™~ ~~ canalard san Grvelpel la accordance wth Internalenaly ott alereatunal Masia, (Oy Designation: 02274 - 14 Der ae gorse Je. Designation: 388/97 Standard Test Method for Cain an acemmenatons led by Ot ed etnies om sanguin eabluhed Inthe Deco om Peep fr the bres Sipe ncn Rar cst) Cone Oxidation Stability of Distillate Fuel Oll (Accelerated Method)" ‘Pas sandard fs sued une the feed de gina mln 10 th Cate of toni arern 898 epuliat (eyo azn an edu change on D2274, the number inet fllomag te deviation Indicates the year of Seu fia teison. A number the Ia ension ut reapprond wemderes indices the yeas of la reapproval A ous surnbind has been oppnvved for une by wnenctes of he US. Deparment of Defense 1.1 Tus test method covers the measurement ‘of the inherent nity of middle disullate petroleum fuels under specified wudizing conditions at 95 °C. sin: 1—Pucls used in esting the proclston measures for ths test cud were describ us pas oi, Uievel fuel, No? heating oil, and DEM, Sy Unnilsle fuel wale for diesels, baller, and gas turbines. THe pm DEM 1 0 hinget sed when referring lo fuel meeting MIL-F- 16484 Tuvencniy, ede ais called F16 ay w conforms wo NATO F16 weireinentc) While the est meihod enay be used for fuels outside the Set of Dee fuels, the precision measures may not apply. 1.2 This test method is not apphcable to fuels containing siJual oll. This test method has not been validated for testing iodiesel, such as mecting Specification Dh751 or blends of njdle dishillates and biodiesel, such as meeting Specification 7467, of both. Test Method D7462 hus been determuned 10 be nable for testing B100 and wil blends of middle distillates nd biodiesel Now 2—No. | and No 2 grates in Specifications 0346 of DITS sreily low up to 5 % biodiesel meeting Specification 04751. Samples uaining biodiesel can result i pura dissolution or compromise ofthe emirare (iter and give erroneous sesuis, 13 The values given in SI units are to be regurded as the andard. The values in parentheses are for information only. L4 This standard does not purport to address all of the ety concerns, if any, associated with its use. It is the sponsibility of the user of tis standard 10 estabiish appro- late safety and health practices and determine the applica- lity of regulatory lmitatlons prior 10 use. Thin tew mod Ls under the Jurisdiction of Commitice O62 on Peisfeuin rue UA om Stability aed Cleaslirey of Lagid Fel Cane ecru approved Dec 1, O14. Puriahed January 2018. Onginally ger-c8 w Vik. Last previous edn approved In 2UIG a» 02274 ~ 10. DOL 13260227414 2. Referenced Documents 2.1 ASTM Standards: D341 Test Method for Gum Content in Fuels by Jet Evapo- ration 10396 Specification for Fuel Oils D943 Test Method for Oxidauon Chasucterisucs of Inhibited Mineral Oils D975 Specificatuwn for Diesel Fuel Oils DJ193 Speciiication for Reagent Water Ds057 Practive for Manual Sampling of Peuoleum and Pouruleum Products 1D4J77 Practice for Automatic Sampling of Pewoleum and Petroleum Products D4625 Test Method for Middle Distillate Fuel Storage Stabiluy at 43°C (HOF) DO6751 Specification for Biodiesel Fuel Blend Stock (B100) for Middle Disullate Fuels 7462 Test Method for Oxidation Subility of Biodiesel (B100) and Blends of Brodiese) with Middle Disullate Peyoleum Fuel (Accelerated Method) 07467 Specificavon for Diesel Fucl Onl, Biodiesel Blend (B6 10 B20) 2.2 Military Specification:® ‘MIL-F- 16884 Fucl, Navy Disttlate 3. Terininology 3.1 Definitions of Terms Specific to This Standard: 3.1.1 adherent insolubles (formerly adherent gum), material which is produced in the course of stressing # Fur eclerenced ASTM wanna, sult Ue ASTM edule, www HSUR.OV, OF ‘oninct ASTM Customer Service at cerviced@astn or, For Avital Book of ASTM Standards vohame fortaion, refer othe staard's Document Summary page on {he ASTM website “Avalahe fram Standavdlration Documenis Order Desk, Bldg. 4, 200 Robbins ‘Ave. Philudelphi, PA 19111-5098, Aun NPODS. A Summary of Changes section appear al the end of this standard Pe OSTY rrmaicral 100 Br Maro” Dre, PO Bex C700, Want Caratancchan, PA 16470-2089 Unied Bites 933Ay 2274-14 apparatus by preclude the presence distillate fuel under the conditions of this test and which adheres (0 the glassware after fuel has been flushed from the system. 