ASTM D4171-03(2010)
(Specification)Standard Specification for Fuel System Icing Inhibitors
Standard Specification for Fuel System Icing Inhibitors
ABSTRACT
This specification covers additives for aviation fuels used to inhibit ice formation in aircraft fuel systems. Three types of fuel system icing inhibitors are provided as follows: type I - ethylene glycol monomethyl ether, type II - anhydrous isopropanol, and type III - diethylene glycol monomethyl ether. The relative density, color, distillation range, non-volatile matter, and odor shall be tested to meet the requirements prescribed. The water properties, heptanes miscibility, acidity, water miscibility, and flash point shall be tested to meet the requirements prescribed.
SIGNIFICANCE AND USE
A1.3.1 Fuel system icing inhibitor performance (Type III) is based upon test results using the pure inhibitor in a specific concentration range. Impurities affect inhibitor solubility in the fuel and reduce the effective concentration. Methods are therefore needed to check additive purity to ensure adequate performance in the aircraft.
SCOPE
1.1 This specification covers additives for aviation fuels (see Specifications D910 and D1655) used to inhibit ice formation in aircraft fuel systems.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 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.
A1.1.1 This test method measures the purity of fuel system icing inhibitors (Type III). The test results are used to determine if the inhibitor meets the purity requirements listed in Table 2.
General Information
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Standards Content (Sample)
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An American National Standard
Designation: D4171 – 03 (Reapproved 2010)
Standard Specification for
Fuel System Icing Inhibitors
This standard is issued under the fixed designation D4171; 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 D1364 Test Method for Water in Volatile Solvents (Karl
Fischer Reagent Titration Method)
1.1 This specification covers additives for aviation fuels
D1476 Test Method for Heptane Miscibility of Lacquer
(see Specifications D910 and D1655) used to inhibit ice
Solvents
formation in aircraft fuel systems.
D1613 Test Method for Acidity in Volatile Solvents and
1.2 The values stated in SI units are to be regarded as
Chemical Intermediates Used in Paint, Varnish, Lacquer,
standard. No other units of measurement are included in this
and Related Products
standard.
D1655 Specification for Aviation Turbine Fuels
1.3 This standard does not purport to address all of the
D1722 Test Method for Water Miscibility of Water-Soluble
safety concerns, if any, associated with its use. It is the
Solvents
responsibility of the user of this standard to establish appro-
D3828 Test Methods for Flash Point by Small Scale Closed
priate safety and health practices and determine the applica-
Cup Tester
bility of regulatory limitations prior to use.
D4052 Test Method for Density, Relative Density, and API
2. Referenced Documents Gravity of Liquids by Digital Density Meter
D5006 Test Method for Measurement of Fuel System Icing
2.1 ASTM Standards:
Inhibitors (Ether Type) in Aviation Fuels
D56 Test Method for Flash Point by Tag Closed Cup Tester
E1 Specification for ASTM Liquid-in-Glass Thermometers
D93 Test Methods for Flash Point by Pensky-Martens
E70 Test Method for pH of Aqueous Solutions With the
Closed Cup Tester
Glass Electrode
D268 Guide for Sampling andTestingVolatile Solvents and
E203 Test Method forWater UsingVolumetric Karl Fischer
Chemical Intermediates for Use in Paint and Related
Titration
Coatings and Material
E300 Practice for Sampling Industrial Chemicals
D891 Test Methods for Specific Gravity, Apparent, of
E450 Method for Measurement of Color of Low-Colored
Liquid Industrial Chemicals
Clear Liquids Using the Hunterlab Color Difference Me-
D910 Specification for Aviation Gasolines
ter
D1078 Test Method for Distillation Range of Volatile Or-
E1064 Test Method for Water in Organic Liquids by Cou-
ganic Liquids
lometric Karl Fischer Titration
D1209 Test Method for Color of Clear Liquids (Platinum-
Cobalt Scale)
3. Classification
D1296 Test Method for Odor of Volatile Solvents and
3.1 Twotypesoffuelsystemicinginhibitorsareprovidedas
Diluents
follows:
D1353 Test Method for Nonvolatile Matter in Volatile
3.1.1 Type I—Ethylene glycol monomethyl ether is used as
Solvents for Use in Paint, Varnish, Lacquer, and Related
an anti-icing additive in both aviation gasoline and aviation
Products
turbine fuels.
