1、Designation: D 7545 09Standard Test Method forOxidation Stability of Middle Distillate FuelsRapid SmallScale Oxidation Test (RSSOT)1This standard is issued under the fixed designation D 7545; the number immediately following the designation indicates the year oforiginal adoption or, in the case of r
2、evision, 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. Scope1.1 This laboratory test method covers a quantitative deter-mination of the stability of middle disti
3、llate fuels such as dieselfuels and heating oils, with up to 100% biodiesel, underaccelerated oxidation conditions, by an automatic instrument.1.2 This test method is designed for products complyingwith Specification D 975 on Diesel Fuel, Grades No. 1D and2D; Specification D 396 on Burner Fuel, Grad
4、es No. 1 and No.2; Specification D 6751 on Biodiesel, B100, and SpecificationD 7467 on Diesel Fuel Oil, B6 to B20.1.3 This test method measures the induction period, underspecified conditions, which can be used as an indication of theoxidation and storage stability of middle distillate fuels.1.4 The
5、 values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.5 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-priat
6、e safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 396 Specification for Fuel OilsD 975 Specification for Diesel Fuel OilsD 4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD 4177 Pract
7、ice for Automatic Sampling of Petroleum andPetroleum ProductsD 6751 Specification for Biodiesel Fuel Blend Stock(B100) for Middle Distillate FuelsD 7467 Specification for Diesel Fuel Oil, Biodiesel Blend(B6 to B20)3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 break point, np
8、ressure in the test apparatus which is10 % below the maximum pressure of the actual test run.3.1.2 induction period, ntime elapsed between startingthe heating procedure of the sample vessel and the break point,measured in minutes.4. Summary of Test Method4.1 A 5 mL sample is introduced into a pressu
9、re vesselwhich is then charged with oxygen to 700 kPa at ambienttemperature. The test is initiated by starting the heater andheating the pressure vessel to a temperature of 140C.4.2 The pressure is recorded continuously until the break-point is reached.Alternatively, the test may be terminated whena
10、 minimum specification requirement is reached.5. Significance and Use5.1 The induction period may be used as an indication of theoxidation and storage stability of middle distillate fuel.5.2 Compared to some other oxidation and storage stabilitytest methods, this method uses a small sample and gives
11、 aresult in a short time period.6. Apparatus6.1 GeneralThis test method uses an automatically con-trolled oxidation tester3(see Fig. 1) comprising an oxidationpressure vessel containing a test sample cup capable of beingrapidly heated, fitted with a pressure sensor capable of mea-suring pressures up
12、 to 2000 kPa and a temperature sensorcapable of reading to 0.1C.6.1.1 Pressure and temperature in the oxidation vessel arerecorded continuously during the test. The oxidation pressurevessel is fitted with filling and relief-valves and a means ofautomatically releasing the pressure. The integrated co
13、oling1This 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 approved July 1, 2009. Published August 2009.2For referenced ASTM standards,
14、visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3The sole source of supply of the apparatus known to the committee at this timeis Petrotest P
15、etroOXY apparatus, available from Petrotest. Instruments GmbH surface of the sample cup for damage; sample cup forsample residues.12.7.2 Contact the manufacturer to resolve leakage prob-lems from other parts of the instrument.12.8 The apparatus automatically records the temperature(to the nearest 0.
