1、Designation: D4171 16a 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, the year of last
2、revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope*1.1 This specification covers additives for aviation fuels (forexample, Specifications D910, D7547, and D1655) used toinhibit
3、ice formation 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 WARNING Mercury has been designated by manyregulatory agencies as a hazardous material that can causecentral nervous system, kidney a
4、nd liver damage. Mercury, orits vapor, may be hazardous to health and corrosive tomaterials. Caution should be taken when handling mercury andmercury containing products. See the applicable product Ma-terial Safety Data Sheet (MSDS) for details and EPAswebsitehttp:/www.epa.gov/mercury/faq.htmfor add
5、i-tional information. Users should be aware that selling mercuryand/or mercury containing products into your state or countrymay be prohibited by law.1.4 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
6、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-MartensClosed Cup Teste
7、rD268 Guide for Sampling and Testing Volatile Solvents andChemical Intermediates for Use in Paint and RelatedCoatings and MaterialD891 Test Methods for Specific Gravity,Apparent, of LiquidIndustrial ChemicalsD910 Specification for Leaded Aviation GasolinesD1078 Test Method for Distillation Range of
8、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 Volatile Sol-vents for Use in Paint, Varnish, Lacquer, and RelatedProductsD1364 Test Method for Water in
9、 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 Te
10、st 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) i
11、n Aviation FuelsD7547 Specification for Hydrocarbon Unleaded AviationGasolineE1 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
12、 ChemicalsE450 Test Method for Measurement of Color of Low-Colored Clear Liquids Using the Hunterlab Color Differ-ence Meter (Withdrawn 1993)3E1064 Test Method for Water in Organic Liquids by Coulo-metric Karl Fischer Titration1This specification is under the jurisdiction of ASTM Committee D02 onPet
13、roleum Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.J0.04 on Additives and Electrical Properties.Current edition approved Dec. 1, 2016. Published January 2017. Originallyapproved in 1982. Last previous edition approved in 2016 as D4171 16. DOI:10.1520/D4
14、171-16A.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.3The last approved version of this historical standar
15、d is referenced onwww.astm.org.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized pri
16、nciples on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.1E2251 Specification for Liquid-in-Glass ASTM Thermom-eters with Low-Hazar
17、d Precision LiquidsE2877 Guide for Digital Contact Thermometers3. 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
18、 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 availability, reduced toxicologicalconcerns, and lack of widely available methodology to
19、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.3.2 Type IIAnhydrous isopropanol, also described as99 % grade 2-Propanol or isopropyl alcohol, is used as ananti-icing additive in aviation ga
20、soline. (Warning Isopropa-nol (2-Propanol) is both flammable and an irritant; use withcaution.)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). Combustib
21、le, toxicmaterial.)3.3.1 Test Method D5006 can be used to determine theconcentration of DiEGME 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 req
22、uirements of Table 2, as manufactured.5. Sampling5.1 The material shall be sampled in accordance withPractice E300.6. Test Methods6.1 Determine the properties enumerated in this specifica-tion in accordance with the following ASTM methods:6.1.1 Relative DensityDetermine the relative density (thatis,
23、 specific gravity) at 20 C or 25 C with respect to water bya method accurate to the third 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 Distill
24、ation Thermometers (40C with a range from72 C to 126 C for isopropanol) conforming to the require-ments of Specification E1 or any other temperature measuringdevice that cover the temperature range of interest, such asthermocouples, thermistors, or resistance temperature detectors(RTDs). An instrume
25、nt meeting Guide E2877 or SpecificationE2251 may be used in preference to 40C if the instrumentprovides equivalent or better accuracy and precision.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 D1
26、476.6.1.8 AcidityTest Method D1613.6.1.9 Water MiscibilityTest Method D1722.6.1.10 Flash PointTest Methods D56, D93,orD3828.7. Keywords7.1 additives; aircraft fuel systems; aviation fuels; fuelsystem icing inhibitors; ice formationTABLE 1 Detailed Requirements for Isopropanol (99 % Grade)(Type II) F
27、SIIProperty RequirementASTM TestMethodAcidity, max, mg KOH/g 0.019 D1613Relative density:20 C 20 C25 C 25 C0.785 to 0.7870.782 to 0.784D268D268Color, platinum-cobalt, max 10 D1209 or E450Distillation range, max, C 1.5 (including 82.3 C) D1078Nonvolatile matter, max,mg/100 mL5 D1353Odor characteristi
