1、Designation: D 4171 03An American National StandardStandard Specification forFuel System Icing Inhibitors1This standard is issued under the fixed designation D 4171; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last
2、revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This specification covers additives for aviation fuels(see Specifications D 910 and D 1655) used to inhibit iceformation i
3、n aircraft fuel systems.1.2 The values stated in SI units are to be regarded asstandard.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices
4、 and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 56 Test Method for Flash Point by the Tag Closed TesterD 93 Test Methods for Flash Point by Pensky-MartensClosed TesterD 268 Test Methods of Sampling and Testing VolatileSolvents and
5、 Chemical Intermediates for Use in Paint andRelated Coatings and MaterialsD 891 Test Methods for Specific Gravity, Apparent, ofLiquid Industrial ChemicalsD 910 Specification for Aviation GasolinesD 1078 Test Method for Distillation Range of VolatileOrganic LiquidsD 1209 Test Method for Color of Clea
6、r Liquids (Platinum-Cobalt Scale)D 1296 Test Method for Odor of Volatile Solvents andDiluentsD 1353 Test Method for Nonvolatile Matter in VolatileSolvents for Use in Paint, Varnish, Lacquer and RelatedProductsD 1364 Test Method for Water in Volatile Solvents (KarlFischer Reagent Titration Method)D 1
7、476 Test Method for Heptane Miscibility of LacquerSolventsD 1613 Test Method for Acidity in Volatile Solvents andChemical Intermediates Used in Paint, Varnish, Lacquer,and Related ProductsD 1655 Specification for Aviation Turbine FuelsD 1722 Test Method for Water Miscibility of Water-SolubleSolvents
8、D 3828 Test Methods for Flash Point by Small Scale ClosedTesterD 4052 Test Method for Density and Relative Density ofLiquids by Digital Density MeterD 5006 Test Method for Measurement of Fuel System IcingInhibitors (Ether Type) in Aviation FuelsE 1 Specification for ASTM ThermometersE 70 Test Method
9、 for pH of Aqueous Solutions with theGlass ElectrodeE 203 Test Method for Water Using Karl Fischer ReagentE 300 Practice for Sampling Industrial ChemicalsE 450 Method for Measurement of Color of Low-ColoredClear Liquids Using the Hunterlab Color DifferenceMeter3E 1064 Test Method for Water in Organi
10、c Liquids byCoulometric Karl Fischer Titration3. Classification3.1 Two types of fuel system icing inhibitors are provided asfollows:3.1.1 Type IEthylene glycol monomethyl ether is used asan anti-icing additive in both aviation gasoline and aviationturbine fuels.NOTE 1Ethylene glycol monomethyl ether
11、 (EGME) was previouslyincluded in this specification, last appearing in D 417194. EGME isconsidered technically satisfactory for this application, but has beengenerally replaced by DiEGME due to availability, reduced toxicologicalconcerns, and lack of widely available methodology to determine FSIIco
12、ncentration in aviation fuels when a mixture is known to be present, orwhen the identity of the FSII present in the fuel is not clearly known.3.2 Type IIAnhydrous isopropanol, also described as99 % grade 2-Propanol or isopropyl alcohol, is used as an1This specification is under the jurisdiction of A
13、STM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.J0.04 on Additives and Electrical Properties.Current edition approved Dec. 1, 2003. Published January 2004. Originallyapproved in 1982. Last previous edition approved in 1998 as D 417198.2For re
14、ferenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Withdrawn.1Copyright ASTM International, 100 Barr Harbor Drive, PO
15、Box C700, West Conshohocken, PA 19428-2959, United States.anti-icing additive in aviation gasoline. (WarningIsopropanol (2-Propanol) is both flammable and an irritant; usewith caution.)3.3 Type IIIDiethylene glycol monomethyl ether (Di-EGME) is used as an anti-icing additive in both aviationgasoline
16、 and aviation turbine fuel. (WarningDiethyleneglycol monomethyl ether, (DiEGME). Combustible, toxicmaterial.)3.3.1 Test Method D 5006 can be used to determine theconcentration of DiEGME in aviation fuels.4. Properties4.1 Type IIIsopropanol anti-icing additive shall conformto the requirements of Tabl
17、e 1, as manufactured.4.2 Type IIIDiethylene glycol monomethyl ether shallconform to the requirements of Table 2, as manufactured.5. Sampling5.1 The material shall be sampled in accordance withPractice E 300.6. Test Methods6.1 The properties enumerated in this specification shall bedetermined in acco
18、rdance with the following ASTM methods:6.1.1 Relative DensityDetermine the relative density (thatis, specific gravity) at 20 or 25C with respect to water by amethod accurate to the third decimal place. See Section 5 ofTest Method D 268, Test Method D 4052, or Method A or B ofTest Methods D 891.6.1.2
