1、Designation: D 2274 03aDesignation: 388/97An American National StandardStandard Test Method forOxidation Stability of Distillate Fuel Oil (AcceleratedMethod)1This standard is issued under the fixed designation D 2274; the number immediately following the designation indicates the year oforiginal ado
2、ption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1
3、. Scope1.1 This test method covers the measurement of the inherentstability of middle distillate petroleum fuels under specifiedoxidizing conditions at 95C.NOTE 1Fuels used in establishing the precision measures for this testmethod were described as gas oil, diesel fuel, No. 2 heating oil, and DFM,a
4、 Navy distillate fuel suitable for diesels, boilers, and gas turbines. (Theterm DFM is no longer used when referring to fuel meeting MIL-F-16884requirements; rather it is called F76 as it conforms to NATO F76requirements.) While the test method may be used for fuels outside therange of these fuels,
5、the precision measures may not apply.1.2 This test method is not applicable to fuels containingresidual oil or significant amounts of components derived fromnon-petroleum sources.1.3 The values given in acceptable SI units are to beregarded as the standard. The values in parentheses are forinformati
6、on only.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 standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Refe
7、renced Documents2.1 ASTM Standards:2D 381 Test Method for Gum Content in Fuels by JetEvaporationD 943 Test Method for Oxidation Characteristics of Inhib-ited Mineral OilsD 1193 Specification for Reagent WaterD 4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD 4177 Practice for Au
8、tomatic Sampling of Petroleum andPetroleum ProductsD 4625 Test Method for Distillate Fuel Storage Stability at43C (110F)2.2 Military Specification:3MIL-F-16884 Fuel, Navy Distillate3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 adherent insolubles (formerly adherent gum)mater
9、ial which is produced in the course of stressing distillatefuel under the conditions of this test and which adheres to theglassware after fuel has been flushed from the system.3.1.2 filterable insolublesmaterial, which is produced inthe course of stressing distillate fuel under the conditions ofthis
10、 test, which is capable of being removed from the fuel byfiltration. This includes both material suspended in the fuel andmaterial easily removed from the oxidation cell and oxygendelivery tube with hydrocarbon solvent.3.1.3 inherent stabilitythe resistance to change whenexposed to air, but in the a
11、bsence of other environmentalfactors such as water, or reactive metallic surfaces and dirt.3.1.4 total insolublessum of the adherent and filterableinsolubles.3.1.5 zero timethe time the first of a batch of oxidationcells is placed in the heating bath.3.1.5.1 DiscussionThis is the time taken as the s
12、tart of the16 h of residence in the heating bath.4. Summary of Test Method4.1 A 350-mL volume of filtered middle distillate fuel isaged at 95C (203F) for 16 h while oxygen is bubbled throughthe sample at a rate of 3 L/h. After aging, the sample is cooledto approximately room temperature before filte
13、ring to obtain1This test method is under the jurisdiction of Committee D02 on PetroleumProducts and Lubricants and is the direct responsibility of Subcommittee D02.14 onStability and Cleanliness of Liquid Fuels.Current edition approved Nov. 1, 2003. Published December 2003. Originallyapproved in 196
14、4. Last previous edition approved in 2003 as D 227403.2For 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.3Availa
15、ble from Standardization Documents Order Desk, Bldg. 4, 700 RobbinsAve., Philadelphia, PA 19111-5098. Attn: NPODS1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.the filterable insolubles quantity. Adherent insolubles are thenremoved
16、from the oxidation cell and associated glassware withtrisolvent. The trisolvent is evaporated to obtain the quantity ofadherent insolubles. The sum of the filterable and adherentinsolubles, expressed as milligrams per 100 mL, is reported astotal insolubles.5. Significance and Use5.1 This test method
17、 provides a basis for the estimation ofthe storage stability of middle distillate fuels such as No. 2 fueloil.5.2 The test method may not provide a prediction of thequantity of insolubles that will form in field storage over anygiven period of time. The amount of insolubles formed in suchfield stora
18、ge is subject to the specific conditions which are toovariable for this test method to predict accurately.5.3 Test Method D 2274 yields results more rapidly thanTest Method D 4625, the 43C bottle test. However, as a resultof the significantly elevated temperature and the pure oxygenatmosphere, the n
