1、Designation: D 5304 06An American National StandardStandard Test Method forAssessing Middle Distillate Fuel Storage Stability byOxygen Overpressure1This standard is issued under the fixed designation D 5304; the number immediately following the designation indicates the year oforiginal adoption or,
2、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. Scope*1.
3、1 This test method covers a procedure for assessing thepotential storage stability of middle distillate fuels such asGrade No. 1D and Grade No. 2D diesel fuels, in accordancewith Specification D 975.1.2 This test method is applicable to either freshly refinedfuels or fuels already in storage.1.3 Thi
4、s test method is suitable for fuels containing stabi-lizer additives as well as fuels containing no such additives.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 as thestand
5、ard. The values given in parentheses are for informationonly.1.6 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-
6、bility of regulatory limitations prior to use. For specificwarning statements, see 4.1, 6.2, 6.3, 7.4, 10.1, and 10.2.2. Referenced Documents2.1 ASTM Standards:2D 525 Test Method for Oxidation Stability of Gasoline(Induction Period Method)D 975 Specification for Diesel Fuel OilsD 4057 Practice for M
7、anual Sampling of Petroleum andPetroleum ProductsD 4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD 4306 Practice for Aviation Fuel Sample Containers forTests Affected by Trace ContaminationE1 Specification for ASTM Liquid-in-Glass Thermometers3. Terminology3.1 Definitions of
8、 Terms Specific to This Standard:3.1.1 membrane filter, na thin medium of closely con-trolled pore size through which a liquid is passed and on whichparticulate matter in suspension is retained.3.1.2 oxygen overpressurepartial pressures of oxygenhigher than that of air at atmospheric pressure.3.1.3
9、potential storage stabilitythe tendency of a fuel toform insolubles under the conditions of this test method.3.1.4 reactorany vessel capable of sustaining pressuresand temperatures above ambient, sometimes designated pres-sure vessel or bomb.3.1.5 weighing assemblya set of two filters and twoaluminu
10、m weighing dishes used to determine total insolublesfor each sample or blank.4. Summary of Test Method4.1 A 100 mL aliquot of filtered fuel is placed in aborosilicate glass container. The container is placed in apressure vessel which has been preheated to 90C. Thepressure vessel is pressurized with
11、oxygen to 800 kPa (abso-lute) (100 psig) for the duration of the test. The pressure vesselis placed in a forced air oven at 90C for 16 h. (WarningObserve all normal precautions while using oxygen underpressure and at high temperatures in the presence of combus-tible liquids. Appropriate shielding sh
12、ould be used for anycontainers under pressure. Pressurize and depressurize thecontainers slowly using appropriate personnel shielding. Neverattempt to open the pressure vessel while it is pressurized. Allfuel and solvent handling should be done in an appropriatefume hood only.) After aging and cooli
13、ng, 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 against other specific fuel samples orstandards with or without stabilize
14、r additives when testedunder identical conditions. This test method is not meant to1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.14 on Stability and Cleanliness of Liquid Fuels.Current edition
15、 approved May 1, 2006. Published May 2006. Originallyapproved in 1992. Last previous edition approved in 2005 as D 530405.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, ref
16、er to the standards Document Summary page onthe ASTM website.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.relate a specific fuel to specific field handling and stor
17、ageconditions. The formation of insolubles is affected by thematerial present in the storage container and by the ambientconditions. Since this test method is conducted in glass understandardized conditions, the results from different fuels can becompared on a common basis.6. Apparatus6.1 Sample or
18、Blank Container, a brown borosilicate glassbottle capable of holding 100 mL of sample but with totalvolume less than 200 mL, or a Test Method D 525 glass insert.A top closure of aluminum foil, perforated with small holes forbreathing, will be required if there is more than one sample perpressure ves
19、sel.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 in this test methodis 800 kPa (absolute) (100 psig). Many pressure gauges arecalibrated in kPa
20、(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 sample containers(WarningPressure vessels having internal volumes from250 to 8000 mLhave been used
21、and found to be suitable. If 250mL vessels such as Test Method D 525 oxidation bombs areused, four will be required. The larger volume pressure vesselscan accommodate multiple sample or blank containers). Thepressure vessel(s) (reactor(s) must be obtained only fromcommercial sources.6.3 Heater, capa
