ASTM D7345-2014 6583 Standard Test Method for Distillation of Petroleum Products and Liquid Fuels at Atmospheric Pressure (Micro Distillation Method)《大气压力下石油产品和液体燃料蒸馏的标准试验方法 (微量蒸馏法.pdf

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1、Designation: D7345 14596/12Standard Test Method forDistillation of Petroleum Products and Liquid Fuels atAtmospheric Pressure (Micro Distillation Method)1This standard is issued under the fixed designation D7345; the number immediately following the designation indicates the year oforiginal adoption

2、 or, in the case 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 test method covers a procedure for determinationof the distillation ch

3、aracteristics of petroleum products andliquid fuels having boiling range between 20 C to 400 C atatmospheric pressure using an automatic micro distillationapparatus.1.2 This test method is applicable to such products as; lightand middle distillates, automotive spark-ignition engine fuels,automotive

4、spark-ignition engine fuels containing up to 10 %ethanol, aviation gasolines, aviation turbine fuels, regular andlow sulfur diesel fuels, biodiesel (B100), biodiesel blends up to20 % biodiesel, special petroleum spirits, naphthas, whitespirits, kerosines, burner fuels, and marine fuels.1.3 The test

5、method is also applicable to hydrocarbons witha narrow boiling range, like organic solvents or oxygenatedcompounds.1.4 The test method is designed for the analysis of distillateproducts; it is not applicable to products containing appreciablequantities of residual material.1.5 The values stated in S

6、I units are to be regarded asstandard. No other units of measurement are included in thisstandard.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

7、 practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 All standards are subject to revision, and parties toagreement on this test method are to apply the most recentedition of the standards indicated below, unless otherwisespecified, such as in

8、 contractual agreements or regulatory ruleswhere earlier versions of the method(s) identified may berequired.2.2 ASTM Standards:2D86 Test Method for Distillation of Petroleum Products atAtmospheric PressureD323 Test Method for Vapor Pressure of Petroleum Products(Reid Method)D1160 Test Method for Di

9、stillation of Petroleum Products atReduced PressureD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD4953 Test Method for Vapor Pressure of Gasoline andGasoline-Oxygenate Blends (Dry Method)D5190 Test Method

10、for Vapor Pressure of Petroleum Prod-ucts (Automatic Method) (Withdrawn 2012)3D5191 Test Method for Vapor Pressure of Petroleum Prod-ucts (Mini Method)D5482 Test Method for Vapor Pressure of Petroleum Prod-ucts (Mini MethodAtmospheric)D5854 Practice for Mixing and Handling of Liquid Samplesof Petrol

11、eum and Petroleum ProductsD6299 Practice for Applying Statistical Quality Assuranceand Control Charting Techniques to Evaluate AnalyticalMeasurement System PerformanceD6300 Practice for Determination of Precision and BiasData for Use in Test Methods for Petroleum Products andLubricantsD6708 Practice

12、 for Statistical Assessment and Improvementof Expected Agreement Between Two Test Methods thatPurport to Measure the Same Property of a Material1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubc

13、ommittee D02.08 on Volatility.Current edition approved Dec. 1, 2014. Published January 2015. Originallyapproved in 2007. Last previous edition approved in 2008 as D7345 08. DOI:10.1520/D7345-14.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at s

14、erviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.*A Summary of Changes section appears at the end of this standardCopyright ASTM Int

15、ernational, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States12.3 Energy Institute Standards:4IP69 Petroleum products - Determination of vapour pressure- Reid methodIP 394 Liquid petroleum products - Vapour pressure - Part 1:Determination of air saturated vapour pre

16、ssure (ASVP)2.4 ISO Standards:5Guide 34 General requirements for the competence of refer-ence material producersGuide 35 Reference materials General and statisticalprinciples for certification3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 automatic apparatus, nmicroprocessor-

17、controlledunit that performs the procedures of automatically controllingthe evaporation of a liquid specimen under specific conditionsof this test method, collecting measurement data and convert-ing this data by patented algorithm in order to predict distilla-tion results in correlation with industr

18、y recognized referencemethod.3.1.2 corrected temperature reading, n temperaturereadings, as described in 3.1.12, corrected to 101.3 kPabarometric pressure.3.1.3 end point (EP) or final boiling point (FBP),nmaximum corrected temperature readings obtained duringthe test at the instant the flask intern

19、al pressure returns to theinitial pressure level registered by automatic apparatus.3.1.3.1 DiscussionThis usually occurs after the evapora-tion of all liquid from the bottom of the distillation flask. Theterm maximum temperature is a frequently used synonym.3.1.4 flask internal pressure, npressure w

20、ithin the distil-lation flask obtained during the test by a differential pressuresensor of automatic apparatus.3.1.4.1 DiscussionThe flask internal pressure data re-corded during the test is automatically converted to the volumepercent recovered or evaporated data by patented algorithmemployed by au

21、tomatic apparatus.3.1.5 initial boiling point (IBP), ncorrected temperaturereadings that corresponds to the instant of the flask internalpressure rise registered by automatic apparatus.3.1.6 liquid temperature, ntemperature of the liquid speci-men in the distillation flask during the test obtained b

22、y a liquidtemperature measuring device of automatic apparatus.3.1.7 percent evaporated, npercent recovered corrected toa predicted by automatic analyzer evaporation loss percent.Percent evaporated is automatically reported for ASTM 7Cthermometer correlation.3.1.8 percent recovered, nvolume percent a