3.12 filterable insolubles, n—-material, which is produced sn the course of stressing distillate fuel under the conditions of this test, which is capable of being removed from the fuel by fileouon, This includes both matenal suspended in the fuel and material easily removed from the oxidation cell and oxygen delivery tube with hydrocarbon solvent. 3.1.3 Inherent stability, n—the resistance to change when the fuel is exposed 10 air, but in the absence of olhet tnvaronmental factors such as water, or reactive metals and ain 3.1.4 total insolubles, n—arithmoetic filterable insolubles. 3,15 cero time, nthe time the fst of a batch of oxidation Ns 15 placed in the heating bath. seer ecurson-Uhieis the ime akeo ashe start ofthe 16 b of residence in the beating bath. sum of the adberent and 4, Summary of Test Method 4.1 A350 mL volume of filtered middle distillate fuel is aged a1 95°C (203 °F) for 16 h whue oxygen is bubbled through the sample at a rute of 3 L/h, After aging, the sample 1s cooled (0 approximately room temperature before filtering (© ‘Obiain the filterable insolubles quantity. Adherent rasotubles fare then removed from the oxidation cell and associated slassware with tisolvent. The tisolvent 1s evaporated to obtain the quanuty of adherent insolubles. ‘The sum of the flterable and adherent insolubles, expressed as milligrams per 100 ml, 1s reported as total insolubles. 5, igalficance and Use 5.1 This test method provides a basis for the estimation of the oxidation stability of middie destillate fuels such as No. 2 fuel oil. 5.2 The test method may not provide a prediction of the ‘quantity of insolubles that will form in field storage over any given period of ume. The amount of insolubles formed in such field storage 1s subyect 10 the specific condivions which are too variable for this test method to predict accurately. 5.3 Test Method D2274 yields results more eapidly than Test Method 14625, the 43°C bottle test. However, as a resull of the significuntly elevated temperature and the pure oxygen almoxphere, the nature and amount of insolubles may deviate to greaier eatent than Test Method D4625 from those formed in field storage. 6, Interferences 6.1 Onidauon is w mayor chemical process causing adherent and filterable insolubles to form, Any substunce such as copper cof chromium thut catalyzes oxidation eeacuons will cause gsealet quunlittes of inselubles tw form, Since the 9 . ted im this tes can ao be used tn Fea Methnd Us where coils of copper aad steel wre used, i iy important that any residues that could contain these metals be elininated from the 94 thorough cleaning prior to use, ¢. ‘of chromtum tons, as wer Se laboratory personnel {ror potential Rurm. chrom, 57% nat be used for cleaning glassware 19 the Prange method. 6.2 Iehas been found the unsolvent, sents greater level of odherent insstubles ub This, therefore, cnuicel thal only reagent tor b, 36, materials be used in preparing the UMSO}ER meggy | PS traviolet lgbt exposure has Deen Found ts joe, ansunt of tou! insolubles. Therefore. the fay fiery Sun be shielded from direct exposure 19 alia, Gunlight or fluorescent). Conduct all sampling, ee romans and weighing away from det sunh gy cS aorevey area as would be cOMpauble With over is * Storage before SUESS, dhe steSs pend ye ing shall be in the dark. : ae that commercial gradey of, can have impuntes wiy.y 6% « ‘operations. down after stress 7, Apparatus Noo dale « suggested that all measuring euipmen re ace neler WSUS OF 4 pe Nee consistency of results. 