22、ble of maintaining the test temperature at90 6 1C for the duration of the test. Ensure heater tempera-ture uniformity. Heater shall be capable of holding the pressurevessel(s) (reactor(s) described in 6.2.(WarningStatic (non-forced air) ovens and unstirred liquid medium baths, such asthe Test Method
23、 D 525 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 heat. (WarningUseof an explosion-proof oven is required.)6.4 Drying Oven, forced air operat
24、ed at 110 6 5C. Staticovens 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 adherent insolubles solvent.6.7 Analytical Balance, capable of weighing to the nearest0.1 mg.6.8
25、 Filtration SystemArrange the following componentsas shown in Fig. 1.6.8.1 Funnel and Funnel Base, with filter support for a47mm diameter membrane and a locking ring or spring actionclip.6.8.2 Ground/Bond Wire, 0.912 2.59 mm (No. 10 throughNo. 19) bare-stranded, flexible, stainless steel, or copperi
26、nstalled in the 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 fla
27、sk equipped with 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
28、low heat so that 10mL of toluene placed in the aluminum dish described in 6.6will require 10 to 25 min to evaporate.FIG. 1 Schematic of Filtration SystemD53040626.10 Thermometer, conforming to the requirements pre-scribed in Specification E1. Temperature measuring devicessuch as ASTM 61C (IP No. 63C
29、), liquid-in-glass thermom-eters, thermocouples, or platinum resistance thermometers thatprovide equivalent or better accuracy and precision may beused.6.11 Forceps, approximately 12 cm long, flat-bladed, withnon-serrated, non-pointed tips.7. Reagents and Materials7.1 Purity of ReagentsReagent grade
30、 chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents conform to the specifications of the Committee onAnalytical Reagents of the American Chemical Society wheresuch specifications are available.3Other grades may be used,provided it is first ascertained th
31、at the reagent is of sufficientlyhigh purity to permit 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
32、 than0.001 % and boiling range between 35 and 100C are satisfac-tory. 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 sta
33、ndards to deliver 800 6 10 kPa (100 6 1 psig).(WarningOxygen at elevated temperature and pressure iscapable 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. Sampling
34、8.1 Field SamplingField sampling should be in accor-dance with Practices D 4057 or D 4177. Bulk fuel to besampled must be above its cloud point and thoroughly mixedprior to aliquot sampling. For field sampling and shipping, useonly epoxy-lined steel cans that have been cleaned according toPractice D
35、 4306.8.2 Laboratory SubsamplingFuel to be sampled 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.
36、9. Preparation of Apparatus9.1 Rinse the sample 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 10
37、5 to 115C. Ensure thesample bottles are cleaned 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 fol
38、lowed by drying in adrying oven at 105 to 115C. Even new aluminum dishes mustbe 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 th
39、e adherentinsolubles evaporation assembly 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 alu
40、minum dishes to the nearest 0.1mg. A separate 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 chan
41、ges in weight due to temperatureand humidity.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. Tra
42、nsfer 100 mL of the filtered fuel to each 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). (WarningIf more than one fuel is to betested simultaneously, additional glass sample containers arerequire
43、d. 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 pressure vessel toan oxygen cylinder via the
44、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 6 10 kPa (100 6 1 psig) as preset on the secondaryregulator. (WarningSee 6.2.)10.3 Clo
45、se the pressure vessel isolation valve and maintaintemperature at 90 6 1C 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 dropped morethan 20 kPa (absolute) (2 psig) and must be repe
46、ated 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 63Reagent Chemicals, American Chemical Society Specifications, America
47、nChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC),
48、 Rockville,MD.D53040635C) 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. After thesample contai
49、ner is empty and the filter is dry, (1) relieve thevacuum, (2) thoroughly rinse the inside of the sample containerwith at least 25 mL of filtered hydrocarbon solvent (see 7.3),and pour into filter holder, and (3) pull solvent through filterwith vacuum. Repeat steps (1) through (3). Wash down filterholder with filtered hydrocarbon solvent from a rinse bottle andpull through filter.10.7 Wash down the inside of the funnel and the outside ofthe joint between the funnel and the filter base with filteredhydrocarbon solvent.10.8 With the vacuum applied
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