1、Designation: D5304 15Standard Test Method forAssessing Middle Distillate Fuel Storage Stability byOxygen Overpressure1This standard is issued under the fixed designation D5304; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the ye
2、ar 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 covers a
3、 procedure for assessing thepotential storage stability of middle distillate fuels such asGrade No. 1D and Grade No. 2D diesel fuels, in accordancewith Specification D975.1.2 This test method is applicable to either freshly refinedfuels or fuels already in storage.1.3 This test method is suitable fo
4、r fuels containing stabi-lizer additives as well as fuels containing no such additives.However, fuels additized with dispersant additives, includingdispersant-containing stability additives, may be ranked inac-curately using this test method compared to fuels that are notadditized with dispersant ad
5、ditives.1.4 Appendix X1 provides information on other suggestedtest times and temperatures for which this test method may beused.1.5 The values stated in SI units are to be regarded asstandard. The values given in parentheses are for informationonly.1.6 This standard does not purport to address all
6、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. For specificwarning statements, see 4.1, 6.2, 6.3, and 7.4.2. Re
7、ferenced Documents2.1 ASTM Standards:2D525 Test Method for Oxidation Stability of Gasoline (In-duction Period Method)D975 Specification for Diesel Fuel OilsD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD43
8、06 Practice for Aviation Fuel Sample Containers forTests Affected by Trace ContaminationE1 Specification for ASTM Liquid-in-Glass Thermometers3. Terminology3.1 Definitions:3.1.1 membrane filter, na porous article of closely con-trolled pore size through which a liquid is passed to separatematter in
9、suspension.3.2 Definitions of Terms Specific to This Standard:3.2.1 oxygen overpressure, npartial pressures of oxygenhigher than that of air at atmospheric pressure.3.2.2 potential storage stability, nthe tendency of a fuel toform insolubles under the conditions of this test method.3.2.3 reactor, na
10、ny vessel capable of sustaining pressuresand temperatures above ambient, sometimes designated pres-sure vessel.3.2.4 weighing assembly, na set of two filters and twoaluminum weighing dishes used to determine total insolublesfor each sample or blank.4. Summary of Test Method4.1 A 100 mL aliquot of fi
11、ltered fuel is placed in aborosilicate glass container. The container is placed in apressure vessel which has been preheated to 90 C. Thepressure vessel is pressurized with oxygen to 800 kPa (abso-lute) (100 psig) for the duration of the test. The pressure vesselis placed in a forced air oven at 90
12、C for 16 h. (WarningObserve all normal precautions while using oxygen underpressure and at high temperatures in the presence of combus-tible liquids. Appropriate shielding should be used for anycontainers under pressure. Pressurize and depressurize thecontainers slowly using appropriate personnel sh
13、ielding. Neverattempt to open the pressure vessel while it is pressurized. Allfuel and solvent handling should be done in an appropriate1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee
14、 D02.14 on Stability and Cleanliness of Liquid Fuels.Current edition approved April 1, 2015. Published May 2015. Originallyapproved in 1992. Last previous edition approved in 2011 as D5304 11. DOI:10.1520/D5304-15.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM C
15、ustomer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocke
16、n, PA 19428-2959. United States1fume hood only.) After aging and cooling, the total amount offuel insoluble products is determined gravimetrically andcorrected according to blank determinations.5. Significance and Use5.1 The results of this test method are useful in ranking aspecific fuel sample aga
17、inst other specific fuel samples orstandards when tested under identical conditions. Specific fuelsamples containing dispersant additives, such as dispersant-containing stability additives, have shown inaccurate rankingagainst fuel samples that do not contain dispersant additivesusing this test meth
18、od.3This test method is not meant to relatea specific fuel to specific field handling and storage conditions.The formation of insolubles is affected by the material presentin the storage container and by the ambient conditions. Sincethis test method is conducted in glass under standardizedconditions
19、, the results from different fuels can be compared ona common basis.6. Apparatus6.1 Sample or Blank Container, a brown borosilicate glassbottle capable of holding 100 mL of sample but with totalvolume less than 200 mL, or a Test Method D525 glass insert.A top closure of aluminum foil, perforated wit
20、h small holes forbreathing, will be required if there is more than one sample perpressure vessel.6.2 Pressure Vessel(s) (Reactor(s), designed for safe oper-ating pressures of 800 kPa (100 psig) in oxygen service(WarningSee 4.1.) equipped with a pressure gauge.(WarningThe pressure for the procedure i
21、n this test methodis 800 kPa (absolute) (100 psig). Many pressure gauges arecalibrated in kPa (gauge). For such gauges, the test pressurewould be 700 kPa (gauge). Maximum gauge gradations shouldbe 20 kPa (5 psig). The gauge should be calibrated againststandards, and capable of holding the four sampl
22、e containers.Pressure vessels having internal volumes from 250 mL to8000 mL have been used and found to be suitable. If 250 mLvessels such as Test Method D525 oxidation vessels are used,four will be required. The larger volume pressure vessels canaccommodate multiple sample or blank containers). The
23、 pres-sure vessel(s) (reactor(s) must be obtained only from com-mercial sources.6.3 Heater, capable of maintaining the test temperature at90 C 6 1 C for the duration of the test. Ensure heatertemperature uniformity. Heater shall be capable of holding thepressure vessel(s) (reactor(s) described in 6.