19、ature and amount of insolubles may deviateto a greater extent than Test Method D 4625 from those formedin field storage.6. Interferences6.1 Oxidation is a major chemical process causing adherentand filterable insolubles to form. Any substance such as copperor chromium that catalyzes oxidation reacti
20、ons will causegreater quantities of insolubles to form. Since the apparatusused in this test can also be used in Test Method D 943, wherecoils of copper and steel are used, it is important that anyresidues that could contain these metals be eliminated from theapparatus by thorough cleaning prior to
21、use. Similarly, topreclude the presence of chromium ions, as well as to protectlaboratory personnel from potential harm, chromic acid shallnot be used for cleaning glassware in the practice of thismethod.6.2 It has been found that commercial grades of acetone, ifused in the trisolvent, can have impu
22、rities which cause anapparently greater level of adherent insolubles to be measured.It is, therefore, critical that only reagent (or higher) gradematerials be used in preparing the trisolvent mixture.6.3 Ultraviolet light exposure has been found to increase theamount of total insolubles. Therefore,
23、the fuel being testedshall be shielded from direct exposure to ultraviolet light(sunlight or fluorescent). Conduct all sampling, measuring,filtration, and weighing away from direct sunlight and in asdark an area as would be compatible with other laboratoryoperations. Storage before stress, the stres
24、s period and cool-down after stressing shall be in the dark.7. ApparatusNOTE 2It is suggested that all equipment be calibrated according tomanufacturers instructions on a periodic basis to assure consistency ofresults.7.1 Oxidation Cell, of borosilicate glass, as shown in Fig. 1,shall consist of a t
25、est tube, condenser, and oxygen deliverytube. This cell is identical to that used in Test Method D 943.FIG. 1 Oxidation CellD 2274 03a27.2 Heating Bath, with a thermostatically controlled liquidmedium, shall be capable of maintaining the bath temperatureat 95 6 0.2C (203 6 0.4F). It shall be fitted
26、with a suitablestirring device to provide a uniform temperature throughout thebath. It shall be large enough to hold the desired number ofoxidation cells immersed to a depth of approximately 350 mm.Further, the bath construction must permit shielding the fuelsamples in the oxidation cells from light
27、 while they areundergoing oxidation.47.3 Flowmeters, shall have a capability of measuring 3 60.3 L/h of oxygen. One flowmeter shall be provided for eachoxidation cell.7.4 Filter Drying Oven, shall be capable of safely evapo-rating the solvent at 80 6 2C (176 6 4F) for the drying offilter materials.7
28、.5 Glassware Drying Oven, shall be capable of dryingglassware at 105 6 5C (221 6 9F).7.6 Filter Assembly, see Fig. 2, shall be capable of holdingthe filters described in 7.7.7.7 Filter Media5, 47 mm diameter cellulose estersurfactant-free membrane filters with a nominal pore size of0.8 m.7.7.1 Singl
29、e filters are to be used for prefiltration.7.7.2 A matched weight pair of filters or alternatively, apreweighed control and sample, filters shall be used fordetermination of filterable insolubles7.8 Evaporating Vessel, borosilicate glass beaker, 200-mLcapacity, tall style.7.9 Hot Plate, capable of h
30、eating a liquid in the evaporatingvessel (7.8) to 135C (275F).8. Reagents and Materials8.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of
31、the American Chemical Society,where such specifications are available.6Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.8.2 Purity of WaterUnless otherwise indicated, referenc
32、eto water shall be understood to mean reagent water as definedby Type III of Specification D 1193.8.3 2.2,4-trimethylpentanel (isooctane), 99.75 % purity pre-filtered through a filter medium of the type specified in 7.7.8.4 Oxygen, 99.5 % purity or better. When the oxygen isdelivered through a plant
33、 system of piping, a filter shall beprovided adjacent to the constant temperature bath to preventthe introduction of line debris or moisture into the oxidationcells; a pressure regulator adequate to maintain a constant flowof gas through the apparatus shall also be used. A tank ofoxygen of the speci
34、fied purity can be used provided it isequipped with a two-stage pressure regulator. (WarningOxygen vigorously accelerates combustion. Do not use equip-ment having exposed surfaces containing oil or grease.)8.5 Trisolvent, a mixture of equal volumes of acetone,methanol, and toluene. See 8.1. (Warning
35、It is particularlyimportant that technical, commercial, practical, or industrialgrades (however they are designated by the particular manu-facturer) are not to be used, as their use may lead to apparentlyincreased levels of adherent insolubles.) (WarningFire haz-ard, toxic.)9. Samples and Sampling9.