28、c, nonresidual D1296Water, max, mass % 0.2 D1364Heptane miscibility at 20 C miscible without turbidity with19 vol heptane (99 % Grade)D1476Water miscibility at 25 C miscible without turbidity whendiluted with 10 vol distilledwaterD1722TABLE 2 Detailed Requirements for Fuel System Icing Inhibitors(Ty
29、pe III)PropertyRequirementASTM TestMethodDiEGME(Type III)Acid number, max, mgKOH/g0.09 D1613Color, platinum-cobalt,max10 D1209 or E450Purity, min, mass % 99.0 Annex A1pH of 25 % solution inwater (25 C 2 C)5.57.5 E70ARelative density,20 C 20 C1.0201.025D891 (Method A orB) or D4052Water, max, mass % D
30、1364, E1064,orE203Point of manufacture 0.10Point of use 0.8Flash point, min, C 85 C D93, D56,orD3828Antioxidant, mg/kg 50150BAPipette 25 mL of the inhibitor into a 100 mL volumetric flask and filled with freshlyboiled and cooled distilled water having a pH of 6.5 to 7.5. Measure the pH valuewith a p
31、H meter calibrated in accordance with Test Method E70.BAcceptable antioxidants are: 2,6-ditertiary-butyl-4-methylphenol, 2,4-dimethyl-6-tertiary-butyl phenol, 2,6-ditertiary-butyl phenol, and 75 % min 2,6-ditertiary-butylphenol plus 25 % max tertiary and tritertiary butyl phenols.D4171 16a2ANNEX(Man
32、datory 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 systemicing inhibitors (Type III). The test results are used to deter-mine if the inhibitor meets the purity requirements listed in
33、Table 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 the inhibitor are separated and measuredwith a flame ionization detector. Quantitation is made by peakarea measurement usin
34、g 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 all impurities (all components otherthan the inhibitor) are subtracted from 100 to calculate thepurity of the icing inhibitor.
35、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. Impurities affect inhibitor solubility in thefuel and reduce the effective concentration. Methods aretherefore needed to check addit
36、ive 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 de-scribed below.A1.4.2 Temperature ControlThe chromatograph must becapable of programmed temperature operation.A1.4.3 Sampl
37、e Inlet SystemAn automatic sampler withsplit injection is recommended, however, manual split 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 no
38、t 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 the icinginhibitors at the levels listed in Table 2.A1.4.5 ColumnAny gas chromatographic column can beused that provides separ
39、ation 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 IntegratorProvide means for the determination ofpeak areas for the impurities and the icing inhibitors. This canbe accomplished with a compute
40、r or electronic integrator.A1.4.7 Analytical BalanceCapable of measuring 0.1 mg.A1.5 ReagentsA1.5.1 Purity of ReagentsUse reagent grade chemicals inall tests. Unless otherwise indicated, it is intended that allreagents conform to the specifications of the Committee onAnalytical Reagents of the Ameri
41、can Chemical Society wheresuch specifications are available.4Other grades may be used,provided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.A1.5.2 AirUse air (hydrocarbon free) as the HFID oxi-dant. (Warni
42、ngAir is usually supplied as a compressed gasunder high pressure and supports combustion.)A1.5.3 HydrogenUse hydrogen (hydrocarbon free) as thefuel for the flame ionization detector. (WarningExtremelyflammable. Hydrogen is usually supplied as a compressed gasunder high pressure.)A1.5.4 HeliumUse hel
43、ium (hydrocarbon free) as the car-rier gas for the chromatograph. (WarningHelium is usuallysupplied as a compressed gas under high pressure.)A1.5.5 Ethylene GlycolUse ethylene glycol (anhydrous,99 + %) as a calibration standard for analysis of diethyleneglycol monomethyl ether. (WarningToxic, irrita
44、nt.)A1.5.6 Ethylene Glycol Monomethyl EtherUse EGME(anhydrous, 99 + %) 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 Socie
45、ty, Washington, DC. For suggestions on the testing of 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.T
46、ABLE A1.1 Recommended Operating ConditionsColumn 30 M by 0.32 mm bonded phase 86 % methyl, 14cyanopropyl 1701 (1.0 m film thickness)fused-silica capillary columnColumn temperature 100 C initial temperature, programmed to 250 Cat 12 C minInjection system Split injection system which contains a glassi
47、nsert liner that is firmly packed with silylatedglass wool. The split ratio is 50:1 and theinjection temperature is 250 CDetector Hydrogen flame ionization at 250 CSample volume 0.5 L with a 5 L syringeCarrier gas Helium at an average flow velocity of 20 cm/second (propane elutes in 2.5 min with aco
48、lumn temperature of 60 C) to give a flow rateof 1 mL minMake-up gas Helium at 20 mL minAir flow 350 mL/minHydrogen flow 30 mL/minD4171 16a3Combustible, toxic material.5)(WarningIn addition to otherprecautions, EGME has been shown to be a teratogen inanimals. Avoid inhalation. Do not get in eyes, on
49、skin, or onclothing. Wash thoroughly after 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 chromatographic instrumentation inaccordance with the manufacturers instructions. System oper-ating conditions will depend upon the column used andoptimization of
