ASTM D4171-98

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An American National Standard
Designation: D 4171 – 98
Standard Specification for
Fuel System Icing Inhibitors
This standard is issued under the fixed designation D 4171; 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 1613 Test Method for Acidity in Volatile Solvents and
Chemical Intermediates Used in Paint, Varnish, Lacquer,
1.1 This specification covers additives for aviation fuels
and Related Products
(see Specifications D 910 and D 1655) used to inhibit ice
D 1655 Specification for Aviation Turbine Fuels
formation in aircraft fuel systems.
D 1722 Test Method for Water Miscibility of Water-Soluble
1.2 The values stated in SI units are to be regarded as
Solvents
standard.
D 3828 Test Methods for Flash Point by Small Scale Closed
1.3 This standard does not purport to address all of the
Tester
safety concerns, if any, associated with its use. It is the
D 4052 Test Method for Density and Relative Density of
responsibility of the user of this standard to establish appro-
Liquids by Digital Density Meter
priate safety and health practices and determine the applica-
E 1 Specification for ASTM Thermometers
bility of regulatory limitations prior to use.
E 70 Test Method for PH of Aqueous Solutions with the
2. Referenced Documents
Glass Electrode
E 203 Test Method for Water Using Karl Fischer Reagent
2.1 ASTM Standards:
E 300 Practice for Sampling Industrial Chemicals
D 56 Test Method for Flash Point by the Tag Closed Tester
E 450 Method for Measurement of Color of Low-Colored
D 93 Test Methods for Flash Point by Pensky-Martens
Clear Liquids Using the Hunterlab Color Difference
Closed Tester
Meter
D 268 Test Methods of Sampling and Testing Volatile
E 1064 Test Method for Water in Organic Liquids by
Solvents and Chemical Intermediates for Use in Paint and
Coulometric Karl Fischer Titration
Related Coatings and Materials
D 891 Test Methods for Specific Gravity of Liquid Indus-
3. Classification
trial Chemicals
3.1 Two types of fuel system icing inhibitor are provided as
D 910 Specification for Aviation Gasolines
follows:
D 1078 Test Method for Distillation Range of Volatile
3.1.1 Type I—Ethylene glycol monomethyl ether is used as
Organic Liquids
an anti-icing additive in both aviation gasoline and aviation
D 1209 Test Method for Color of Clear Liquids (Platinum-
turbine fuels.
Cobalt Scale)
D 1296 Test Method for Odor of Volatile Solvents and
NOTE 1—Ethylene glycol monomethy ether (EGME) was previously
Diluents included in this specification, last appearing in D 4171–94. EGME is
considered technically satisfactory for this application, but has been
D 1353 Test Method for Nonvolatile Matter in Volatile
generally replaced by DiEGME due to availability, reduced toxicological
Solvents for Use in Paint, Varnish, Lacquer and Related
concerns, and lack of widely available methodology to determine FSII
Products
concentration in aviation fuels when a mixture is known to be present, or
D 1364 Test Method for Water in Volatile Solvents (Fischer
when the identity of the FSII present in the fuel is not clearly known.
Reagent Titration Method)
3.2 Type II—Anhydrous isopropanol, also described as
D 1476 Test Method for Heptane Miscibility of Lacquer
99 % grade 2-Propanol or isopropyl alcohol, is used as an
Solvents
anti-icing additive in aviation gasoline.
NOTE 2—Isopropanol, (2-Propanol). Flammable material. Irritant.
This specification is under the jurisdiction of ASTM Committee D02 on
3.3 Type III—Diethylene glycol monomethyl ether is used
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
as an anti-icing additive in both aviation gasoline and aviation
D02.J0 on Aviation Fuels.
turbine fuel.
Current edition approved June 10, 1998. Published September 1998. Originally
published as D 4171 – 82. Last previous edition D 4171 – 97a.
Annual Book of ASTM Standards, Vol 05.01.
3 5
Annual Book of ASTM Standards, Vol 06.04. Annual Book of ASTM Standards, Vol 05.02.
4 6
Annual Book of ASTM Standards, Vol 15.05. Annual Book of ASTM Standards, Vol 14.03.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D4171–98
NOTE 3—Warning: Diethylene glycol monomethyl ether, (DiEGME). TABLE 2 Detailed Requirements for Fuel System Icing Inhibitors
(Type III)
Combustible, toxic material.
Requirement
4. Properties
Property ASTM Test
DiEGME
Method
4.1 Type II—Isopropanol anti-icing additive shall conform (Type III)
to the requirements of Table 1, as manufactured.
Acid number, max, mg 0.09 D 1613
KOH/g
4.2 Type III—Diethylene glycol monomethyl ether shall
Color, platinum-cobalt, 10 D 1209 or E450
conform to the requirements of Table 2, as manufactured.
max
Purity, min, mass % 99.0 Annex A1
A
5. Sampling
pH of 25 % solution in 5.5–7.5 E 70
water (25 6 2°C)
5.1 The material shall be sampled in accordance with
Relative density, 1.020– D 891 (Method A or
Practice E 300.
