1、Designation: D4171 03 (Reapproved 2010)An American National StandardStandard Specification forFuel System Icing Inhibitors1This standard is issued under the fixed designation D4171; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, t
2、he year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This specification covers additives for aviation fuels(see Specifications D910 and D1655) used to inhibit i
3、ceformation in aircraft fuel systems.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the us
4、er of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D56 Test Method for Flash Point by Tag Closed Cup TesterD93 Test Methods for Flash Point by Pensky-MartensClose
5、d Cup TesterD268 Guide for Sampling and Testing Volatile Solvents andChemical Intermediates for Use in Paint and RelatedCoatings and MaterialD891 Test Methods for Specific Gravity, Apparent, ofLiquid Industrial ChemicalsD910 Specification for Aviation GasolinesD1078 Test Method for Distillation Rang
6、e of Volatile Or-ganic LiquidsD1209 Test Method for Color of Clear Liquids (Platinum-Cobalt Scale)D1296 Test Method for Odor of Volatile Solvents andDiluentsD1353 Test Method for Nonvolatile Matter in VolatileSolvents for Use in Paint, Varnish, Lacquer, and RelatedProductsD1364 Test Method for Water
7、 in Volatile Solvents (KarlFischer Reagent Titration Method)D1476 Test Method for Heptane Miscibility of LacquerSolventsD1613 Test Method for Acidity in Volatile Solvents andChemical Intermediates Used in Paint, Varnish, Lacquer,and Related ProductsD1655 Specification for Aviation Turbine FuelsD1722
8、 Test Method for Water Miscibility of Water-SolubleSolventsD3828 Test Methods for Flash Point by Small Scale ClosedCup TesterD4052 Test Method for Density, Relative Density, and APIGravity of Liquids by Digital Density MeterD5006 Test Method for Measurement of Fuel System IcingInhibitors (Ether Type
9、) in Aviation FuelsE1 Specification for ASTM Liquid-in-Glass ThermometersE70 Test Method for pH of Aqueous Solutions With theGlass ElectrodeE203 Test Method for Water Using Volumetric Karl FischerTitrationE300 Practice for Sampling Industrial ChemicalsE450 Method for Measurement of Color of Low-Colo
10、redClear Liquids Using the Hunterlab Color DifferenceMeter3E1064 Test Method for Water in Organic Liquids by Cou-lometric 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 a
11、dditive in both aviation gasoline and aviationturbine fuels.NOTE 1Ethylene glycol monomethyl ether (EGME) was previouslyincluded in this specification, last appearing in D417194. EGME isconsidered technically satisfactory for this application, but has beengenerally replaced by DiEGME due to availabi
12、lity, reduced toxicologicalconcerns, and lack of widely available methodology to determine FSIIconcentration 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.1This specification is under the jurisdiction of ASTM Committ
13、ee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.J0.04 on Additives and Electrical Properties.Current edition approved July 1, 2010. Published July 2010. Originally approvedin 1982. Last previous edition approved in 2001 as D417103. DOI: 10.1520/D4171-03
14、R10.2For referenced 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
15、 Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3.2 Type IIAnhydrous isopropanol, also described as99 % grade 2-Propanol or isopropyl alcohol, is used as ananti-icing additive in aviation gasoline. (WarningIsopropanol (2-Propanol) is both flammable and an irritant; usewith cauti
16、on.)3.3 Type IIIDiethylene glycol monomethyl ether (Di-EGME) is used as an anti-icing additive in both aviationgasoline and aviation turbine fuel. (WarningDiethyleneglycol monomethyl ether, (DiEGME). Combustible, toxicmaterial.)3.3.1 Test Method D5006 can be used to determine theconcentration of DiE
17、GME in aviation fuels.4. Properties4.1 Type IIIsopropanol anti-icing additive shall conformto the requirements of Table 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 accor
18、dance withPractice E300.6. Test Methods6.1 The properties enumerated in this specification shall bedetermined in accordance 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 th
19、ird decimal place. See Section 5 ofTest Method D268, Test Method D4052, or Method A or B ofTest Methods D891.6.1.2 ColorTest Method D1209 or E450.6.1.3 Distillation RangeTest Method D1078 using ASTMSolvents Distillation Thermometers (40C with a range from 72to 126C for isopropanol) conforming to the
20、 requirements ofSpecification E1.6.1.4 Nonvolatile MatterTest Method D1353.6.1.5 OdorTest Method D1296.6.1.6 WaterTest Method D1364, E1064,orE203.6.1.7 Heptane MiscibilityTest Method D1476.6.1.8 AcidityTest Method D1613.6.1.9 Water MiscibilityTest Method D1722.6.1.10 Flash PointTest Methods D56, D93
21、,orD3828.7. Keywords7.1 additives; aircraft fuel systems; aviation fuels; fuelsystem icing inhibitors; ice formationTABLE 1 Detailed Requirements for Isopropanol (99 % Grade)(Type II) FSIIProperty RequirementASTM TestMethodAcidity, max, mg KOH/g 0.019 D1613Relative density:20/20C25/25C0.785 to 0.787
