ASTM D4860-91(1995)
(Test Method)Standard Test Method for Free Water and Particulate Contamination in Mid-Distillate Fuels (Clear and Bright Numerical Rating)
Standard Test Method for Free Water and Particulate Contamination in Mid-Distillate Fuels (Clear and Bright Numerical Rating)
SCOPE
1.1 This test method provides a rapid, portable means for field and laboratory use to visually inspect for particulate matter and numerically rate free water in aviation turbine and distillate fuels.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.3 This standard does not purport to address all of the safety problems, 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. For specific hazard statements, see 11.2.3.1 and Annex A1.
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NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
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Designation: D 4860 – 91 (Reapproved 1995) An American National Standard
Standard Test Method for
Free Water and Particulate Contamination in Mid-Distillate
Fuels (Clear and Bright Numerical Rating)
This standard is issued under the fixed designation D 4860; 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 sometimes referred to as silt or sediment, present in fuel as a
result of contamination by air-blown dusts, corrosion by-
1.1 This test method provides a rapid, portable means for
products, fuel instability, or protective-coating deterioration.
field and laboratory use to inspect visually for particulate
3.1.3 clear-and-bright (also termed clean-and-bright)— a
matter and numerically rate free water in aviation turbine and
condition in which the fuel contains no visible water drops or
distillate fuels.
particulates and is free of haze or cloudiness.
1.2 The values stated in SI units are to be regarded as the
3.1.4 Micro-Separometer clear-and-bright (MSEP-
standard. The values given in parentheses are for information
C&B)—a numerical rating indicating the presence and ease of
only.
removal of free water and particulate contamination by filtra-
1.3 This standard does not purport to address all of the
tion.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Summary of Test Method
priate safety and health practices and determine the applica-
4.1 Visual inspection of the fuel sample for free water and
bility of regulatory limitations prior to use. For specific hazard
particulate matter is performed immediately when the sample
statements, see Note 6 and Annex A1.
is taken. A glass container is used to view for water haze, and
2. Referenced Documents the fuel sample is swirled to create a vortex to detect the
presence of particulate matter.
2.1 ASTM Standards:
4.2 A numerical rating for free water is obtained by filtering
D 1500 Test Method for ASTM Color of Petroleum Prod-
a portion of the fuel sample at a programmed rate (50 mL/45
ucts (ASTM Color Scale)
s) through a standard fiberglass coalescer/filter. A portion of the
D 1744 Test Method for Water in Liquid Petroleum Prod-
effluent is used to establish a reference (100) level by a light
ucts by Karl Fischer Reagent
transmittance measurement. Another portion of the unproc-
D 2276 Test Method for Particulate Contaminant in Avia-
essed (unfiltered) fuel sample is then compared to the 100
tion Fuel by Line Sampling
reference level. The results are reported on a 50 to 100 scale to
D 2709 Test Method for Water and Sediment in Middle
the nearest whole number. A test can be performed in 5 to 10
Distillate Fuels by Centrifuge
min.
D 4057 Practice for Manual Sampling of Petroleum and
Petroleum Products
NOTE 1—The standard fiberglass coalescer/filter consists of a precision
D 4176 Test Method for Free Water and Particulate Con-
machined, aluminum housing, containing fiber-glass material that has
been selected to specific air flow characteristics. These criteria have a
tamination in Distillate Fuels (Visual Inspection Proce-
direct bearing on the test results.
dures)
5. Significance and Use
3. Terminology
5.1 The test provides a field test to evaluate visually a fuel
3.1 Definitions of Terms Specific to This Standard:
sample for particulate matter and free water similar to Test
3.1.1 free water—water in excess of that soluble in the fuel
Method D 4176 plus a numerical rating for free water. High
at the temperature of the test and appearing in the fuel as a haze
numerical ratings indicate that the fuel is relatively free of free
or cloudiness, or as droplets.
water. The degree of water and particulate contamination can
3.1.2 solid particulates—small solid or semi-solid particles,
be measured using other methods such as Test Methods
D 1744, D 2276, and D 2709.
This test method is under the jurisdiction of ASTM Committee D02 on
5.2 The color of the sample does not affect the measure-
Petroleum Products and Lubricantsand is the direct responsibility of Subcommittee
ment. Limited laboratory evaluations of samples have deter-
D02.14 on Stability and Cleanliness of Liquid Fuels.
Current edition approved Dec. 23, 1991. Published February 1992. Originally mined the degree of free water can be rated in fuels with dark
published as D 4860 – 88. Last previous edition D 4860 – 88.
opaque color having a darker rating than 5 in Test Method
Annual Book of ASTM Standards, Vol 05.01.