7.4 Oxidation Cell, of borosilicate £1as6, a5 own shall consist of a test (Wbe, condenser, aed oryecn ie ube, This cell is identical to that used in Test Mwy 0. 7.2 Heating Bath, with a thermostaveally conaula i medium, shall be capable of maintaining the buh tence: » at 95°C = 0.2 °C (203 SF = 0.4 °F). It shall be Fuad 62, Svitable surring device to provide a uniform wagers throughout the bath. It shall be lante enough te hold thes = number of oxidsuon cells immersed © u depih of gor mately 350 min, Further, the bath construction mist shielding the fuel samples in the oxidation cells while they are undergoing ovdauon.* - 7.3 Flowmeters, shall have a capability of ace JLAME O.3LM of orygen. One Howmeter shall Wen, for each oxidation cell. re te i 74 Filter Drying Oven, shall be capable of sift se ruling the solvent at 80°C = 2°C (176°P 4 fia, drying of filters. 15 Glassware Drying Oven, shall bo capac of 35, glassware at 105°C = S°C 221 °F 2 9"P. 1.6 Filtration Assembly, see Fig 2, shall & ae | holding the titers described 19 7. 7.7 Filter Media’, 47 wm diameter vetlvlos > * surfactant-free membrane filters with nonund AN & OX im, TIL Single filters are to be UNAS for prvtlisalas. hwy te ata Nave fees ed a ASTM Encraecal Wea a stuamed hy rrywesing Roscaith Mepeat KL DEOL? filen 3% Laing the purser an tha mea epee srs & anaale teen spies a apcusy FA |ij rates are FIG. 1 Oxidation Cell | 0.2 Apporatus for Determining Fiterabie Insoluble ) 172A matched weight pair of filters or alternatively, a | eed contol and sample, Giters shall be used for | ktermnation of filterable insolubles 14 Evaporating Vessel, borosilicate glass beuker, 200 mL. | Sracily, all style. 19 Hor Plate, capable of heating a liquid in the evaporating 1, "#1 (1.8) t0 135 C (275 °R). ‘ Weagents and Materials dl Pini of Reagents—Reayont grade chemicals shall be ‘all wsts, Untess otherwise indicated, it is intended that os, all reagents shall conform to the specifications of the Commit tee on Analytical Reagents of the American Chemical Society, where such specifications are available.° Other grades may be used, provided it is first ascertained that the reagent 15 of sufficiently high purity to permit its use without lessening the accuracy of the determination. 82 Purity of Water—Unless otherwise indicated, reference to water shall be understood to mean reagent water as defined by Type Ill of Speciticauion D193. 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 is Welivered through a plant system of piping, a filter shall be provided adjacent (o the constant temperature bath to prevent the introduction of line debris or moisture unto the oxidauon cells; a pressure regulator adequate to maintain a constant flow fof gas through the apparatus shall also be used. A wank of ‘oxygen of the specified purity can be used provided it is equipped with a two-stage pressure regulator. (Warning-— ‘Oxygen vigorously accelerates combustion. Do not use equip- ment having exposed surfaces containing oil or grease.) “Reagent Chemievls, American Chemical Soclesy Spectirations, Amencan Chemical Society, Washington, OC. For Suggestions on the testing of reagents Ook Tied by the Amencan Chemical Society, see Annual Standards for Luboratory Chemicals, BDH Lit, Poole, Dorset, UX. and the ‘Stes Phurmaicwpelt fond Nutlonal Fornulon, WS, Pharmacopstal Coovention, tne. USPC), Rockville, MD.Af 2274-14 8.5 Trisohent, a mixture of equal volumes of acetone, ‘methanel, and toluene. See Rt. (Waralag—lt is parucular!y tmporant thi cca, commer pasta, of esa g wever they are desigmated by the particular manu Facturer) are not to be used, as thetr use may lead 10 apparently increased levels of adherent insolubles,) (Warnlng—Fue havand, toe.) 9, Samples and Sampling 9.1 When obiaining samples for the laboratory, follow Practices D4057 or D177, or other standard pracuce capable of providing representative samples. 