NOTE 1—Ethylene glycol monomethyl ether (EGME) was previously
This specification is under the jurisdiction of ASTM Committee D02 on
included in this specification, last appearing in D4171–94. EGME is
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
considered technically satisfactory for this application, but has been
D02.J0.04 on Additives and Electrical Properties.
generally replaced by DiEGME due to availability, reduced toxicological
Current edition approved July 1, 2010. Published July 2010. Originally approved
concerns, and lack of widely available methodology to determine FSII
in 1982. Last previous edition approved in 2001 as D4171–03. DOI: 10.1520/
concentration in aviation fuels when a mixture is known to be present, or
D4171-03R10.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or when the identity of the FSII present in the fuel is not clearly known.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. Withdrawn.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D4171 – 03 (2010)
TABLE 2 Detailed Requirements for Fuel System Icing Inhibitors
3.2 Type II—Anhydrous isopropanol, also described as
(Type III)
99 % grade 2-Propanol or isopropyl alcohol, is used as an
Requirement
anti-icing additive in aviation gasoline. (Warning—
Property ASTM Test
DiEGME
Isopropanol (2-Propanol) is both flammable and an irritant; use
Method
(Type III)
with caution.)
Acid number, max, mg 0.09 D1613
3.3 Type III—Diethylene glycol monomethyl ether (Di-
KOH/g
EGME) is used as an anti-icing additive in both aviation
Color, platinum-cobalt, 10 D1209 or E450
gasoline and aviation turbine fuel. (Warning—Diethylene max
Purity, min, mass % 99.0 Annex A1
glycol monomethyl ether, (DiEGME). Combustible, toxic
A
pH of 25 % solution in 5.5–7.5 E70
material.)
water (25 6 2°C)
3.3.1 Test Method D5006 can be used to determine the
Relative density, 1.020– D891 (Method A or
20°/20°C 1.025 B) or D4052
concentration of DiEGME in aviation fuels.
Water, max, mass % D1364, E1064,or
E203
4. Properties
Point of manufacture 0.10
Point of use 0.8
4.1 Type II—Isopropanol anti-icing additive shall conform
Flash point, min, °C 85°C D93, D56,or
to the requirements of Table 1, as manufactured.
D3828
B
Antioxidant, mg/kg 50–150
4.2 Type III—Diethylene glycol monomethyl ether shall
A
conform to the requirements of Table 2, as manufactured. Twenty-five millilitres of the inhibitor shall be pipetted into a 100-ml volumetric
flask and filled with freshly boiled and cooled distilled water having a pH of 6.5 to
7.5. The pH value shall be measured with a pH meter calibrated in accordance with
5. Sampling
Test Method E70.
B
Acceptable antioxidants are: 2,6-ditertiary-butyl-4-methylphenol, 2,4-dimethyl-
5.1 The material shall be sampled in accordance with
6-tertiary-butyl phenol, 2,6-ditertiary-butyl phenol, and 75 % min 2,6-ditertiary-
Practice E300.
butyl phenol plus 25 % max tertiary and tritertiary butyl phenols.
6. Test Methods
6.1.1 Relative Density—Determine the relative density (that
is, specific gravity) at 20 or 25°C with respect to water by a
6.1 The properties enumerated in this specification shall be
method accurate to the third decimal place. See Section 5 of
determined in accordance with the following ASTM methods:
Test Method D268, Test Method D4052, or Method A or B of
Test Methods D891.