19、 ColorTest Method D 1209 or E 450.6.1.3 Distillation RangeTest Method D 1078 usingASTM Solvents Distillation Thermometers (40C with a rangefrom 72 to 126C for isopropanol) conforming to the require-ments of Specification E 1.6.1.4 Nonvolatile MatterTest Method D 1353.6.1.5 OdorTest Method 1296.6.1.6
20、 WaterTest Method D 1364, E 1064, or E 203.6.1.7 Heptane MiscibilityTest Method D 1476.6.1.8 AcidityTest Method D 1613.6.1.9 Water MiscibilityTest Method D 1722.6.1.10 Flash PointTest Methods 56, D 93, or D 3828.7. Keywords7.1 additives; aircraft fuel systems; aviation fuels; fuelsystem icing inhibi
21、tors; ice formationTABLE 1 Detailed Requirements for Isopropanol (99 % Grade)(Type II) FSIIProperty RequirementASTM TestMethodAcidity, max, mg KOH/g 0.019 D 1613Relative density:20/20C25/25C0.785 to 0.7870.782 to 0.784D 268D 268Color, platinum-cobalt, max 10 D 1209 or E450Distillation range, max, C
22、1.5 (including 82.3C) D 1078Nonvolatile matter, max,mg/100 mL5 D 1353Odor characteristic, nonresidual D 1296Water, max, mass % 0.2 D 1364Heptane miscibility at 20C miscible without turbidity with19 vol 99 % heptaneD 1476Water miscibility at 25C miscible without turbidity whendiluted with 10 vol dist
23、illedwaterD 1722TABLE 2 Detailed Requirements for Fuel System Icing Inhibitors(Type III)PropertyRequirementASTM TestMethodDiEGME(Type III)Acid number, max, mgKOH/g0.09 D 1613Color, platinum-cobalt,max10 D 1209 or E450Purity, min, mass % 99.0 Annex A1pH of 25 % solution inwater (25 6 2C)5.57.5 E 70AR
24、elative density,20/20C1.0201.025D 891 (Method A orB) or D4052Water, max, mass % D 1364, E1064, orE 203Point of manufacture 0.10Point of use 0.8Flash point, min, C 85C D 93, D 56, orD 3828Antioxidant, mg/kg 50150BATwenty-five millilitres of the inhibitor shall be pipetted into a 100-ml volumetricflas
25、k and filled with freshly boiled and cooled distilled water having a pH of 6.5 to7.5. The pH value shall be measured with a pH meter calibrated in accordance withTest Method E 70.BAcceptable antioxidants are: 2,6-ditertiary-butyl-4-methylphenol, 2,4-dimethyl-6-tertiary-butyl phenol, 2,6-ditertiary-b
26、utyl phenol, and 75 % min 2,6-ditertiary-butyl phenol plus 25 % max tertiary and tritertiary butyl phenols.D4171032ANNEX(Mandatory Information)A1. TEST METHOD FOR DETERMINING PURITY OF FUEL SYSTEM ICING INHIBITORS (TYPES I AND III)A1.1 ScopeA1.1.1 This test method measures the purity of fuel systemi
27、cing inhibitors (Type III). The test results are used to deter-mine if the inhibitor meets the purity requirements listed inTable 2.A1.2 Summary of Test MethodA1.2.1 A representative sample of fuel system icing inhibi-tor (Type III) is injected into a capillary gas chromatograph andthe components of
28、 the inhibitor are separated and measuredwith a flame ionization detector. Quantitation is made by peakarea measurement using external standardization and a com-puting integrator. As the linear dynamic range of many gaschromatographic detectors is often exceeded for the majorcomponent, the sum of al
29、l impurities (all components otherthan the inhibitor) are subtracted from 100 to calculate thepurity of the icing inhibitor.A1.3 Significance and UseA1.3.1 Fuel system icing inhibitor performance (Type III) isbased upon test results using the pure inhibitor in a specificconcentration range. Impuriti
30、es affect inhibitor solubility in thefuel and reduce the effective concentration. Methods aretherefore needed to check additive purity to ensure adequateperformance in the aircraft.A1.4 ApparatusA1.4.1 Gas ChromatographAny gas chromatographic in-strumentation can be used that meets the requirements
31、de-scribed below.A1.4.2 Temperature ControlThe chromatograph must becapable of programmed temperature operation.A1.4.3 Sample Inlet SystemAn automatic sampler withsplit injection is recommended, however, manual split injectionis acceptable if care is taken to assure injected sample volumeand rate of
32、 injection is constant. On-column injection isacceptable, however, modifications to the procedure are re-quired which are not specified here.A1.4.4 DetectorA hydrogen flame ionization detector(HFID) is recommended, however, any detector can be usedthat has the sensitivity to measure the purity of th
33、e icinginhibitors at the levels listed in Table 2.A1.4.5 ColumnAny gas chromatographic column can beused that provides separation of the impurities from the fuelsystem icing inhibitor (Type III). Columns and conditions thathave been used successfully are shown in Table A1.1.A1.4.6 IntegratorMeans mu
