ASTM D6217-98(2003)e1
(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 38C.
Note 1—Middle distillate fuels with flash points less than 38C 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 the 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.
General Information
Relations
Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
An American National Standard
´1
Designation:D6217–98 (Reapproved 2003)
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 (´) indicates an editorial change since the last revision or reapproval.
´ NOTE—Warning notes were editorially moved into the standard text in August 2003.
1. Scope D93 Test Methods for Flash Point by Pensky-Martens
Closed Cup Tester
1.1 Thistestmethodcoversthedeterminationofthemassof
D 396 Specification for Fuel Oils
particulate contamination in a middle distillate fuel by filtra-
D 975 Specification for Diesel Fuel Oils
tion. This test method is suitable for all No. 1 and No. 2 grades
D 1193 Specification for Reagent Water
in Specifications D 396, D 975, D 2880 and D 3699 and for
D 1655 Specification for Aviation Turbine Fuels
grades DMA and DMB in Specification D 2069.
D 2069 Specification for Marine Fuels
1.2 This test method is not suitable for fuels whose flash
D 2276 Test Method for Particulate Contaminant in Avia-
point as determined by Test MethodsD56,D93 or D 3828 is
tion Fuel by Line Sampling
less than 38°C.
D 2880 Specification for Gas Turbine Fuel Oils
NOTE 1—Middle distillate fuels with flash points less than 38°C have 4
D 3699 Specification for Kerosine
been ignited by discharges of static electricity when the fuels have been
D3828 TestMethodsforFlashPointbySmallScaleClosed
filtered through inadequately bonded or grounded membrane filter sys-
Tester
tems. See Test Methods D 2276 and D 5452 for means of determining
D 4057 Practice for Manual Sampling of Petroleum and
particulate contamination in Specification D 1655 aviation turbine fuels
and other similar aviation fuels. See Guide D 4865 for a more detailed Petroleum Products
discussion of static electricity formation and discharge.
D 4865 Guide for Generation and Dissipation of Static
Electricity in Petroleum Fuel Systems
1.3 The precision of this test method is applicable to
D 5452 Test Method for Particulate Contamination inAvia-
particulate contaminant levels between 0 to 25 g/m provided
tion Fuels by Laboratory Filtration
that 1 L samples are used and the 1 L is filtered completely.
Higher levels of particulate contaminant can be measured, but
3. Terminology
are subject to uncertain precision.
3.1 Definitions:
1.4 The values stated in SI units are to be regarded as the
3.1.1 bond, v—to connect two parts of a system electrically
standard.
by means of a conductive wire to eliminate voltage differences.
1.5 This standard does not purport to address all of the
3.1.2 ground, v—to connect electrically with earth.
safety concerns, if any, associated with its use. It is the
3.1.3 membrane filter, n—a thin medium of closely con-
responsibility of the user of this standard to establish appro-
trolled pore size through which a liquid is passed and on which
priate safety and health practices and determine the applica-
particulate matter in suspension is retained.
bility of regulatory limitations prior to use.
3.2 Definitions of Terms Specific to This Standard:
2. Referenced Documents 3.2.1 control membrane, n—the lower of the two stacked
membrane filters used in this test method.
2.1 ASTM Standards:
3.2.2 filtered flushing fluids, n—either of two solvents,
D56 Test Method for Flash Point by Tag Closed Tester
heptane or 2,2,4-trimethylpentane, filtered through a nominal
0.45 µm membrane filter.
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.14 on Stability and Cleanliness of Liquid Fuels.
Current edition approved June 10, 2003. Published August 2003. Originally Annual Book of ASTM Standards, Vol 11.01.
approved in 1998. Last previous edition approved in 1998 as D 6217–98. 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.
´1
D6217–98 (2003)
FIG. 1 Schematic of Filtration System
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
NOTE 2—The electrical bonding apparatus described in Test Method
4.1 A measured volume of about 1 L of fuel is vacuum
D 5452 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
copper ions catalyze gum formation during the stability test.
tared nylon control membrane. When the level of particulate
contamination is low, a single set will usually suffice; when the
6.1.3 Receiving Flask, 1.5 L or larger borosilicate glass
contamination is high or of a nature that induces slow filtration
vacuum filter flask, which the filtration apparatus fits into,
rates, two or more sets may be required to complete filtration
equipped with a sidearm to connect to the safety flask.
in a reasonable time.