12 Analyze fuel samples as soon as pos When a fuel cannot be tested within one day. anert gas such as oxygen-free nitrogen, argon, or belium and store at a temperature no higher than 10°C (50°F) but not lower than the cloud point, (Warning —Plastic containers art not acceptable for samples due to the potental for leaching of plasticwers. Samples should be taken preferably in metal cans provigusly cleaned according to Practice D4057. Borosilicate lass containers can be used if they are wrapped or boxed 10 ‘exclude hight, Do not use soft (soda) glass containers.) 9.3 Test Samples—Reduction of the tuboratory sample 1¢ test sample size (about 400 mL for each determunation) depends upon the size of saruple received By the laboratory. 1f the laboratory sample is stored in a tank, drum, of 19 L (5 zal) or larger can, use the pertineot procedures of Pracuice D4(5?. Thoroughly mix smaller laboratory samples by shaking. rolling, or other techniques before taking an aliquot portion by pounng, pipetting, or other means. Clean any tube, thief, pipet, beaker, of other equipment that is 10 contact the laboratory sample with insolvent and rinse with a poruon of the sample prior to use. Prior to mining thoroughly and aking an aliquot, Slow samples that have been stored at temperatures much below 10°C (50°F) to warm to room temperature, thus allowing any separated wax (0 redissolve ani sible after receipt. blanket it with an 1d to allow the viscosity to decrease t0 @ point where miring 1s effecove, 10, Preparation of Apparatus 10.1 Preparation of Glassware Other Than Oxidation Celts-Ranse all glassware thoroughly with trisolvent followed by water, Uien wah with a mutdly alkaline or neutral laboratory detergent. Rinse three umes with deionized or distilled wuter followed by acetone 10 remove water 10.2 Prepuration of Oxidation Cells and Accessories —Atier completion of 10.1, fill oxidation cells with laboratory detergent in water, Place the oxygen dehvery tube in the oudation cell, place the condenser over the oxygen delivery tube und allow 10 soak at Ieust two hours, Wash, drain, theo rinse five times with Lap wuter followed by three cunses with diswlled of detonized water meeuing Specification D1 198 Type TIT requirements. Ronse with acetone, drun und allow the oxidation cell and oxygen delivery tube to Ury 10.3 Preparation of Evoporating Beukers—Dry tbe 200 mL. cleaned beakers (10.1) for J h in an oven at 1O8*C * 5°C Q21°F = 9°F), Place the beakers in a desiccator (without desiccant) and allow them to cool for I-b. Weigh beakers to the nearest 0.1 mg. 11, Procedure 11.5 Preparing the Sample—Place one fier 77) on the fier support and clamp the fey SOS Jappont a> shown in Fis. 2 AMpIY sucuon eee BO KPa(1? ps0). Pour 400 mL of the fuel throug re Top imo a.clean (10 1 500 ml glass tause geo preparation for each sample 10 be run After an Complete, discund We Hier mecha. Never ase ine Ma. fara socond increment of fucl, because any mus an & fon the filters By @ previous increment of fuel ae AS | greater removal oF solids from the next iocreneat 112 Assembling the Oxidation Apparatus 11.21 Place # clean osygen delivery ovation sell (Section 10) and pour 380 ml Filtered fuel into the cell. As soon thereafier as poss: ovcase more than 1 h after measuring the fuel, moa’? Tegvell in the 95 °C (203 °F) heating bath, Dunrg ek period store the cell it the dark The level ot ha | PRidauon cell shall be below the level of the haul mee the heating bath, Bea, ! 11.2.2 Place a condenser over the Ou) 0 elnan nag || oxidation cell, connect the condenser 10 the coving 3 Connect the oxygen delivery tube to the 0.) gen suxpiy Mad conn et adjust Oe oxygen Dow UR eee | Make sure samples are protected from bight. When te a: kar’ srtest cells is less than the capacity ofthe heaung hak = 5 empty positions with dummy ovation cells gum 360 mal of a stuble petroleum liquid wath phyccd prpeg | ‘imilar to these of the fuel being tested. 