1、Designation: D7545 09D7545 13Standard Test Method forOxidation Stability of Middle Distillate FuelsRapid SmallScale Oxidation Test (RSSOT)1This standard is issued under the fixed designation D7545; the number immediately following the designation indicates the year oforiginal adoption or, in the cas
2、e of revision, 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.1. Scope Scope*1.1 This laboratory test method covers a quantitative determination of the stability of
3、middle distillate fuels such as diesel fuelsand heating oils, with up to 100% biodiesel, under accelerated oxidation conditions, by an automatic instrument.1.2 This test method is designed for products complying with Specification D975 on Diesel Fuel, Grades No. 1D and 2D;Specification D396 on Burne
4、r Fuel, Grades No. 1 and No. 2; Specification D6751 on Biodiesel, B100, and Specification D7467on Diesel Fuel Oil, B6 to B20.1.3 This test method measures the induction period, under specified conditions, which can be used as an indication of theoxidation and storage stability of middle distillate f
5、uels.1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establ
6、ish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D396 Specification for Fuel OilsD975 Specification for Diesel Fuel OilsD4057 Practice for Manual Sampling of Petroleum and Petroleum ProductsD4
7、177 Practice for Automatic Sampling of Petroleum and Petroleum ProductsD6751 Specification for Biodiesel Fuel Blend Stock (B100) for Middle Distillate FuelsD7467 Specification for Diesel Fuel Oil, Biodiesel Blend (B6 to B20)2.2 Other Standards:CEN/TR 16366:2012 Liquid Petroleum ProductsMiddle Distil
8、lates and Fatty Acid Methyl Ester (FAME) Fuels andBlendsRound Robin Report on Applicability of Rapid Small Scale Oxidation Test Method3EN 590 Automotive FuelsDieselRequirements and Test Methods3EN 16091 Liquid Petroleum ProductsMiddle Distillates and Fatty Acid Methyl Ester (FAME) Fuels and BlendsDe
9、termination of Oxidation Stability by Rapid Small Scale Oxidation Method3ISO 4259 Petroleum ProductsDetermination and Application of Precision Data in Relation to Methods of Test43. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 break point, npressure in the test apparatus which
10、 is 10 % below the maximum pressure of the actual test run.3.1.2 induction period, ntime elapsed between starting the heating procedure of the sample vessel and the break point,measured in minutes.1 This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products Products, Liqu
11、id Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.14 on Stability and Cleanliness of Liquid Fuels.Current edition approved July 1, 2009Oct. 1, 2013. Published August 2009October 2013. Originally approved in 2009. Last previous edition approved in 2009 asD7545 09. DOI: 10.1
12、520/D7545-09.10.1520/D7545-13.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 Available from European Commi
13、ttee for Standardization (CEN), Avenue Marnix 17, B-1000, Brussels, Belgium, http:/www.cen.eu.4 Available from International Organization for Standardization (ISO), 1, ch. de la Voie-Creuse, CP 56, CH-1211 Geneva 20, Switzerland, http:/www.iso.org.This document is not an ASTM standard and is intende
14、d only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current
15、versionof the standard as published by ASTM is to be considered the official document.*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 States14. Summary of Test Method4.1 A5 mLA
16、 5 mL sample is introduced into a pressure vessel which is then charged with oxygen to 700 kPa at ambienttemperature. The test is initiated by starting the heater and heating the pressure vessel to a temperature of 140C.4.2 The pressure is recorded continuously until the breakpoint is reached. Alter
17、natively, the test may be terminated when aminimum specification requirement is reached.5. Significance and Use5.1 The induction period may be used as an indication of the oxidation and storage stability of middle distillate fuel.5.2 Compared to some other oxidation and storage stability test method
18、s, this method uses a small sample and gives a resultin a short time period.6. Apparatus6.1 GeneralThis test method uses an automatically controlled oxidation tester5 (see Fig. 1) comprising an oxidation pressurevessel containing a test sample cup capable of being rapidly heated, fitted with a press
19、ure sensor capable of measuring pressuresup to 2000 kPa and a temperature sensor capable of reading to 0.1C.6.1.1 Pressure and temperature in the oxidation vessel are recorded continuously during the test. The oxidation pressure vesselis fitted with filling and relief-valves and a means of automatic
20、ally releasing the pressure. The integrated cooling fan cools thepressure vessel from the test temperature to ambient temperature by a flow of air. See Annex A1 for detailed information.6.2 Volumetric DeviceClean and free from contaminations of previous samples, capable of delivering 5.0 6 0.1 mL.6.