22、0.782 to 0.784D268D268Color, platinum-cobalt, max 10 D1209 or E450Distillation range, max, C 1.5 (including 82.3C) D1078Nonvolatile matter, max,mg/100 mL5 D1353Odor characteristic, nonresidual D1296Water, max, mass % 0.2 D1364Heptane miscibility at 20C miscible without turbidity with19 vol 99 % hept
23、aneD1476Water miscibility at 25C miscible without turbidity whendiluted with 10 vol distilledwaterD1722TABLE 2 Detailed Requirements for Fuel System Icing Inhibitors(Type III)PropertyRequirementASTM TestMethodDiEGME(Type III)Acid number, max, mgKOH/g0.09 D1613Color, platinum-cobalt,max10 D1209 or E4
24、50Purity, min, mass % 99.0 Annex A1pH of 25 % solution inwater (25 6 2C)5.57.5 E70ARelative density,20/20C1.0201.025D891 (Method A orB) or D4052Water, max, mass % D1364, E1064,orE203Point of manufacture 0.10Point of use 0.8Flash point, min, C 85C D93, D56,orD3828Antioxidant, mg/kg 50150BATwenty-five
25、 millilitres of the inhibitor shall be pipetted into a 100-ml volumetricflask 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 E70.BAcceptable antioxidants are: 2,6-ditertiary-b
26、utyl-4-methylphenol, 2,4-dimethyl-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.D4171 03 (2010)2ANNEX(Mandatory Information)A1. TEST METHOD FOR DETERMINING PURITY OF FUEL SYSTEM ICING INHIBITORS (TY
27、PES I AND III)A1.1 ScopeA1.1.1 This test method measures the purity of fuel systemicing 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
28、-tor (Type III) is injected into a capillary gas chromatograph andthe components of 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 g
29、aschromatographic detectors is often exceeded for the majorcomponent, the sum of all 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 up
30、on test results using the pure inhibitor in a specificconcentration range. Impurities 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 Chromatogra
31、phAny gas chromatographic in-strumentation can be used that meets the requirements 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
32、injectionis acceptable if care is taken to assure injected sample volumeand rate of 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, ho
33、wever, any detector can be usedthat has the sensitivity to measure the purity of the 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 condition
34、s thathave been used successfully are shown in Table A1.1.A1.4.6 IntegratorMeans must 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.
35、5 ReagentsA1.5.1 Purity of ReagentsReagent grade chemicals willbe used in all tests. 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
36、may beused, provided it is first ascertained that the reagent is ofsufficiently high 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 sup
37、ports combustion.)A1.5.3 HydrogenHydrogen (hydrocarbon free) is used asthe fuel for 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.
38、 (WarningHelium isusually supplied as a compressed gas under high pressure.)A1.5.5 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,
39、 99 + %) is used as a calibration standard for analysis ofdiethylene glycol monomethyl 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
40、reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, 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 b
41、y 0.32 mm bonded phase 86 % methyl, 14cyanopropyl 1701 (1.0 film thickness)fused-silica 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.
42、The split ratio is 50:1 and theinjection temperature is 250CDetector Hydrogen flame ionization at 250CSample volume 0.5 microlitre witha5microlitre 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
43、1 mL/minMake-up gas Helium at 20 mL/minAir flow 350 mL/minHydrogen flow 30 mL/minD4171 03 (2010)3Combustible, 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
44、 handling.)A1.5.7 Triethylene Glycol Monomethyl EtherThis mate-rial is used as a calibration 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 chrom
45、atographic instrumentation inaccordance with the manufacturers instructions. System oper-ating conditions will depend upon the column used andoptimization of performance. See TableA1.1 for recommendedconditions.NOTE A1.1The position of the capillary column in the injection portand in the detector is
46、 very important. Consult the instrument manufactur-ers instruction manual for specific 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
47、few mm of the exit end of the flame jet.A1.6.2 System PerformanceSystem operating conditionsmust 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 f
48、ollowing equation:R 52t22 t1!W11 W2(A1.1)where:t1= time (seconds) for peak 1 at apex,t2= 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 in
49、terest by preparing and analyzing samplesof known composition. As any one component used 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 mon