D 1500.
Annual Book of ASTM Standards, Vol 05.02.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 4860
6. Interferences chargeable battery pack or being connected to an a-c power
source using power cords that are furnished for various
6.1 When a fuel is visually inspected at or below the cloud
voltages. Connection to an a-c power source provides power to
point temperature of the fuel, small amounts of solid wax
the unit and effects battery recharge. The accessories as well as
particles can be confused with a water-induced haze or
the expendable materials for six tests can be packed in the
cloudiness.
cover of the lockable case.
6.2 The presence of free water or particulate can be ob-
7.1.2 The Micro-Separometer Mark V Deluxe model and
scured and missed during visual inspection of the fuel, if the
the associated control panel is shown in Fig. 1. The emulsifier
ASTM color rating is greater than five.
is on the right side of the raised panel and the syringe drive
7. Apparatus mechanism is on the left side. The control panel containing the
4 operating controls is mounted on the fixed panel in the left side
7.1 Micro-Separometer, Mark V Deluxe
of the case.
7.1.1 The Micro-Separometer is a completely portable and
7.1.3 All of the controls are located in a push-button array
self contained unit capable of operating on an internal re-
on the control panel. The push buttons illuminate when
depressed, thus, indicating operational status. A circuit breaker
located on the control panel provides protection for the a-c
The Micro-Separometer is available from EMCEE Electronics, Inc., 520
power circuit.
Cypress Ave., Venice, FL 34292.
FIG. 1 Micro-Separometer Mark V Deluxe and Control Panel
D 4860
7.1.4 By depressing the ON push button, the electronic 7.2.2 Syringe, (Barrel, B and Plunger, C), a disposable
circuits are energized. The ON push button light pulses on and plastic syringe.
off when the instrument is being operated by an a-c source and 7.2.3 Vials, (D)—25-mm outside diameter vial premarked
constantly remains on when the battery (d-c) pack is used. The for proper alignment in the turbidimeter.
A-G lettered push buttons sequentially illuminate on and off 7.2.4 Alumicel Coalescer/Filter (E), labeled Clear and
indicating ready operational status. Bright—an expendable, precalibrated aluminum coalescer/
filter cell with a tapered end to fit the syringe.
NOTE 2—Of the lettered (A-G) push buttons, only the C push button is
7.2.5 Wire Aid (F)—A piece of wire with a loop on one end,
applicable to this test method.
used to release the air trapped in the barrel of the syringe when
7.1.5 The RESET push button can be depressed at any time
the plunger is being inserted. A wire aid is supplied with each
to cancel the test in progress and restore the program to the
Micro-Separometer.
initial start mode. The lettered push buttons commence to
7.2.6 Beaker, catch pan or the plastic container supplied
illuminate sequentially, thus indicating a ready operational
with each Micro-Separometer can be used to receive the waste
status enabling test mode selection.
fuel during the coalescence period of the test (not shown).
7.1.6 Test mode selection is accomplished by depressing the
7.3 New Syringe, Syringe Plug, Test Sample Vial, and
applicable lettered (C) push button. The depressed push button 5
Alumicel Coalescer/Filter are used in each test. These
illuminates and the sequential illumination of the other lettered
expendable materials are available in a kit containing supplies
push buttons ceases. The START push button also illuminates
for six tests. This kit, termed Micro-Separometer Clear and
and the syringe drive mechanism moves to the UP position.
Bright Six Pack, is designed to fit inside the top lid of the
7.1.7 The START push button, when depressed sequentially
Micro-Separometer.
after depressing the C lettered push button, initiates the
7.4 Sample Container, cylindrical, wide-mouth, clear-glass,
automatic program for the clear-and-bright test.
container capable of holding at least 900 mL of fuel. The
7.1.8 The turbidimeter is located under the main control
minimum dimensions of the container shall be 100 mm in
panel and consists of a well in which the sample vial is placed,
diameter with a height of 120 mm. The container shall have a
a light source, and a photocell. A mark on the panel in front of
lid to seal the contents.
the turbidimeter well is used to align the sample vial.
7.1.9 By depressing the appropriate ARROWED push but-
8. Sampling
ton, the displayed value on the meter can be increased/
8.1 Sampling shall be consistent with the procedures of
decreased, as required, to establish the 100 reference level for
Practice D 4057. When practical, take the sample directly into
the vial of filtered fuel sample in the turbidimeter.
the sample container; however, in some instances the sample
7.2 Accessory equipment and expendable materials needed
can be transferred from the apparatus used to secure the sample
to perform the test are shown in Fig. 2 and consist of the
to the sample container used in the test.
following:
NOTE 3—Exercise care when transferring a sample from one container
7.2.1 Syringe Plug, (A)—A plastic plug used to stopper the
to another to ensure the test sample is representative of the fuel source.
syringe.