16、1C) and pressure (to the nearest 1 kPa) of theoxidation vessel continuously.12.9 The test apparatus will automatically terminate the testwhen the pressure readings show a 10% drop from themaximum observed pressure. This is the breakpoint.12.10 Record the induction period to the nearest 1 min.12.11 A
17、lternatively, terminate the test when the test timeexceeds a predetermined minimum requirement.NOTE 3The apparatus will automatically switch on the fan to cool thepressure vessel to approximately room temperature. When the apparatushas cooled sufficiently, the apparatus automatically releases the pr
18、essureslowly from the pressure vessel through the valve at a rate not exceeding345 kPa/min. When the pressure release process has finished, open theapparatus and clean according Section 10.13. Report13.1 Report the induction period to the nearest wholeminute, and reference this test method. If the t
19、est was stopped(12.11) prior to observing the pressure drop required in 12.9,report induction period (referencing this test method) as greaterthan N minutes, where N is the predetermined minimum timewithin the induction period.14. Precision and Bias14.1 The precision of the test method has not yet b
20、eendetermined by a formal inter laboratory study. Preliminaryexaminations for repeatability have shown a value of “r” = 3.2minutes as interim precision.14.1.1 ReproducibilityThe reproducibility of this testmethod is yet to be determined and will be available on orbefore 2013.14.2 BiasSince the value
21、 of oxidation stability measuredby this test method is defined solely by this test method, nostatement of bias can be made.15. Keywords15.1 breakpoint; diesel fuel; biodiesel; induction period;middle distillate fuels; oxidation stability; oxygen uptakeANNEXES(Mandatory Information)A1. AUTOMATICALLY
22、CONTROLLED OXIDATION TESTERA1.1 Pressure Vessel and ClosureA1.1.1 Internal volume without sample: 20 mL. Inner di-ameter: 47 6 0.15 mm.A1.1.2 Made of corrosion-resistant material and constructedto withstand a working pressure of 1800 kPa.A1.1.3 Interior surfaces: smooth (polished), chemically in-ert
23、 surface to facilitate cleaning and prevent corrosion.A1.2 “O-ring”A1.2.1 Seal for test sample cup.D7545095A1.2.2 Made of material being resistant to oxygen, middledistillate fuel components and heat, typically fluoro-elastomerFPM/FKM (commonly known as Viton4), coated with PTFE.A1.3 HeatingA1.3.1 I
24、nstalled power rating: 500 W. Typically electricheating, near the bottom of the pressure vessel, facilitates bestheat transfer to the sample.A1.3.2 The heater control shall be capable of maintainingthe test cup temperature within 60.5C at the test temperaturesof 140C.A1.4 ValvesA1.4.1 Solenoid valve
25、s with small dead volume and orificesizes 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.A1.6 Temperature SensorA1.6.1 Platinum resistance thermomet
26、er, accuracy 6(0.1 +0.0017 3 (t), where (t) is the actual temperature in C, rangeup to 200C.A1.7 Connecting PipesA1.7.1 Small orifices, typical inner diameter: 0.5 to 1.0 mm.A1.8 Cooling FanA1.8.1 Capable of cooling the pressure vessel from the testtemperature to ambient temperature by applying a st
27、ream of airto the outside of the pressure vessel.A1.9 General RequirementsA1.9.1 All equipment in contact with the sample andoxygen shall be made of corrosion-resistant materials.A1.9.2 The pressure vessel shall have an over-temperaturesafeguard.A1.9.3 A cooling device for rapid cooling is recommend
28、ed.A1.9.4 A safety and isolation hood above the pressurevessel closure is recommended (see Fig. 1).A2. INSTRUMENT CALIBRATIONA2.1 Temperature CalibrationA2.1.1 Calibrate temperature sensor (A1.6) at ambient andat 140C concerning offset and gain, in accordance with themanufacturers manual.A2.1.2 Fill
29、 the cup with 10 6 0.1 mL of the calibration fluid(7.5).A2.1.3 Ensure that the temperature calibration sensorsdepth is fixed at 15 6 0.5 mm (Fig. 2, item 5).A2.1.4 Cover the test sample cup with the temperaturecalibration equipment (6.3)(Fig. 2).A2.1.5 When the temperature is stabilized, record thet
30、emperatures indicated by the temperature sensor (A1.6) andthe temperature calibration sensor.A2.1.6 Calculate offset and gain according to manufactur-ers manual and change, if required, according to manufactur-ers manual.A2.2 Pressure CalibrationA2.2.1 Calibrate the pressure sensor (A1.5) at two pre
31、s-sures.A2.2.2 Cover the empty sample cup with the screw-cap(Fig. 1, item 3).A2.2.3 Connect the oxygen filling line to the instrument andpressurize the test cell to 700 kPa.A2.2.4 Close the filling valve, remove the oxygen fillingline and replace it by the calibration equipment (Fig. 3)(6.4).A2.2.5
32、Start the calibration procedure in accordance withthe manufacturers manual.A2.2.6 Open the valve to the pressure calibration sensor.Pressure will slightly drop.A2.2.7 Record the pressures indicated by the pressuresensor (A1.5) and the pressure calibration sensor.A2.2.8 Close the valve to the pressur
33、e calibration equip-ment (6.4).A2.2.9 Reduce the pressure in the test cell to approximately20 kPa, and open the valve to the calibration equipment.Pressure will slightly increase to 90 to 100 kPa.A2.2.10 Record the pressures indicated by the pressuresensor (A1.5) and the pressure calibration sensor.
34、A2.2.11 Release the pressure.A2.2.12 Calculate offset and gain according to the manu-facturers manual and change if required according to manu-facturers manual.4Registered trademark of DuPont Performance Elastomers, 300 BellevueParkway, Suite 300, Wilmington, DE 19809.D7545096ASTM International take
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