24、2. Static (non-forced air) ovens and unstirred liquid medium baths, such asthe Test Method D525 water bath, are unsuitable. Use of theseheaters will give erroneous results due to nonuniformity oftemperature.) The reactor should be placed in an oven so thatthe entire reactor is uniformly receiving he
25、at. (WarningUseof an explosion-proof oven is required.)6.4 Drying Oven, forced air operated at 110 C 6 5 C.Static ovens or vacuum ovens are not suitable.6.5 Water Aspirator or Vacuum Pump, as a source ofvacuum.6.6 Aluminum Dish (disposable), capable of holding 47 mmdiameter filters and 30 mL of adhe
26、rent insolubles solvent.6.7 Analytical Balance, capable of weighing to the nearest0.1 mg.6.8 Filtration SystemArrange the following componentsas shown in Fig. 1.3Williams, S., “Engineering Investigation of 2004/05 East Coast F-76 RapidFuel Degradation,” NAVAIRSYSCOM REPORT 4451/06-006, August 14, 20
27、06.FIG. 1 Schematic of Filtration SystemD5304 1526.8.1 Funnel and Funnel Base, with filter support for a47 mm diameter membrane and a locking ring or spring actionclip.6.8.2 Ground/Bond Wire, 0.912 mm to 2.59 mm (No. 10through No. 19) bare-stranded, flexible, stainless steel, orcopper installed in t
28、he flasks and grounded as shown in Fig. 1.6.8.3 Receiving Flask, 1.5 L or larger borosilicate glassvacuum filter flask, which the filtration apparatus fits into,equipped with a sidearm to connect to the safety flask.6.8.4 Safety Flask, 1.5 L or larger borosilicate glass vacuumfilter flask equipped w
29、ith a sidearm to connect the vacuumsystem. A fuel and solvent resistant rubber hose through whichthe grounding wire passes shall connect the sidearm of thereceiving flask to the tube passing through the rubber stopperin the top of the safety flask.6.9 Hot Plate, capable of operating at low heat so t
30、hat10 mL of toluene placed in the aluminum dish described in 6.6will require 10 min to 25 min to evaporate.6.10 Thermometer, conforming to the requirements pre-scribed in Specification E1. Temperature measuring devicessuch as ASTM 61C (IP No. 63C), liquid-in-glassthermometers, thermocouples, or plat
31、inum resistance ther-mometers that provide equivalent or better accuracy andprecision may be used.6.11 Forceps, approximately 12 cm long, flat-bladed, withnon-serrated, non-pointed tips.7. Reagents and Materials7.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise
32、 indicated, it is intended thatall reagents conform to the specifications of the Committee onAnalytical Reagents of the American 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
33、 its use without lessening the accuracy orprecision of the determination.7.2 Nylon Membrane Filters, plain, 47 mm diameter, poresize 0.8 m.7.3 Hydrocarbon SolventHexanes, heptane, isooctane, orpetroleum ether with residue upon evaporation of less than0.001 % and boiling range between 35 C and 100 C
34、aresatisfactory. Filter before use with the filter specified in 7.2.7.4 OxygenUse 99.5 % minimum oxygen from cylinderswith two stage regulators capable of delivering up to 1600 kPa(200 psig). The secondary regulator should be calibratedagainst standards to deliver 800 kPa 6 10 kPa (100 psig 61 psig)
35、. (WarningOxygen at elevated temperature and pres-sure is capable of causing explosion or fire.)7.5 Adherent Insolubles Solvent (TAM)An equal volumemixture of toluene, acetone, and methanol (TAM). Filter beforeuse with the filter specified in 7.2.8. Sampling8.1 Field SamplingField sampling should be
36、 in accor-dance with Practices D4057 or D4177. Bulk fuel to be sampledmust be above its cloud point and thoroughly mixed prior toaliquot sampling. For field sampling and shipping, use onlyepoxy-lined steel cans that have been cleaned according toPractice D4306.8.2 Laboratory SubsamplingFuel to be sa