36、1 When obtaining samples for the laboratory, followPractices D 4057 or D 4177, or other standard practice capableof providing representative samples.9.2 Analyze fuel samples as soon as possible after receipt.When a fuel cannot be tested within one day, blanket it with aninert gas such as oxygen-free
37、 nitrogen, argon, or helium andstore at a temperature no higher than 10C (50F) but not lowerthan the cloud point. (WarningPlastic containers are notacceptable for samples due to the potential for leaching ofplasticizers. Samples should be taken preferably in metal canspreviously cleaned according to
38、 Practice D 4057. Borosilicateglass containers can be used if they are wrapped or boxed toexclude light. Do not use soft (soda) glass containers.)9.3 Test SamplesReduction of the laboratory sample totest sample size (about 400 mL for each determination)depends upon the size of sample received by the
39、 laboratory. Ifthe laboratory sample is stored in a tank, drum, or 19-L (5-gal)or larger can, use the pertinent procedures of Practice D 4057.Thoroughly mix smaller laboratory samples by shaking, roll-ing, or other techniques before taking an aliquot portion bypouring, pipetting, or other means. Cle
40、an any tube, thief, pipet,beaker, or other substance that is to contact the laboratorysample with trisolvent and rinse with a portion of the sample4This apparatus is available from suppliers of specialty petroleum testingequipment.5Supporting data have been filed at ASTM International Headquarters a
41、nd maybe obtained by requesting Research Report RR: D02-1012. Filters may be qualifiedusing the procedure in this research report.6Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the Americ
42、an Chemical Society, see Annual Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.FIG. 2 Apparatus for Determining Filterable InsolublesD 2274 03a3prior to use. Prior to
43、 mixing thoroughly and taking an aliquot,allow samples that have been stored at temperatures muchbelow 10C (50F) to warm to room temperature; thus allow-ing any separated wax to redissolve and to allow the viscosityto decrease to a point where mixing is effective.10. Preparation of Apparatus10.1 Pre
44、paration of Glassware Other Than OxidationCellsRinse all glassware thoroughly with trisolvent followedby water, then wash with a mildly alkaline or neutral laboratorydetergent. Rinse three times with deionized or distilled waterfollowed by acetone to remove water.10.2 Preparation of Oxidation Cells
45、and AccessoriesAfter completion of 10.1, fill oxidation cells with laboratorydetergent in water. Place the oxygen delivery tube in theoxidation cell, place the condenser over the oxygen deliverytube and allow to soak at least two hours. Wash, drain, thenrinse five times with tap water followed by th
46、ree rinses withdistilled or deionized water meeting Specification D 1193 TypeIII requirements. Rinse with acetone; drain and allow theoxidation cell and oxygen delivery tube to dry.10.3 Preparation of Evaporating BeakersDry the 200-mLcleaned beakers (10.1) for1hinanoven at 105 6 5C (2216 9F). Place
47、the beakers in a desiccator (without desiccant)and allow to cool for 1 h. Weigh beakers to the nearest 0.1 mg.11. Procedure11.1 Preparing the SamplePlace one filter (described in7.7) on the filter support and clamp the filter funnel to thesupport as shown in Fig. 2. Apply suction (approximately 80kP
48、a (12 psi). Pour 400 mL of the fuel through the filter (see7.7) into a clean (10.1) 500-mL glass suction flask. Repeatpreparation for each sample to be run. After filtration iscomplete, discard the filter media. Never use the same filtersfor a second increment of fuel, because any material deposited
49、on the filters by a previous increment of fuel can result in agreater removal of solids from the next increment.11.2 Assembling the Oxidation Apparatus:11.2.1 Place a clean oxygen delivery tube into a cleanoxidation cell (Section 10) and pour 350 6 5 mL of the filteredfuel into the cell. As soon thereafter as possible, but in no casegreater than 1 h after measuring the fuel, immerse the test cellin the 95C (203F) heating bath. During any interim periodstore the cell in the dark. The level of fuel in the oxidation cellshall be below the