34、st be provided for the deter-mination of peak areas for the impurities and the icinginhibitors. This can be accomplished with a computer orelectronic integrator.A1.4.7 Analytical BalanceCapable of measuring 0.1 mg.A1.5 ReagentsA1.5.1 Purity of ReagentsReagent grade chemicals willbe used in all tests
35、. Unless otherwise indicated, it is intendedthat all reagents conform to the specifications of the Committeeon Analytical Reagents of the American Chemical Societywhere such specifications are available.4Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently hig
36、h purity to permit its use without lessening theaccuracy of the determination.A1.5.2 AirAir (hydrocarbon free) is used as the HFIDoxidant. (WarningAir is usually supplied as a compressedgas under high pressure and supports combustion.)A1.5.3 HydrogenHydrogen (hydrocarbon free) is used asthe fuel for
37、 the flame ionization detector. (WarningExtremely flammable. Hydrogen is usually supplied as acompressed gas under high pressure.)A1.5.4 HeliumHelium (hydrocarbon free) is used as thecarrier gas for the chromatograph. (WarningHelium isusually supplied as a compressed gas under high pressure.)A1.5.5
38、Ethylene GlycolEthylene glycol (anhydrous,99 + %) is used as a calibration standard for analysis ofdiethylene glycol monomethyl ether. (WarningToxic, irri-tant.)A1.5.6 Ethylene Glycol Monomethyl EtherEGME (anhy-drous, 99 + %) is used as a calibration standard for analysis ofdiethylene glycol monomet
39、hyl ether. (WarningSee Note 1.)(WarningEthylene glycol monomethyl ether (EGME).4Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for Labor
40、atoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.TABLE A1.1 Recommended Operating ConditionsColumn 30M by 0.32 mm bonded phase 86 % methyl, 14cyanopropyl 1701 (1.0 film thickness)fused-si
41、lica capillary columnColumn temperature 100C initial temperature, programmed to 250Cat 12C/minInjection system Split injection system which contains a glassinsert liner that is firmly packed with silylatedglass wool. The split ratio is 50:1 and theinjection temperature is 250CDetector Hydrogen flame
42、 ionization at 250CSample volume 0.5 microlitre with a 5 microlitre syringeCarrier gas Helium at an average flow velocity of 20 cm/second (propane elutes in 2.5 min with acolumn temperature of 60C) to give a flow rateof 1 mL/minMake-up gas Helium at 20 mL/minAir flow 350 mL/minHydrogen flow 30 mL/mi
43、nD4171033Combustible, toxic material.5)(WarningIn addition to otherprecautions, EGME has been shown to be a teratogen inanimals. Avoid inhalation. Do not get in eyes, on skin, or onclothing. Wash thoroughly after handling.)A1.5.7 Triethylene Glycol Monomethyl EtherThis mate-rial is used as a calibra
44、tion standard for analysis of diethyleneglycol monomethyl ether. The purity of this material should bedetermined and the standard adjusted for this purity.A1.6 Preparation of ApparatusA1.6.1 Install the gas chromatographic instrumentation inaccordance with the manufacturers instructions. System oper
45、-ating conditions will depend upon the column used andoptimization of performance. See Table A1.1 for recommendedconditions.NOTE A1.1The position of the capillary column in the injection portand in the detector is very important. Consult the instrument manufactur-ers instruction manual for specific
46、instructions. In general the columnshould be installed in such a manner that one end extends into the injectionport and into the bottom of the glass liner and the other end extends intothe detector up to within a few mm of the exit end of the flame jet.A1.6.2 System PerformanceSystem operating condi
47、tionsmust be used that effect baseline separation of the componentsof interest. A minimum resolution of 1.5 is required toaccurately determine icing inhibitor purity. The resolution iscalculated according to the following equation:R 52t22 t1!W11 W2(A1.1)where:t1= time (seconds) for peak 1 at apex,t2
48、= time (seconds) for peak 2 at apex,W1= peak width at base (seconds) for peak 1, andW1= peak width at base (seconds) for peak 2.A1.7 ProcedureA1.7.1 CalibrationDetermine the response factor foreach component of interest by preparing and analyzing samplesof known composition. As any one component use
49、d in thecalibration standard may contain one of the other components,it is best to prepare one calibration standard for each compo-nent in a pure solvent at the expected concentration range (inthis case, approximately 0.05 % by mass). A “pure” solvent inthis case means one of high purity (99 %) which does notcontain the components of interest.A1.7.1.1 Calibration standards for ethylene glycol, EGME,and triethylene glycol monomethyl ether should be preparedfor analysis of DiEGME. The purity of triethylene glycolmo