6.1.4 Safety Flask, 1.5 Lor larger borosilicate glass vacuum
4.2 After the filtration has been completed, the membranes
filter flask equipped with a sidearm to connect the vacuum
are washed with solvent, dried, and weighed. The particulate
system. A fuel and solvent resistance rubber hose through
contamination level is determined from the increase in the
which the grounding wire passes shall connect the sidearm of
mass of the test membranes relative to the control membranes,
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.
6.1.5 Vacuum System, either a water aspirated or a mechani-
5. Significance and Use
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 Lof 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
NOTE 3—When using a solid-pan balance, the air ionizer may be
to complete the filtration.This test method used about a quarter
omitted provided that, when weighing a membrane filter, it is placed on
of the volume used in the aviation fuel methods.
the pan so that no part protrudes over the edge of the pan.
5.2 The mass of particulates present in a fuel is a significant
6.2.2 Analytical Balance, single- or double-pan, the preci-
factor, along with the size and nature of the individual
sion standard deviation of which must be 0.07 mg or less.
particles, in the rapidity with which fuel system filters and
6.2.3 Crucible Tongs, for handling clean sample container
other small orifices in fuel systems can become plugged. This
lids.
test method provides a means of assessing the mass of
6.2.4 Drying Oven, naturally convected (without fan-
particulates present in a fuel sample.
assisted air circulation), controlling to 90 6 5°C.
5.3 The test method can be used in specifications and
6.2.5 Flushing Fluid Dispenser, an apparatus for dispensing
purchase documents as a means of controlling particulate
flushing fluid through a nominal 0.45 µm membrane filter.
contaminationlevelsinthefuelspurchased.Maximumparticu-
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
6.1 Filtration System—Arrange the following components
as shown in Fig. 1.
Supporting data (a membrane approval procedure) have been filed at ASTM
6.1.1 Funnel and Funnel Base, with filter support for a 47
International Headquarters and may be obtained by requesting Research Report RR:
mmdiametermembrane,andlockingringorspringactionclip. D02-1012.
´1
D6217–98 (2003)
FIG. 2 Apparatus for Filtering and Dispensing Flushing Fluid
provided the flushing fluid is pre-filtered through a 0.45-µm pore size
where such specifications are available. Other grades may be
membrane filter and precautions are taken to maintain appropriate
used, provided it is first ascertained that the reagent is of
cleanliness of the interior of the wash bottle
sufficient purity to permit its use without lessening the accu-
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 D 1193.
and marked at 10 mL intervals. 100 mL graduated cylinders
7.3 Flushing Fluids:
may be required for samples which filter slowly.
7.3.1 Heptane,(Warning—Flammable.)
6.2.8 Petri Dishes, approximately 12.5 cm in diameter, with
7.3.2 2,2,4-trimethylpentane (isoctane),(Warning—
removable glass supports for membrane filters.
Flammable.)
7.4 Propan-2-ol (2-propanol; isopropyl alcohol),
NOTE 5—Small watch glasses, approximately 5 to 7 cm in diameter,
have also been found suitable to support the membrane filters. (Warning—Flammable.)
7. Reagents and Materials
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For Suggestions on the testing of reagents not
7.1 Purity of Reagents—Reagent grade chemicals shall be
listed by the American Chemical Society, see Annual Standards for Laboratory
used in all tests. Unless otherwise indicated, it is intended that
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
all reagents shall conform to the specifications of the Commit-
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
tee onAnalytical Reagents of theAmerican Chemical Society, MD.
´1
D6217–98 (2003)
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 D 4057 or equivalent, taking precautions for cleanli-
diameter, nominal pore size 0.8-µm. ness of all equipment used. Ensure that the sample has not
passed through intermediate containers prior to placement in
NOTE 6—Membrane filters with a grid imprinted on their surface, may
the prepared container. (Warning—Samples obtained from
be used as control membrane filters for identification.
static storage may give results which are not representative of
7.8 Protective Cover, polyethylene film or clean aluminum
the bulk contents of the tank because of particulate matter
foil.
settling. Where possible, the contents of the tank should be
circulated or agitated before sampling, or the sampling per-
8. Preparation of Apparatus and Sample Containers
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 (50°F), 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 filling. Glass containers also allow for visual the fuel is highly contaminated, more than one set of filters
inspection of the container, after the sample is emptied, to may be required (see Section 11). The two membrane filters
confirm complete rinsing of the container. Epoxy lined sample used for each individual test shall be identified by marking the
cans, polytetrafluoroethylene (PTFE) bottles, and high density petri d
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.