37、mpled must beabove its cloud point and thoroughly mixed prior to aliquotsampling. Use clean amber or clean borosilicate glass contain-ers for laboratory handling. Fuel in clear bottles must beprotected from light, for example, by wrapping in aluminumfoil.9. Preparation of Apparatus9.1 Rinse the samp
38、le containers thoroughly with the TAMsolvent followed by water. Then wash with a mildly alkaline orneutral pH laboratory detergent. Rinse with deionized ordistilled water. Let bottles stand overnight with distilled waterin them. Dry in a drying oven at 105 C to 115 C. Ensure thesample bottles are cl
39、eaned thoroughly. Leave no soap residueon the inside of the bottles (Note 1).NOTE 1Even a slight soap residue left on the walls of the bottle couldalter sediment results.9.2 Soak the aluminum weighing dishes in fresh, cleanTAM solvent for several minutes followed by drying in adrying oven at 105 C t
40、o 115 C. Even new aluminum dishesmust be cleaned with TAM solvent and dried before the initialweighing. Two hours after removal from the oven, firmly nestone dish inside of another for each sample replicate and foreach blank replicate to be run. This is both the adherentinsolubles evaporation assemb
41、ly and, in combination with twounweighed nylon membrane filters, the weighing assembly foreach test sample or blank.9.3 Using forceps, place two dry filters in the aluminumweighing dish assembly from 9.2 and weigh the entire assem-bly of two filters and two aluminum dishes to the nearest 0.1mg. A se
42、parate two filter plus two weighing dish assembly (theso-called weighing assembly) is required for each sample andblank replicate. Weigh the filter and weighing dish assemblythree times about one-half hour apart and take the averagereading. This allows for changes in weight due to temperatureand hum
43、idity.9.4 Place the pressure vessel(s) specified in 6.2 in a heaterspecified in 6.3 to preheat to test temperature.10. Procedure10.1 Place two unweighed nylon membrane filters in a filterfunnel. Prefilter, under vacuum (see 6.5), 220 mL of fuel to betested. Transfer 100 mL of the filtered fuel to ea
44、ch of two glasssample containers (see 6.1). Place these sample containers plustwo blank sample containers in the pre-heated pressure ves-sel(s) (see 9.4). If more than one fuel is to be tested4Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For
45、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), Rockville,MD.D5304 153simultaneously,
46、additional glass sample containers are re-quired. However, only a single pair of blank containers isrequired. Close the pressure vessel(s) after inspecting thevessel seals and replacing if necessary.10.2 Set the oxygen cylinder secondary regulator to deliver800 kPa (absolute) (100 psig). Connect the
47、 pressure vessel toan oxygen cylinder via the preset regulator and pressurizeslowly to about 800 kPa (100 psig). (WarningSee 4.1.)Release the pressure slowly, repeat the pressurization andrelease the pressure slowly. The third and final time, pressurizeto 800 kPa 6 10 kPa (100 psig 6 1 psig) as pres
48、et on thesecondary regulator. (WarningSee 6.2.)10.3 Close the pressure vessel isolation valve and maintaintemperature at 90 C 6 1 C for 16 h 6 15 min using thethermometer specified in 6.10.10.4 At the end of the aging period, measure and record thepressure. The test is invalid if the pressure has dr
49、opped morethan 20 kPa (absolute) (2 psig) and must be repeated afterreplacing the pressure vessel seals. Slowly release the pressureto atmospheric, then open the reactor.10.5 Remove the sample containers from the pressure ves-sel(s) and allow the containers to cool slowly to ambient (25 C6 5 C) in the dark for a minimum of 1 h. Do not expose thesamples to light prior to filtration.10.6 Place the two filters from a preweighed weighingassembly from 9.3 in a filter assembly and apply suction.Completely filter the contents of a sample container
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