2 11.2.3 Record the time the first oxdaticn cel i tax the bath as zero ume. st New 4-Nituary Specifcstion NOL-FGEES perms oe es, moaned Tent Method D2275 procedure in Shah the une Grey | ov is extended to 40 b, Perils ther Gan 16 b my Lore st webuthor m oiher specifications. Howeses, the presiven angns Fea Mod 02274 apply only 10 tbe 16D pen! nie age | L1.3 Cooling the Sample: TRL 16 b= 0.25 h from zero time, remove de sere | from wie heating bath in the same sequence a they wer 7a therein. Cover the opening of each cell with 2 per: alunvnum foil of plasuc 10 prevent entrance of da 2x1 ‘moisture, Record the Ume the first cell 15 removed. 11.32 Place in a dark, ventilated site at conn tegen | which shail be above the cloud pornt of the fuel, nal = fatuins room temperature but for 0 tonger thao 48 beet & ee, M4 Determining Filteruble Insolubles. ILA Assemble the filter apparatus as Musial using one set of matched pair filters (or preweighedso=\ & sample filters). Apply vacuum as nacessazy to fier af in-an adequate ume (approximately 80 KPa U2 pL NE > cooled suinple Uveugh the filter. Filter alt fee’ Bara’ > ps oe filters before pouring isooctane rinses into the Nem S10 the filtration of the sample cannot he comyies! as a result of severo filter plugging, filter he reusning Me Separate vet of iter 114.2 On completion of Gliration, oxidation velt with three separate $0 mL eae at mpl roe > Sink! 936acces bore oF vessel capable of directing sSegiane. Pas all sings Uoogh the fer sqynnon and ising of the ovulation apparats hn 2 Mjawn the sides of the tunnel with an S mb af Govctane directed as a fine gonctane should be directed in a manner would push particles 10 Ue middle of the re 1s complete disconnect the op pan of eg wash Jown the rim of th filter media se OY rane filter assembly with @ forther 50 mL spasm ee Tiong, Be cenain the area of the fliers au or intion funnel 1s adequately rinsed to « * oe dof residual distillate fuel. Disconunue wsonnect the filter assembly, Discard the a oe an unl ot penne filters at 80 °C (176 °F) fer 30 min, cool vn, and weigh the upper (sample) and lower eparately 0 the nearest 0.1 mg. ing Adherent Insolubles: the tina) lasing of the oxidation cel) and the fy mide wilh isooctane, dissolve adherent in- ipe surfaces of these pieces usiog three equal “as 00 oy le ga set ee ine TS = Sail. of tnsolvent a eaermine ihe oxsdavon celt and the oxygen delivery 52 Eace of sin oF color indicating incomplete at Trsuvh stain of color is noted, nnse with a fourth 2a me of talent. 38) enone te solvent from the rinsings in either of ans 1 Collect the rinsings in a tared 200 mL tat beaker. poe be beaker and contents on a hot plate and evaporate the vat at 135°C under a hood. When all the solvent has, pawasd place the tured beaker in a desiccator (without ran oe similar container (© cool for 1h. The container el rowel the beaker from airborne dusudin. Afwer 1 hy seg de beaker to the nearest O.f mg, ViS32 Optonally, collect the naasings in one or (wo wel beakers of the type specified for Test Method Dist i eaporue the tsolvent at 160°C by the Test Method “PH att meted, 154 Kun on adherent insolubles blank by evaporating @ | care of tivilsent equal to that used an the test and correct ‘12 prescove of impunbes in the solvent. 