8.2 Use the following procedure when the sample is drawn
directly into the sample container from a sampling valve:
8.2.1 Be sure the sampling valve is free of loose solid
contaminants. If rust or other loose encrustations are present,
remove with a cloth; then flush the sampling valve before
taking the actual sample.
8.2.2 Rinse a clean sample container thoroughly with the
fuel being sampled.
8.2.3 Draw approximately 700 mL of fuel into the sample
container (at least ⁄4 full) as rapidly as possible. Use a full flush
rather than permitting the fuel sample to trickle out.
8.2.4 A lid must be placed on the container to prevent water
absorption or loss from the sample to the ambient environment,
especially if the test is performed under different environmen-
tal conditions than those of the sample site or at a later time.
9. Preparation of Apparatus
9.1 Locate the Micro-Separometer on a clean workbench in
an area in which the temperature is within the operating limits
of the instrument, 0 to 50° (32 to 122°F).
A registered trademark of EMCEE Electronics, Inc.
A B CDEF
The Micro-Separometer Clear & Bright Six Pack is available from EMCEE
FIG. 2 Test Supplies and Accessory Electronics, Inc., 520 Cypress Ave., Venice, FL 34292.
D 4860
9.2 Open the case and remove the six-pack box from the lid.
Raise the right panel until completely vertical and locked in
place. When a-c power is available, connect the power cord
and turn the instrument on; otherwise operate using battery
power.
9.3 Depress the switch (push button) marked ON.
NOTE 4—Flickering of the power indicator light, during any portion of
a test sequence being performed when using battery power, indicates that
recharging is necessary.
9.4 Have ready a supply of syringes, syringe plugs, vials,
and Alumicel coalescer/filters. In addition, have the wire aid
readily available and the catch pan positioned under the syringe
drive mechanism to accept the spent fuel.
10. Conditioning
10.1 Under no circumstances is the test fuel to be prefiltered
as filter media can remove the very materials, water and
particulate matter, that the test is designed to detect.
FIG. 3 Plunger Insertion
10.2 The sample temperature shall not be lower than the
temperature at which the fuel will be stored and used. Too low
drive mechanism. Electrically bond the coalescer/filter to the
a temperature may cause a haze to form from water previously
instrument by using the ground lead provided. Insert the end
in solution. When possible, perform the test with the fuel
with the banana plug into the recepticle located left of the
sample at a temperature representing a real-use situation.
syringe drive mechanism and attach the alligator clip to one of
11. Procedure
the coalescer/filter fins. Position a waste container beneath the
11.1 Visual inspection for water or particulate contamina- Alumicel coalescer/filter to collect the unwanted portion of the
tion. processed fuel sample during the coalescing/filtering period of
11.1.1 Immediately upon drawing a sample for field testing, the test (Fig. 4).
check visually for evidence of water or particulate contamina-
NOTE 5—Caution: Alumicel coalescer/filters should be electrically
tion. Hold the sample container up to the ambient light source
bonded to the Micro-Separometer to prevent buildup of an electrostatic
and view the fuel through the walls of the container, visually
charge that could result in ignition of flammable test fluids (Fig. 4).
examining for haze or lack of clarity. Check the same sample
11.2.4 Initiate the Coalescing/Filtering Process:
by swirling the fuel in the sample container to produce a
11.2.4.1 Depress the START push button which initiates the
vortex. The bottom of the vortex is visually examined for
automatic program (see Table 1). The automatic program is a
particulate matter. Record the visual clarity as clear-and-bright
series of timed events controlled by the instrument that begins
or not clear-and-bright. Record if particulate matter or water
with the syringe drive mechanism forcing the fuel through the
was or was not viewed at the bottom of the vortex. Cap the
Alumicel coalescer/filter.
container.
11.2.4.2 Disregard the first 5 mL of expended fuel and,
11.2 Numerical Rating of Free Water Using Micro-
using a new vial, collect the next 15 mL of fuel sample being
Separometer Mark V Deluxe:
11.2.1 Select the clear-and-bright test mode by depressing
the push button marked C which illuminates. The syringe drive
mechanism travels to the UP position and the proper syringe
drive speed is automatically selected.
11.2.2 Prepare Fuel Sampl
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