may be required for samples which filter slowly.
6.2.8 Petri Dishes, approximately 12.5 cm in diameter, with
removable glass supports for membrane filters.
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For Suggestions on the testing of reagents not
listed by the American Chemical Society, see Annual Standards for Laboratory
Supporting data (a membrane approval procedure) have been filed at ASTM Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
International Headquarters and may be obtained by requesting Research Report and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
D02-1012. MD.
D6217–98 (2008)
7.3.1 Heptane,(Warning—Flammable.) sampled. When it is not practical to clean the sampling lines,
7.3.2 2,2,4-trimethylpentane (isoctane),(Warning— rinse them thoroughly with the fuel to be sampled.
9.3 Precautions to avoid sample contamination shall include
Flammable.)
7.4 Propan-2-ol (2-propanol; isopropyl alcohol), selection of an appropriate sampling point. Samples should
preferentiallybeobtaineddynamicallyfromasamplingloopin
(Warning—Flammable.)
a distribution line, or from the flushing line of a field sampling
7.5 Liquid or Powder Detergent, water-soluble, for cleaning
kit. Ensure that the line to be sampled is flushed with fuel
glassware.
before taking the sample.
7.6 Nylon Test Membrane Filters, plain, 47-mm diameter,
9.3.1 Where it is desirable or only possible to obtain
nominal pore size 0.8-µm.
samples from static storage, follow the procedures given in
7.7 Nylon Control Membrane Filters (see Note 6), 47-mm
Practice D4057 or equivalent, taking precautions for cleanli-
diameter, nominal pore size 0.8-µm.
ness of all equipment used. Ensure that the sample has not
NOTE 6—Membrane filters with a grid imprinted on their surface, may
passed through intermediate containers prior to placement in
be used as control membrane filters for identification.
the prepared container. (Warning—Samples obtained from
7.8 Protective Cover, polyethylene film or clean aluminum
static storage may give results which are not representative of
foil. the bulk contents of the tank because of particulate matter
settling. Where possible, the contents of the tank should be
8. Preparation of Apparatus and Sample Containers circulated or agitated before sampling, or the sampling per-
formed shortly after a tank has been filled.)
8.1 Clean all components of the filtration apparatus, sample
9.4 Visually inspect the sample container before taking the
containers, their caps and petri dishes as described in 8.1.1-
samples to verify that there are no visible particles present
8.1.7.
inside the container. Fill the sample container 95 volume %
8.1.1 Remove any labels, tags, and so forth.
full, leaving space for vapor expansion. Protect the fuel sample
8.1.2 Wash with warm tap water containing detergent.
from prolonged exposure to light by wrapping the container in
8.1.3 Rinse thoroughly with warm tap water.
aluminum foil or storing it in the dark to reduce the possibility
8.1.4 Rinse thoroughly with reagent water. Container caps
of particulate formation by light-promoted reactions. Do not
should be handled only externally with clean laboratory
transfer the fuel sample from its original sample container into
crucible tongs during this and subsequent washings.
an intermediate storage container. If the original sample
8.1.5 Rinse thoroughly with propan-2-ol that has been
container is damaged or leaking, then a new sample must be
filtered through a 0.45 µm membrane filter.
obtained.
8.1.6 Rinse thoroughly with filtered flushing fluid and dry.
9.5 Analyzefuelsamplesassoonaspossibleaftersampling.
8.1.7 Keepacleanprotectivecover(thecovermayberinsed
When a fuel cannot be analyzed within one day, blanket it with
with filtered flushing fluid), over the top of the sample
an inert gas such as oxygen-free nitrogen, argon, or helium and
container until the cap is installed. Similarly protect the funnel
store it at a temperature no higher than 10°C, except for
opening of the assembled filtration apparatus with a clean
samples with cloud points above 10°C which are to be stored
protective cover until ready for use.
at a temperature 2°C above their cloud point.
9. Sampling
10. Preparation of Membrane Filters
9.1 The sample container shall be 1 L (60.15 L) in volume
10.1 Each set of test filters consists of one test membrane
and have a screw on cap. Glass containers are preferred to filter and one control membrane filter. For fuels containing
facilitate a visual inspection of the contents and the container
little particulate materials, only one set of filters is required. If
before and after
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