1、Designation: D7545 13D7545 14Standard 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*1.1 This laboratory test method covers a quantitative determination of the stability of middle
3、 distillate fuels such as diesel fuelsand heating oils, with up to 100% biodiesel, under accelerated oxidation conditions, by an automatic instrument.NOTE 1This test method is technically equivalent to test method EN 160911.2 This test method is designed for products complying with Specification D97
4、5 on Diesel Fuel, Grades No. 1D and 2D;Specification D396 on Burner 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 indic
5、ation of theoxidation and storage stability of middle distillate fuels.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 u
6、se. It is the responsibilityof the user of this standard to establish 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
7、Practice for Manual Sampling of Petroleum and Petroleum ProductsD4177 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
8、Standards:CEN/TR 16366:2012 Liquid Petroleum ProductsMiddle Distillates 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
9、 Distillates and Fatty Acid Methyl Ester (FAME) Fuels and BlendsDetermination 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
10、 Standard:3.1.1 break point, npressure in the test apparatus which is 10 % below the maximum pressure of the actual test run.1 This test method is under the jurisdiction ofASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of SubcommitteeD02.14 on
11、 Stability and Cleanliness of Liquid Fuels.Current edition approved Oct. 1, 2013Jan. 1, 2014. Published October 2013January 2014. Originally approved in 2009. Last previous edition approved in 20092013 asD7545 09.D7545 13. DOI: 10.1520/D7545-13.10.1520/D7545-14.2 For referencedASTM standards, visit
12、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 Committee for Standardization (CEN), Avenue Marnix 17, B-1000, Brussels,
13、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 intended only to provide the user of an ASTM standard an indication of what
14、 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 versionof the standard as published by ASTM is to be considered the
15、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 States13.1.2 induction period, ntime elapsed between starting the heating procedure of the sample vessel and t
16、he break point,measured in minutes.4. Summary of Test Method4.1 A 5 mL sample is introduced into a pressure vessel which is then charged with oxygen to 700 kPa at ambient temperature.The test is initiated by starting the heater and heating the pressure vessel to a temperature of 140C.4.2 The pressur
17、e is recorded continuously until the breakpoint is reached. Alternatively, 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 C
18、ompared to some other oxidation and storage stability test methods, 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 tes
19、t sample cup capable of being rapidly heated, fitted with a pressure 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 vessel
20、is fitted with filling and relief-valves and a means of automatically 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 contamin
21、ations of previous samples, capable of delivering 5.0 6 0.1 mL.6.3 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.
22、1C, iscalibrated by an approved calibration service, such as one 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
23、sensor (Fig. 3). The pressure calibration sensor iscalibrated to 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
24、. Reagents and Materials7.1 Solvent for the removal of oxidation 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 a
25、cetone, may be used if shown to meet the requirements for the removal 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 t
26、hat will not scratch the surface.7.4 “O -ring” SealSee A1.2.7.5 Temperature 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
27、relating to hot andflammable fuels, the apparatus shall be operated 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”
28、seal and discard.5 The sole source of supply of the apparatus known to the committee at this time is Anton Paars PetroOxy apparatus, available from Anton Paar ProveTec GmbH,Ludwig-Erhard-Ring 13,15827 Dahlewitz, Germany. If you are aware of alternative suppliers, please provide this information to A
29、STM International Headquarters. Yourcomments will receive careful consideration at a meeting of the responsible technical committee,1 which you may attend.D7545 1421. Unlocking mechanism for insulating hood2. Safety and insulating hood3. Screw cap for closing the test container4. Oxygen outlet5. Oxy
30、gen inlet6. “O-ring” seal for test sample cup7. Test sample cup8. Locking mechanism for insulating hood9. Operating panel with displayFIG. 1 Schematic of Apparatus for Rapid Small Scale Oxidation TestD7545 143NOTE 2To avoid contamination of the new test, it is necessary to discard the used “O-ring”
31、seal, because it might be soaked with oxidation productsfrom the previous test.10.3 Wipe the test sample cup, the seal groove and the cover of the test vessel with lint-free cleaning tissue (7.3) soaked withsolvent until free of gum or other oxidation residues.10.4 Allow the test sample cup and cove
32、r to dry in air and visually inspect for cleanliness.NOTE 3Compressed air is generally unsuitable to speed up evaporation of solvent because it can contain traces of oil that could contaminate the nexttest.10.5 Insert a new “O-ring” seal.1. Calibration cover with duct for temperature calibration sen
33、sor2. Calibration fluid3. Temperature sensor for block temperature4. Heating block5. Immersion depth of temperature calibration sensor and bottom ofcalibration cover6. Seal7. Temperature calibration sensor8. Connector plug to measuring deviceFIG. 2 Temperature Calibration EquipmentD7545 14411. Calib
34、ration11.1 Recalibrate the tester every 12 months for correct temperature and pressure detection.11.2 Calibration of Temperature IndicatorCalibrate the temperature sensor (A1.6) to the nearest 0.1C using the temperaturecalibration equipment (6.3) according to A2.1.11.3 Calibration of Pressure Detect
35、orCalibrate the pressure sensor (A1.5) to the nearest 10 kPa, using the pressure calibrationequipment (6.4) according to A2.2.11.4 Verify, at least every 3 months, that the heater is operating properly and the pressure vessel is reaching 14060.5C within5 min.12. Procedure12.1 Switch the apparatus on
36、. Bring the pressure vessel and the fuel specimen to be tested to a temperature of 15 to 25C.12.2 Using a volumetric device (6.2), place 5 6 0.1 mL of the sample into the test sample cup (Fig. 1, item 7).12.3 Cover the test sample cup with the screw-cap (Fig. 1, item 3) and close the pressure vessel
37、.FIG. 3 Pressure Calibration EquipmentD7545 14512.4 Introduce oxygen (7.2) into the pressure vessel until a pressure of 700 6 5 kPa is attained and stabilized over 20 s.12.5 Start the heater with no delay between charging with oxygen and starting the test. The apparatus automatically starts thetimer
38、.12.6 The apparatus brings the oxidation pressure vessel and test specimen to 140 6 0.5C within 5 min.12.7 If, during the initial 5 min of the test, a steady drop in pressure is observed, discontinue the test and discard the testspecimen.12.7.1 Under no circumstances may the leakage rate exceed a va
39、lue of 2 kPa/h. If the leakage rate shows an increase, checkthe following components: O-ring for damage or residues of samples; 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
40、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 breakp
41、oint.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 4The apparatus will automatically switch on the fan to cool the pressure vessel to approximately room temperature. When the apparatu
42、s 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 peri
43、od 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 period
44、.14. Precision and Bias14.1 Precision:14.1.1 The precision statements below were developed from data 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 accordan
45、ce with ISO 4259. Samples in the round robins included B100 (FAME), B0, B5, B7, B10 and B30 samples, Theinduction periods measured were between 22 min to 215 min.14.1.3 The samples had been prepared by blending of B0 which meets the requirements of the EN 590 with a sulfur contentsbelow 15 mg/kg onl
46、y with other fuels such that the resulting final blends for B5 and B7 also met the requirements of EN 590. Othersamples all contained less than 15 mg/kg sulfur. Since Specifications D396 and D975 both include grades with sulfur above 15mg/kg, these precision statements are not based on samples with
47、sulfur contents in the range of all specification grades. The effectof sulfur contents 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 using the same a
48、pparatusunder 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, rounded to the n
49、earest 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 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 5The precision statements are from an approved technical report CEN/TR 16366:2012 and can be obtained f