1 Cakulation NU Calculate the filterabte amsolubles mass (A) va milli- Fee pa 100 mL. Subtract the muss of the blunk (bottom) 22 ¥,.1n imllygans, feorn Haut of the sample (op) Ntler Ws, *saligrans, (Lay and divide by 3.8 to reduce the nesul to 120 riL as, wy Wy aw 122 Cueulae the uthezemt insolubles mass (H) an mult Fe~pet OX mL. Suburact the fare mass of the Blank (W,) and, PCAN beakers from these final masses (WY). (Wy) vat time Ay 02274 -14 TABLE 1 Calculated Precision Data for Severe! Levels of Totst ~~. tnvolubies” Toul now en may Wore Racers, Recnetey Ta naan, 8 030 ve os. oat os 0 coe +8 1 oe ww? 20 be rs 28 ow 1s 3 on 1 Tin tee JSANe a ey Waar aN 8 OO GT OG Tespectively. Subtract the mass of the blank from the corrected, mass of the adherem msolubles (11.5) and divide by 3.5. (eB a= Oo) be yoo @ ‘(are mass of the blank beaker, mg, tare mass of the saniple beaker, Mg. final mass of the blank beaker, emg, and final mass of the sample beaker, tg 12.3 Calculate the total insolubles mass (CV an millygrarns per 100 mL as the sum of the flterable wsolubles (AD and re adherent insolubles (B). CnA-8 o where: C= want insctubles, my/100 mL, A. = fillerable insolubles, my/l00 mL, an B = adherent insolubles, mg/100 mL Nun 6—Sonne specelcations may MAGUIRE Felts 19 SK uMEs wf tnt sae than as mg/IOD mL Tn ach casen the 9 Auer i mY ML ca De ‘converted to Stunts hy multiplying) 8 13, Report VBL Report tou insotubles (Cn my/tOO mL, wo the reurest 0.1 mg/100 mL. 13.2 A repo af filteruble smotubles (A), and the aitherent Insolubles (8) os opuonal Repos units a milhigrams pvr 400 mL. 14, Precision aad Bins” JAA Prevision~The prvisioa (see Table 1) of dus test ethos! as determined by statistical EvaTMnatoN ob AnierlANs -ravory FESULS tS as Follows IFT Repeotubility—The dutfereace triwcen Iwo test results, obtained by the same Operator wih the ume alas unde? vonstant operating conditions on identical text material would in the Tong run. am the normal and coatevt oper ot the test metheal, exceed the following Values vnty an ane Case 1a twenty, us suing teva Mol a ASTM erate nal Meabyacen ad ty Re aNernd ny reosing Mescarh Ropes RM DED FoNS hy o2274 -14 14,12 Reproducibitin—The difference between two single ‘and independent results obtained by different operators work- ing in different laboraiones on identical test material would, in th eee, Statement on bis 1s being mode, . the long nun, 19 the normal and corest operation of the fest me mete we method, excel the flowing vals only in one cave a9 16. Kernord ” 15.1 dese fel Glerableisolbies; mide oo VearaaNeTmgTITAD) «ay ouiauen sui stay SUMMARY OF CHANGES 142 Biar—Sinee there 18 no ace suitable for detrmising the Nas tea Subcommittee DO2.14 has entfed the location of selected changes to this standard since the last i, (2274-10) tbat may impact the use of this standard, (Approved Dec. 1, 2014.) Me (1) Numerous minor changes io Scope subsection | 3, Termi nology subsections 3.1.3 and 3.1.4, Significance and: Use subsecuon $.1, Apparatus Note 3 and subsections 7.4 and 7.6, ‘Samples und Sampling subsection 9.3, Preparation of Appari- ASTM iaravora! tas ne poston sina Pardons Users of oe sacar 8 Srintnngomant ol sch i.e aro Pa Ont sp0AEDIy tus subsection 10.3, and Procedure subsections INA, 14S, and U15.3.1 t0 improve grammar, conformance with ASTM Form and Style. raapectog te vataty of any pate ooh esserad in connacton wi ay van marcaned eorntyadesod Pat cetemiraion ol he va°aty OF PY RCA AtAN os, re hak Tha arcadia syec to revon at any Se byt resporabie letra! commen and mus be evant ext hr ear ard Anot rows, 408 re sn be eadrtea fo ASTM iat ore: Ma BQ Pesoars io terra Comte WP OU Hy ee or aunninin, Your comments are neted otha To rans0on O18 NE 071 80SAra! eas Your conenens wl receve c470Ki corso" aa medng he "Span jos fel thal your cOmerens have NO TONBG MT BAY yo eNO ‘Trace your awa Arann fo te ASTM Commo on Stancarae of te adsrens shown balou ‘Tne slanted i cooyngbied by ASTM Interatona 100 Bar Ho" ried Siaras India! reps singe oF mute opie} of us ame er er erdas2-9588 prove, 610-800-9585 (fs), or servceeanmion (ema, OF rows (he ASTM wedaiy ee ostm om) Pereasen rps to protoeaoy the sarda’d may 0 yor Onve, PO Box C700, Was Consroroctan, PA 15425-2959, ‘andard may be ob'aiied By COMaCt”g ASTM A! Pp adv 20 be s#ev'es rom te Copyran Cearance Caner 222 ‘Ronuang bie, Dances. MA 1829, Te! (878) 64-2600. Paps CORITON COM Hay stay, « t | \ ‘ \ \ { 1 : i | | ' \ \ \ \ | {