20°/20°C 1.025 B) or D4052
Water, max, mass % D 1364, E1064, or
E 203
6. Test Methods
Point of manufacture 0.10
6.1 The properties enumerated in this specification shall be
Point of use 0.8
Flash point, min, °C 85°C D 93, D56, or
determined in accordance with the following ASTM methods:
D 3828
6.1.1 Relative Density—Determine the relative density (that
B
Antioxidant, mg/kg 50–150
is, specific gravity) at 20 or 25°C with respect to water by a
A
Twenty-five milliliters of the inhibitor shall be pipetted into a 100-ml volumetric
method accurate to the third decimal place. See Section 5 of
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
Test Method D 268, Test Method D 4052, or Method A or B of
Test Method E 70.
D891.
B
Acceptable antioxidants are: 2,6-ditertiary-butyl-4-methylphenol, 2,4-dimethyl-
6.1.2 Color—Test Method D 1209 or E 450.
6-tertiary-butyl phenol, 2,6-ditertiary-butyl phenol, and 75 % min 2,6-ditertiary-
butyl phenol plus 25 % max tertiary and tritertiary butyl phenols.
TABLE 1 Detailed Requirements for Isopropanol (99 % Grade)
(Type II) FSII
6.1.3 Distillation Range—Test Method D 1078 using
ASTM Test
ASTM Solvents Distillation Thermometers (40C with a range
Property Requirement
Method
from 72 to 126°C for isopropanol) conforming to the require-
Acidity, max, mg KOH/g 0.019 D 1613
ments of Specification E 1.
Relative density:
6.1.4 Nonvolatile Matter—Test Method D 1353.
20/20°C 0.785 to 0.787 D 268
6.1.5 Odor—Test Method 1296.
25/25°C 0.782 to 0.784 D 268
Color, platinum-cobalt, max 10 D 1209 or E450
6.1.6 Water—Test Method D 1364, E 1064, or E 203.
Distillation range, max, °C 1.5 (including 82.3°C) D 1078
6.1.7 Heptane Miscibility—Test Method D 1476.
Nonvolatile matter, max, 5 D 1353
mg/100 mL 6.1.8 Acidity—Test Method D 1613.
Odor characteristic, nonresidual D 1296
6.1.9 Water Miscibility—Test Method D 1722.
Water, max, mass % 0.2 D 1364
6.1.10 Flash Point—Test Methods 56, D 93, or D 3828.
Heptane miscibility at 20°C miscible without turbidity with D 1476
19 vol 99 % heptane
7. Keywords
Water miscibility at 25°C miscible without turbidity when D 1722
diluted with 10 vol distilled
7.1 additives; aircraft fuel systems; aviation fuels; fuel
water
system icing inhibitors; ice formation
ANNEX
(Mandatory Information)
A1. TEST METHOD FOR DETERMINING PURITY OF FUEL SYSTEM ICING INHIBITORS (TYPES I AND III)
A1.1 Scope area measurement using external standardization and a com-
puting integrator. As the linear dynamic range of many gas
A1.1.1 This test method measures the purity of fuel system
chromatographic detectors is often exceeded for the major
icing inhibitors (Type III). The test results are used to deter-
component, the sum of all impurities (all components other
mine if the inhibitor meets the purity requirements listed in
than the inhibitor) are subtracted from 100 to calculate the
Table 2.
purity of the icing inhibitor.
A1.2 Summary of Test Method
A1.3 Significance and Use
A1.2.1 A representative sample of fuel system icing inhibi- A1.3.1 Fuel system icing inhibitor performance (Type III) is
tor (Type III) is injected into a capillary gas chromatograph and based upon test results using the pure inhibitor in a specific
the components of the inhibitor are separated and measured concentration range. Impurities affect inhibitor solubility in the
with a flame ionization detector. Quantitation is made by peak fuel and reduce the effective concentration. Methods are
D4171–98
therefore needed to check additive purity to ensure adequate used, provided it is first ascertained that the reagent is of
performance in the aircraft. sufficiently high purity to permit its use without lessening the
accuracy of the determination.
A1.4 Apparatus
A1.5.2 Air—Air (hydrocarbon free) is used as the HFID
oxidant.
A1.4.1 Gas Chromatograph—Any gas chromatographic in-
strumentation can be used that meets the requirements de-
NOTE A1.1—Air: Warning: Air is usually supplied as a compressed
scribed below.
gas under high pressure and supports combustion.
A1.4.2 Temperature Control—The chromatograph must be
A1.5.3 Hydrogen—Hydrogen (hydrocarbon free) is used as
capable of programmed temperature operation.
the fuel for the flame ionization detector.
A1.4.3 Sample Inlet System—An automatic sampler with
split injection is recommended, however, manual split injection NOTE A1.2—Hydrogen: Warning: Extremely flammable. Hydrogen is
usually supplied as a compressed gas under high pressure.
is acceptable if care is taken to assure injected sample volume
and rate of injection is constant. On-column injection is
A1.5.4 Helium—Helium (hydrocarbon free) is us
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