ASTM D6422-99
(Test Method)Standard Test Method for Water Tolerance (Phase Separation) of Gasoline-Alcohol Blends (Withdrawn 2007)
Standard Test Method for Water Tolerance (Phase Separation) of Gasoline-Alcohol Blends (Withdrawn 2007)
SCOPE
1.1 This test method covers the ability of gasoline-alcohol blends to retain water in solution or in a stable suspension at the lowest temperature to which they are likely to be stored or exposed in use.
1.2 This test method is intended to measure the temperature at which a gasoline-alcohol blend separates into two distinct phases in accordance with the criteria defined in this test method. Samples that form a haze are considered not to have phase separated.
1.3 This test method is applicable to gasoline-alcohol blends for use as fuels in spark-ignition engines that contain saturated C1 to C4 alcohols only. The test method does not apply to fuels that contain an alcohol as the primary component, such as M85 or Ed85, or to gasoline-ether blends.
1.4 The values stated in SI units are the standard, except when other units are specified by federal regulation. Values given in parentheses are provided for informational purposes.
1.5 This standard may involve hazardous materials, operations, and equipment. 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.
WITHDRAWN RATIONALE
This test method covers the ability of gasoline-alcohol blends to retain water in solution or in a stable suspension at the lowest temperature to which they are likely to be stored or exposed in use.
This standard is being withdrawn without replacement; it lacks a precision statement and no acceptable precision statement could be developed from the round-robin program.
Formerly under the jurisdiction of Committee D02 on Petroleum Products and Lubricants, this test method was withdrawn in February 2007.
General Information
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
Designation:D6422–99
Standard Test Method for
Water Tolerance (Phase Separation) of Gasoline-Alcohol
Blends
This standard is issued under the fixed designation D 6422; 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 5842 Practice for Sampling and Handling of Fuels for
Volatility Measurement
1.1 This test method covers the ability of gasoline-alcohol
E 1 Specification forASTM Liquid-in-Glass Thermometers
blends to retain water in solution or in a stable suspension at
the lowest temperature to which they are likely to be stored or
3. Terminology
exposed in use.
3.1 Definitions:
1.2 This test method is intended to measure the temperature
3.1.1 gasoline, n—a volatile mixture of liquid hydrocar-
at which a gasoline-alcohol blend separates into two distinct
bons, generally containing small amounts of additives, suitable
phases in accordance with the criteria defined in this test
for use as a fuel in spark-ignition, internal combustion engines.
method. Samples that form a haze are considered not to have
3.1.2 gasoline-alcohol blend, n—a fuel consisting primarily
phase separated.
of gasoline, along with a substantial amount (more than 0.35
1.3 Thistestmethodisapplicabletogasoline-alcoholblends
mass % oxygen or more than 0.15 mass % oxygen if methanol
for use as fuels in spark-ignition engines that contain saturated
is the only oxygenate) of one or more alcohols.
C to C alcohols only.The test method does not apply to fuels
1 4
3.1.3 phase separation, n—the formation of two layers, a
that contain an alcohol as the primary component, such as M85
lower aqueous constituent and an upper hydrocarbon constitu-
or Ed85, or to gasoline-ether blends.
ent, separated by either a common boundary or a layer of
1.4 The values stated in SI units are the standard, except
emulsion.
when other units are specified by federal regulation. Values
3.1.3.1 Discussion—Test specimens having droplets cling-
given in parenthesis are provided for informational purposes.
ing to the sides of the container or collected on its bottom, that
1.5 This standard may involve hazardous materials, opera-
are visible to the unaided eye, are considered to be phase
tions, and equipment. This standard does not purport to
separated.
address all of the safety concerns, if any, associated with its
use. It is the responsibility of the user of the standard to
4. Summary of Test Method
establish appropriate safety and health practices and deter-
4.1 The sample of fuel is cooled at a controlled rate to its
mine the applicability of regulatory limitations prior to use.
lowest expected storage or use temperature and is periodically
2. Referenced Documents observed for phase separation. The apparatus of Test Method
2 D 2500 or a dry ice-isopropyl alcohol bath may be used. A
2.1 ASTM Standards:
maximum cooling rate of 2°C (4°F)/min is specified because
D 2500 Test Method for Cloud Point of Petroleum Products
phase separation in gasoline-alcohol blends can have a rela-
D 4057 Practice for Manual Sampling of Petroleum and
tively long but unpredictable induction period.