21、3 Temperature Calibration EquipmentComprising a cover and a temperature calibration sensor (Fig. 2). The temperaturecalibration sensor is fixed to a depth of 15 6 0.5 mm. The temperature calibration sensor, calibrated to the nearest 0.1C, iscalibrated by an approved calibration service, such as one
22、that is traceable to the National Institute of Standards and Technology(NIST) or to a national authority in the country in which the equipment is used or manufactured.6.4 Pressure Calibration EquipmentComprising a pressure calibration sensor (Fig. 3). The pressure calibration sensor iscalibrated to
23、the nearest 10 kPa by an approved calibration service, such as one that is traceable to the National Institute ofStandards and Technology (NIST) or to a national authority in the country in which the equipment is used or manufactured.7. Reagents and Materials7.1 Solvent for the removal of oxidation
24、residues from the test vessel. The solvent shall be of suitable purity to leave no residueon the apparatus. Ethanol of 94% minimum purity has been found to be suitable. Other solvents, such as a mixture of equalvolumes of toluene and acetone, may be used if shown to meet the requirements for the rem
25、oval of oxidation residues from thetest vessel without leaving any residue in the sample test cup.7.2 OxygenCommercially available extra-dry oxygen of not less than 99.6% purity.7.3 Lint-free Cleaning TissueFor sensitive surfaces and that will not scratch the surface.7.4 “O -ring” SealSee A1.2.7.5 T
26、emperature Calibration FluidStable middle distillate liquid with a flash point above +60C and a boiling point above+150C.8. Hazards8.1 (WarningTo provide protection against possible explosive rupture of the pressure vessel and hazards relating to hot andflammable fuels, the apparatus shall be operat
27、ed behind an appropriate safety shield.)9. Sampling9.1 Sample in accordance with Practice D4057 or D4177.10. Preparation of Apparatus10.1 Remove the previous sample by means of a pipette or similar device.10.2 Remove the used “O-ring” seal and discard.5 The sole source of supply of the apparatus kno
28、wn to the committee at this time is Petrotest PetroOXY Anton Paars PetroOxy apparatus, available from Petrotest.Instruments GmbH surface of the sample cup for damage; sample cup for sampleresidues.12.7.2 Contact the manufacturer to resolve leakage problems from other parts of the instrument.12.8 The
29、 apparatus automatically records the temperature (to the nearest 0.1C) and pressure (to the nearest 1 kPa) of theoxidation vessel continuously.12.9 The test apparatus will automatically terminate the test when the pressure readings show a 10% drop from the maximumobserved pressure. This is the break
30、point.12.10 Record the induction period to the nearest 1 min.12.11 Alternatively, terminate the test when the test time exceeds a predetermined minimum requirement.NOTE 3The apparatus will automatically switch on the fan to cool the pressure vessel to approximately room temperature. When the apparat
31、us hascooled sufficiently, the apparatus automatically releases the pressure slowly from the pressure vessel through the valve at a rate not exceeding 345kPa/min. When the pressure release process has finished, open the apparatus and clean according Section 10.13. Report13.1 Report the induction per
32、iod to the nearest whole minute, and reference this test method. If the test was stopped (12.11) priorto observing the pressure drop required in 12.9, report induction period (referencing this test method) as greater than N minutes,where N is the predetermined minimum time within the induction perio
33、d.14. Precision and Bias14.1 The precision of the test method has not yet been determined by a formal inter laboratory study. Preliminary examinationsfor repeatability have shown a value of “r” = 3.2 minutes as interim precision.Precision:14.1.1 The precision statements below were developed from dat
34、a for EN 16091, which is technically identical to this testmethod.14.1.2 The data were developed in round robin tests in 2008 and 2009 supervised by the technical committee CEN/TC19/JWG1and in accordance with ISO 4259. Samples in the round robins included B100 (FAME), B0, B5, B7, B10 and B30 samples
35、, Theinduction periods measured were between 22 min to 215 min.14.1.3 ReproducibilityThe reproducibility of this test method is yet to be determined and will be available on or before2013.samples had been prepared by blending of B0 which meets the requirements of the EN 590 with a sulfur contents be
