1、Designation: D2274 14Designation: 38897Standard 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 revision
2、, 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 U.S. Department of Defense.1. Scope*1.1 This test method
3、covers the measurement of the inherentstability of middle distillate petroleum fuels under specifiedoxidizing conditions at 95 C.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 suita
4、ble 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, the precision measures may
5、not apply.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 de
6、termined 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 thememb
7、rane filter and give erroneous results.1.3 The values given in SI units are to be regarded as thestandard. The values in parentheses are for information 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
8、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 for
9、Oxidation Characteristics of InhibitedMineral 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 Middle Dist
10、illate 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 Diesel F
11、uel 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),nmaterial which is produced in the course of stressing1This test method is under the juri
12、sdiction of Committee D02 on PetroleumProducts, Liquid Fuels, and Lubricants and is the direct responsibility of Subcom-mittee D02.14 on Stability and Cleanliness of Liquid Fuels.Current edition approved Dec. 1, 2014. Published January 2015. Originallyapproved in 1964. Last previous edition approved
13、 in 2010 as D2274 10. DOI:10.1520/D2274-14.2For 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.3Available from St
14、andardization Documents Order Desk, Bldg. 4, 700 RobbinsAve., Philadelphia, PA 19111-5098. Attn: NPODS*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 States1distillate fuel und
15、er the conditions of this test and whichadheres to the glassware after fuel has been flushed from thesystem.3.1.2 filterable insolubles, nmaterial, which is producedin the course of stressing distillate fuel under the conditions ofthis test, which is capable of being removed from the fuel byfiltrati
16、on. 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 stability, nthe resistance to change whenthe fuel is exposed to air, but in the absence of otherenvironmental factors such as water
17、, or reactive metals anddirt.3.1.4 total insolubles, narithmetic sum of the adherent andfilterable insolubles.3.1.5 zero time, nthe 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 b
18、ath.4. Summary of Test Method4.1 A 350 mL volume of filtered middle distillate fuel isaged at 95 C (203 F) for 16 h while oxygen is bubbledthrough the sample at a rate of 3 L/h. After aging, the sampleis cooled to approximately room temperature before filtering toobtain the filterable insolubles qua
19、ntity. Adherent insolublesare then removed from the oxidation cell and associatedglassware with trisolvent. The trisolvent is evaporated to obtainthe quantity of adherent insolubles. The sum of the filterableand adherent insolubles, expressed as milligrams per 100 mL,is reported as total insolubles.
20、5. Significance and Use5.1 This test method provides a basis for the estimation ofthe oxidation stability of middle distillate fuels such as No. 2fuel oil.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 a
21、mount of insolubles formed in 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 43 C bottle test. However, as a result ofthe significantly elevated temp
22、erature and the pure oxygenatmosphere, the nature and amount of insolubles may deviateto a greater extent than Test Method D4625 from those formedin field storage.6. Interferences6.1 Oxidation is a major chemical process causing adherentand filterable insolubles to form. Any substance such as copper
23、or chromium that catalyzes 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 t
24、heapparatus by thorough cleaning 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 aceton
25、e, ifused in the trisolvent, 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
26、theamount of total insolubles. 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 laboratoryop
27、erations. Storage before stress, the stress period and cool-down after stressing shall be in the dark.7. ApparatusNOTE 3It is suggested that all measuring equipment be calibratedaccording to manufacturers instructions on a periodic basis to assureconsistency of results.7.1 Oxidation Cell, of borosil
28、icate glass, as shown in Fig. 1,shall 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 C 6 0.2 C (203 F 6 0.
29、4 F). It shall be fitted with asuitable stirring device to provide a uniform temperaturethroughout the bath. It shall be large enough to hold the desirednumber of oxidation cells immersed to a depth of approxi-mately 350 mm. Further, the bath construction must permitshielding the fuel samples in the
30、 oxidation cells from lightwhile they are undergoing oxidation.47.3 Flowmeters, shall have a capability of measuring3Lh6 0.3 L h of oxygen. One flowmeter shall be providedfor each oxidation cell.7.4 Filter Drying Oven, shall be capable of safely evapo-rating the solvent at 80 C 6 2 C (176 F 6 4 F) f
31、or thedrying of filters.7.5 Glassware Drying Oven, shall be capable of dryingglassware at 105 C 6 5 C (221 F 6 9 F).7.6 Filtration Assembly, see Fig. 2, shall be capable ofholding the filters described in 7.7.7.7 Filter Media5, 47 mm diameter cellulose estersurfactant-free membrane filters with a no
32、minal pore size of0.8 m.7.7.1 Single filters are to be used for prefiltration.4This apparatus is available from suppliers of specialty petroleum testingequipment.5Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D02-1012. Filters
33、may be qualifiedusing the procedure in this research report.D2274 1427.7.2 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
34、.9 Hot Plate, capable of heating a liquid in the evaporatingvessel (7.8) to 135 C (275 F).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-te
35、e on Analytical Reagents of 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 o
36、therwise indicated, referenceto water shall be understood 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
37、isdelivered through a plant 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
38、 tank ofoxygen of the specified 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.)6Reagent Chemicals, American Chemical Society Specifications, Ameri
39、canChemical Society, Washington, DC. For Suggestions on the testing of reagents notlisted by the American 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
40、), Rockville,MD.FIG. 1 Oxidation CellFIG. 2 Apparatus for Determining Filterable InsolublesD2274 1438.5 Trisolvent, a mixture of equal volumes of acetone,methanol, and toluene. See 8.1.(WarningIt is particularlyimportant that technical, commercial, practical, or industrialgrades (however they are de
41、signated by the particular manu-facturer) are not to be used, as their use may lead to apparentlyincreased levels of adherent insolubles.) (WarningFirehazard, toxic.)9. Samples and Sampling9.1 When obtaining samples for the laboratory, followPractices D4057 or D4177, or other standard practice capab
42、leof 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 nitrogen, argon, or helium andstore at a temperature no higher than 10 C (50 F) but notlower than the cloud po
43、int. (WarningPlastic containers arenot acceptable for samples 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 no
44、t 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 laboratory. Ifthe laboratory sample is stored in a tank, drum, or 19 L (5 gal)or larger can, use the pertinen
45、t procedures of Practice D4057.Thoroughly mix smaller laboratory samples by shaking,rolling, or other techniques before taking an aliquot portion bypouring, pipetting, or other means. Clean any tube, thief, pipet,beaker, or other equipment that is to contact the laboratorysample with trisolvent and
46、rinse with a portion of the sampleprior to use. Prior to mixing thoroughly and taking an aliquot,allow samples that have been stored at temperatures muchbelow 10 C (50 F) to warm to room temperature; thusallowing any separated wax to redissolve and to allow theviscosity to decrease to a point where
47、mixing is effective.10. Preparation of Apparatus10.1 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 acet
48、one to remove water.10.2 Preparation of Oxidation Cells 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, d
49、rain, thenrinse five times with tap water followed by 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) for 1 h in an oven at 105 C 6 5C(221F 6 9 F). Place the beakers in a desiccator (withoutdesiccant) and allow them to cool for 1 h. Weigh beakers to thenearest 0.1 mg.11. Procedure11.1 Preparing the SamplePlace one filter (