Petroleum Products
D 4306 Practice for Aviation Fuel Sample Containers for
5. Significance and Use
Tests Affected by Trace Contamination
5.1 Gasoline-alcohol blends have a very limited ability to
D 4814 SpecificationforAutomotiveSpark-IgnitionEngine
retain water in solution or in a stable suspension, and if the
Fuel
amount of water in the blend exceeds this limit, the fuel will
separate into a lower aqueous phase and an upper hydrocarbon
This test method is under the jurisdiction of ASTM Committee D-2 on
phase. The most important factor governing the ability of a
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
specific fuel to retain water without such separation is its
D02.A on Gasoline and Oxygenated Fuels.
temperature. This test method is intended to determine the
Current edition approved June 10, 1999. Published August 1999.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
maximumtemperatureatwhichthefuelwillseparate.The10th
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
percentile 6-h minimum temperatures or 10°C (50°F), which-
Standards volume information, refer to the standard’s Document Summary page on
ever is lower, for the time of year and geographic area of the
the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D6422–99
United States in which the fuel may be stored or used are 44.2 to 45.8 mm. It must be supported free of excessive
tabulated in Table 13 of Specification D 4814. The tempera- vibration and supported firmly in a vertical position in the
tures represent the maximum temperatures above which the cooling bath specified in 6.7 so that no more than 25 mm
fuel must not separate into two distinct phases. projects out of the cooling medium.
5.2 Since the aqueous phase can be highly corrosive to 6.5 Disk, made of cork or felt, 6 mm in thickness, to fit
many metals and the spark-ignition engine cannot operate on loosely on the inside bottom of the jacket.
such a fuel that has phase separated, such separation is very 6.6 Gasket—A ring form, about 5 mm in thickness, to fit
undesirable. snugly around the test container and loosely inside the jacket.
5.3 Blends containing low-molecular weight alcohols are The gasket may be made of rubber, leather, or other material
generally hygroscopic and can eventually absorb enough that is elastic enough to cling to the test container and hard
moisture from ambient air to cause separation. The problem of enough to hold its shape. Its purpose is to prevent the test
phase separation can usually be avoided if the fuels are container from touching the jacket.
sufficiently water-free initially and care is taken during distri- 6.7 Cooling Baths, maintained at prescribed temperatures
bution to prevent contact with water. To help ensure this, with a firm support to hold the jacket vertically, capable of
gasoline-alcohol blends shall be tested to the lowest tempera- reducing the test specimen temperature to –42°C (–44°F) for
tures that they expect to encounter, dependent on the time and the test analysis, similar to that specified in 6.7 of Test Method
geographic location of intended use, as tabulated in D 2500. The required bath temperatures may be maintained by
Table 13 of Specification D 4814. refrigeration, if available, otherwise by suitable freezing mix-
tures, such as a dry ice-isopropyl alcohol bath.
6. Apparatus (see Fig. 1)
6.8 Pipettes (optional), disposable or volumetric, for rins-
6.1 Test Container—The test container must be made of
ing and transferring test specimens into the test container.
clear, cylindrical glass, with a flat bottom, that has a 33.2 to
34.8-mm outside diameter, a 30 to 32.4-mm inside diameter, a
7. Reagents and Materials
wall thickness no greater than 1.6 mm, and a height between
7.1 Acetone—Technical grade acetone is suitable for use in
115 to 125 mm. The jar shall be marked with a line to indicate
the cooling baths, provided it does not leave a residue on
the test specimen height 54 6 3 mm above the inside bottom.
drying.
The specification conforms to the test jar identified in Test
NOTE 1—Warning: Extremely flammable.
Method D 2500.
6.2 Thermometer—ASTM thermometer 6C (range –80 to
7.2 Carbon Dioxide (Solid) or Dry Ice—A commercial
+20°C, with 1°C graduations, 76-mm immersion) meeting the
grade of dry ice is suitable for use in the cooling baths.
requirements in Specification E 1. A thermometer mounted to
NOTE 2—Warning: Extremely cold (–78.5°C). Avoid direct contact
pass through the stopper must be provided for each test
with the skin.
container.
6.3 Viton Rubber Stopper—Astopper of appropriate dimen-
7.3 Isopropyl Alcohol (2-propanol)—A commercial grade
sions to snugly fit the test container, bored centrally for the test
of dry isopropyl alcohol is suitable for use in the cooling baths.
thermometer. Other suitable types of rubber stoppers may be
NOTE 3—Warning: Flammable.
substituted for the Viton rubber stoppers.
6.4 Jacket, made of metal or glass, watertight, cylindrical, 7.4 Methyl Alcohol—A commercial or technical grade of
flat bottom, about 115 mm in depth, with an inside diameter of dry methyl alcohol is suitable for use in the cooling baths.
NOTE 1—Dimensions are in millimetres (not to scale).
FIG. 1 Position of Thermometer in Fuel Sample
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