TABLE 1 Detailed Requirements for Isopropanol (99 % Grade)
6.1.2 Color—Test Method D1209 or E450.
(Type II) FSII
6.1.3 Distillation Range—Test Method D1078 usingASTM
ASTM Test
Property Requirement Solvents DistillationThermometers (40C with a range from 72
Method
to 126°C for isopropanol) conforming to the requirements of
Acidity, max, mg KOH/g 0.019 D1613
Specification E1.
Relative density:
6.1.4 Nonvolatile Matter—Test Method D1353.
20/20°C 0.785 to 0.787 D268
25/25°C 0.782 to 0.784 D268
6.1.5 Odor—Test Method D1296.
Color, platinum-cobalt, max 10 D1209 or E450
6.1.6 Water—Test Method D1364, E1064,or E203.
Distillation range, max, °C 1.5 (including 82.3°C) D1078
Nonvolatile matter, max, 5 D1353 6.1.7 Heptane Miscibility—Test Method D1476.
mg/100 mL
6.1.8 Acidity—Test Method D1613.
Odor characteristic, nonresidual D1296
6.1.9 Water Miscibility—Test Method D1722.
Water, max, mass % 0.2 D1364
Heptane miscibility at 20°C miscible without turbidity with D1476 6.1.10 Flash Point—Test Methods D56, D93,or D3828.
19 vol 99 % heptane
Water miscibility at 25°C miscible without turbidity when D1722
7. Keywords
diluted with 10 vol distilled
7.1 additives; aircraft fuel systems; aviation fuels; fuel
water
system icing inhibitors; ice formation
D4171 – 03 (2010)
ANNEX
(Mandatory Information)
A1. TEST METHOD FOR DETERMINING PURITY OF FUEL SYSTEM ICING INHIBITORS (TYPES I AND III)
TABLE A1.1 Recommended Operating Conditions
A1.1 Scope
Column 30M by 0.32 mm bonded phase 86 % methyl, 14
A1.1.1 This test method measures the purity of fuel system
cyanopropyl ’1701’ (1.0 µ film thickness)
icing inhibitors (Type III). The test results are used to deter-
fused-silica capillary column
Column temperature 100°C initial temperature, programmed to 250°C
mine if the inhibitor meets the purity requirements listed in
at 12°C/min
Table 2.
Injection system Split injection system which contains a glass
insert liner that is firmly packed with silylated
glass wool. The split ratio is 50:1 and the
A1.2 Summary of Test Method
injection temperature is 250°C
A1.2.1 A representative sample of fuel system icing inhibi- Detector Hydrogen flame ionization at 250°C
Sample volume 0.5 microlitre witha5microlitre syringe
tor(TypeIII)isinjectedintoacapillarygaschromatographand
Carrier gas Helium at an average flow velocity of 20 cm/
the components of the inhibitor are separated and measured
second (propane elutes in 2.5 min with a
column temperature of 60°C) to give a flow rate
with a flame ionization detector. Quantitation is made by peak
of −1 mL/min
area measurement using external standardization and a com-
Make-up gas Helium at 20 mL/min
puting integrator. As the linear dynamic range of many gas
Air flow 350 mL/min
Hydrogen flow 30 mL/min
chromatographic detectors is often exceeded for the major
component, the sum of all impurities (all components other
than the inhibitor) are subtracted from 100 to calculate the
purity of the icing inhibitor.
A1.5 Reagents
A1.3 Significance and Use
A1.5.1 Purity of Reagents—Reagent grade chemicals will
be used in all tests. Unless otherwise indicated, it is intended
A1.3.1 Fuelsystemicinginhibitorperformance(TypeIII)is
thatallreagentsconformtothespecificationsoftheCommittee
based upon test results using the pure inhibitor in a specific
on Analytical Reagents of the American Chemical Society
concentration range. Impurities affect inhibitor solubility in the
where such specificat
...
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