36、low 15mg/kg only with other fuels such that the resulting final blends for B5 and B7 also met the requirements of EN 590. Other samplesall contained less than 15 mg/kg sulfur. Since Specifications D396 and D975 both include grades with sulfur above 15 mg/kg, theseprecision statements are not based o
37、n samples with sulfur contents in the range of all specification grades. The effect of sulfurcontents or other associated differences in fuels will have on the precision of this test method is unknown.14.1.4 RepeatabilityThe difference between successive test results, obtained by the same operator u
38、sing the same apparatusunder constant operating conditions on identical test material, would in the long run, in the normal and correct operation of thistest method, exceed the following only in one case in twenty.r50.0288X10.4965 (1)where:X = the mean of the two test results expressed in minutes, r
39、ounded to the nearest 0.01 min.14.1.5 ReproducibilityThe difference between two single and independent test results obtained by different operators workingin different laboratories, on identical material, would in long run, in the normal and correct operation of this test method, exceedthe following
40、 only in one case in twenty.R50.0863X11.3772 (2)where:X = the mean of the two test results expressed in minutes, rounded to the nearest 0.01 min.NOTE 4The precision statements are from an approved technical report CEN/TR 16366:2012 and can be obtained from CEN (European Committeefor Standardization)
41、.D7545 13614.2 BiasSince the value of oxidation stability measured by this test method is defined solely by this test method, no statementof bias can be made.15. Keywords15.1 breakpoint; diesel fuel; biodiesel; induction period; middle distillate fuels; oxidation stability; oxygen uptakeANNEXES(Mand
42、atory Information)A1. AUTOMATICALLY CONTROLLED OXIDATION TESTERA1.1 Pressure Vessel and ClosureA1.1.1 Internal volume without sample: 20 mL. Inner diameter: 47 6 0.15 mm.A1.1.2 Made of corrosion-resistant material and constructed to withstand a working pressure of 1800 kPa.A1.1.3 Interior surfaces:
43、smooth (polished), chemically inert surface to facilitate cleaning and prevent corrosion.A1.2 “O-ring”A1.2.1 Seal for test sample cup.A1.2.2 Made of material being resistant to oxygen, middle distillate fuel components and heat, typically fluoro-elastomerFPM/FKM (commonly known as Viton6), coated wi
44、th PTFE.A1.3 HeatingA1.3.1 Installed power rating: 500 W. Typically electric heating, near the bottom of the pressure vessel, facilitates best heattransfer to the sample.A1.3.2 The heater control shall be capable of maintaining the test cup temperature within 60.5C at the test temperatures of140C.A1
45、.4 ValvesA1.4.1 Solenoid valves with small dead volume and orifice sizes and short cycling ratesA1.5 Pressure SensorA1.5.1 Absolute or relative pressure transducer.A1.5.2 Pressure range: 0 to 2000 kPa (min). Accuracy 63% full scale span. Typical sensitivity: 1 to 25 mV/kPa.6 Registered trademark of
46、DuPont Performance Elastomers, 300 Bellevue Parkway, Suite 300, Wilmington, DE 19809.D7545 137A1.6 Temperature SensorA1.6.1 Platinum resistance thermometer, accuracy 6(0.1 + 0.0017 (t), where (t) is the actual temperature in C, range up to200C.A1.7 Connecting PipesA1.7.1 Small orifices, typical inne
47、r diameter: 0.5 to 1.0 mm.A1.8 Cooling FanA1.8.1 Capable of cooling the pressure vessel from the test temperature to ambient temperature by applying a stream of air to theoutside of the pressure vessel.A1.9 General RequirementsA1.9.1 All equipment in contact with the sample and oxygen shall be made
48、of corrosion-resistant materials.A1.9.2 The pressure vessel shall have an over-temperature safeguard.A1.9.3 A cooling device for rapid cooling is recommended.A1.9.4 A safety and isolation hood above the pressure vessel closure is recommended (see Fig. 1).A2. INSTRUMENT CALIBRATIONA2.1 Temperature Ca
49、librationA2.1.1 Calibrate temperature sensor (A1.6) at ambient and at 140C concerning offset and gain, in accordance with themanufacturers manual.A2.1.2 Fill the cup with 10 6 0.1 mL of the calibration fluid (7.5).A2.1.3 Ensure that the temperature calibration sensors depth is fixed at 15 6 0.5 mm (Fig. 2, item 5).A2.1.4 Cover the test sample cup with the temperature calibration equipment (6.3) (Fig. 2).A2.1.5 When the temperature is stabilized, record the temperatures indicated by the temperature sensor (A1.6) and thetemperature calib
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