1、Designation: D2274 10Designation: 388/97Standard Test Method forOxidation Stability of Distillate Fuel Oil (AcceleratedMethod)1This standard is issued under the fixed designation D2274; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revisio
2、n, the 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.This standard has been approved for use by agencies of the Department of Defense.1. Scope*1.1 This test method cove
3、rs 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 Navy distillate fuel suitable f
4、or 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, the precision measures may not a
5、pply.1.2 This test method is not applicable to fuels containingresidual oil. This test method has not been validated for testingbiodiesel, such as meeting Specification D6751 or blends ofmiddle distillates and biodiesel, such as meeting SpecificationD7467, or both. Test Method D7462 has been determi
6、ned to besuitable for testing B100 and all blends of middle distillatesand biodiesel.NOTE 2No. 1 and No. 2 grades in Specifications D396 or D975currently allow up to 5 % biodiesel meeting Specification D6751. Samplescontaining biodiesel can result in partial dissolution or compromise of themembrane
7、filter and give erroneous results.1.3 The values given in acceptable SI units are to beregarded as the standard. The values in parentheses are forinformation 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
8、user 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:2D381 Test Method for Gum Content in Fuels by Jet Evapo-rationD396 Specification for Fuel OilsD943 Test Method
9、 for Oxidation Characteristics of Inhib-ited Mineral OilsD975 Specification for Diesel Fuel OilsD1193 Specification for Reagent WaterD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD4625 Test Method for Midd
10、le Distillate Fuel StorageStability at 43C (110F)D6751 Specification for Biodiesel Fuel Blend Stock (B100)for Middle Distillate FuelsD7462 Test Method for Oxidation Stability of Biodiesel(B100) and Blends of Biodiesel with Middle DistillatePetroleum Fuel (Accelerated Method)D7467 Specification for D
11、iesel Fuel Oil, Biodiesel Blend(B6 to B20)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)material which is produced in the course of stressing distillatefuel under the cond
12、itions of this test and which adheres to theglassware after fuel has been flushed from the system.1This 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.Curre
13、nt edition approved Aug. 1, 2010. Published September 2010. Originallyapproved in 1964. Last previous edition approved in 2008 as D227403a(2008).DOI: 10.1520/D2274-10.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual
14、Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from Standardization Documents Order Desk, Bldg. 4, 700 RobbinsAve., Philadelphia, PA 19111-5098. Attn: NPODS1*A Summary of Changes section appears at the end of this standard.Copyrig
15、ht ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3.1.2 filterable insolublesmaterial, which is produced inthe course of stressing distillate fuel under the conditions ofthis test, which is capable of being removed from the fuel byfiltration.
16、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 absence of other environmentalfactors such as water, or reactive metal
17、lic 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 start of the16 h of residence in the heating bath.4. Summary of Test M
18、ethod4.1 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 filtering to obtainthe filterable insolubles quantity. Adherent insolubles
19、 are thenremoved 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
20、 This test method 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 i
21、n suchfield storage is subject to the specific conditions which are toovariable for this test method to predict accurately.5.3 Test Method D2274 yields results more rapidly than TestMethod D4625, the 43C bottle test. However, as a result of thesignificantly elevated temperature and the pure oxygen a
22、tmo-sphere, the nature and amount of insolubles may deviate to agreater extent than Test Method D4625 from those formed infield storage.6. Interferences6.1 Oxidation is a major chemical process causing adherentand filterable insolubles to form. Any substance such as copperor chromium that catalyzes
23、oxidation reactions will causegreater quantities of insolubles to form. Since the apparatusused in this test can also be used in Test Method D943, wherecoils of copper and steel are used, it is important that anyresidues that could contain these metals be eliminated from theapparatus by thorough cle
24、aning prior to 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
25、, can have impurities 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 insolubl
26、es. Therefore, 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 st
27、ress, the stress period and cool-down after stressing shall be in the dark.7. ApparatusNOTE 3It 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
28、 consist of a test tube, condenser, and oxygen deliverytube. This cell is identical to that used in Test Method D943.7.2 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 with a suitablesti
29、rring 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 while they areund
30、ergoing 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.7.5 Glassware Dryin
31、g 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 Single filters are to b
32、e 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 heating a liquid in
33、 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 that4This apparatus is available from suppliers of specialty petroleum testingequipment.5Supporting data have been
34、filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D02-1012. Filters may be qualifiedusing the procedure in this research report.D2274 102all reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Socie
35、ty,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, referenceto water shall be understo
36、od to mean reagent water as definedby Type III of Specification D1193.8.3 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 system of piping, a filter
37、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 specified purity can be used prov
38、ided 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.(WarningIt is particularlyimportant t
39、hat 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 Sampling9.1 When obtaining samples for
40、the laboratory, followPractices D4057 or D4177, or other standard practice capableof providing representative samples.6Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For Suggestions on the testing of reagents notlisted by the American Chemical
41、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. 1 Oxidation CellFIG. 2 Apparatus for Determining Filterable InsolublesD2274 1039.2 Analyze fue
42、l 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 nitrogen, argon, or helium andstore at a temperature no higher than 10C (50F) but not lowerthan the cloud point. (WarningPlastic containers are notacceptable for s
43、amples due to the potential for leaching ofplasticizers. Samples should be taken preferably in metal canspreviously cleaned according to Practice D4057. Borosilicateglass containers can be used if they are wrapped or boxed toexclude light. Do not use soft (soda) glass containers.)9.3 Test SamplesRed
44、uction of the laboratory sample totest sample size (about 400 mL for each determination)depends upon the size of sample received by the laboratory. Ifthe laboratory sample is stored in a tank, drum, or 19-L (5-gal)or larger can, use the pertinent procedures of Practice D4057.Thoroughly mix smaller l
45、aboratory samples by shaking, roll-ing, or other techniques before taking an aliquot portion bypouring, pipetting, or other means. Clean any tube, thief, pipet,beaker, or other substance that is to contact the laboratorysample with trisolvent and rinse with a portion of the sampleprior to use. Prior
46、 to 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
47、Preparation 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 Cel
48、ls 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
49、 three rinses withdistilled or deionized water meeting Specification D1193 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 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 thesu