23、utomaticallyreported by the analyzer; expressed as a percentage of thecharge volume, associated with a simultaneous temperaturereadings. Percent recovered is reported for ASTM 8C ther-mometer correlation.3.1.9 percent recovery, npercent recovery predicted by theautomatic apparatus and expressed as a

24、 percentage of thecharge volume.3.1.10 percent residue, nvolume of residue in the distil-lation flask predicted by the automatic apparatus and expressedas a percentage of the charge volume.3.1.11 reference method, nASTM D86 test method or itsanalogs which is widely used for expression of the distill

25、ationcharacteristics of petroleum products in industry.3.1.12 temperature readings, nvapor and liquid tempera-ture has through use of an algorithm of the automatic apparatusbeen adjusted to mimic the same temperature lag and emergentstem effects as would be seen when using an ASTM 7C/7F or8C/8F liqu

26、id-in-glass thermometer to determine the distillationcharacteristics of the material under test by industry recognizedreference method.3.1.13 vapor temperature, ntemperature of the vapors inthe distillation flask during the test obtained by a vaportemperature measuring device of automatic apparatus.

27、4. Summary of Test Method4.1 A specimen of the sample is transferred into the distil-lation flask, the distillation flask is placed into position on theautomatic apparatus, and heat is applied to the bottom of thedistillation flask.4.2 The automatic apparatus measures and records speci-men vapor and

28、 liquid temperatures, and pressure in thedistillation flask as the sample gradually distills under atmo-spheric pressure conditions. Automatic recordings are madethroughout the distillation and the data stored into the appara-tus memory.4.3 At the conclusion of the distillation, the collected data i

29、streated by the data processing system, converted to distillationcharacteristics and corrected for barometric pressure.4.4 Test results are commonly expressed as percent recov-ered or evaporated versus corresponding temperature in com-pliance with industry recognized standard form and referencemetho

30、d either in a table or graphically, as a plot of thedistillation curve.5. Significance and Use5.1 The distillation (volatility) characteristics of hydrocar-bons and other liquids have an important effect on their safetyand performance, especially in the case of fuels and solvents.The boiling range g

31、ives information on the composition, theproperties, and the behavior of the fuel during storage and use.Volatility is the major determinant of the tendency of ahydrocarbon mixture to produce potentially explosive vapors.5.2 The distillation characteristics are critically importantfor both automotive

32、 and aviation gasolines, affecting starting,warm-up, and tendency to vapor lock at high operatingtemperature or at high altitude, or both. The presence of highboiling point components in these and other fuels can signifi-cantly affect the degree of formation of solid combustiondeposits.4Available fr

33、om Energy Institute, 61 New Cavendish St., London, WIG 7AR,U.K., http:/www.energyinst.org.uk.5Available from International Organization for Standardization (ISO), 1 rue deVaremb, Case postale 56, CH-1211, Geneva 20, Switzerland, http:/www.iso.ch.D7345 1425.3 Distillation limits are often included in

34、 petroleum prod-uct specifications, in commercial contract agreements, processrefinery/control applications, and for compliance to regulatoryrules.5.4 This test method can be applied to contaminated prod-ucts or hydrocarbon mixtures. This is valuable for fast productquality screening, refining proce

35、ss monitoring, fuel adultera-tion control, or other purposes including use as a portableapparatus for field testing.5.5 This test method uses an automatic micro distillationapparatus, provides fast results using small sample volume, andeliminates much of the operator time and subjectivity incomparis

36、on to Test Method D86.6. Apparatus6.1 Basic Components of the Automatic Apparatus:66.1.1 The basic components of the micro distillation unit arethe distillation flask, a condensate recovery area with wastebeaker, an enclosure for the distillation flask with the heatsource and flask support, the spec

37、imen liquid temperaturemeasuring device, the specimen vapor temperature measuringdevice, the distillation flask internal pressure measuring device,the ambient pressure measuring device, the control systems forregulating the distillation process, and the data processingsystem for converting recorded

38、information into typical indus-try recognized standard report form.6.2 Adetailed description of the apparatus is given in AnnexA1.6.3 Barometer for CalibrationA pressure measuring de-vice capable of measuring local station pressure with anaccuracy of 0.1 kPa (1 mmHg) or better, at the same elevation

39、relative to sea level where the apparatus is located.6.3.1 The barometer is only required for periodic calibrationof the external and internal pressure measuring devices.6.3.2 (WarningDo not take readings from ordinary aner-oid barometers, such as those used at weather stations andairports, since th

40、ese are precorrected to give sea level read-ings.)6.4 Sampling DeviceGlass or plastics syringe capacity10 mL 6 0.3 mL or constant volume dispenser capacity 10 mL6 0.3 mL.6.5 Waste BeakerGlass approximately 200 mL capacity,outside diameter approximately 70 mm and height approxi-mately 130 mm fitted w

41、ith a cover to reduce evaporation. Thecover design shall allow the beaker to remain open to atmo-spheric pressure.7. Reagents and Materials7.1 Cleaning Solvents, suitable for cleaning and drying thetest flask such as; petroleum naphtha and acetone. (WarningFlammable. Liquid causes eye burns. Vapor h

42、armful. May befatal or cause blindness if swallowed or inhaled.)7.2 Toluene, 99.5 % purity. (WarningExtremely flam-mable. Harmful if inhaled. Skin irritant on repeated contact.Aspiration hazard.)7.3 n-Hexadecane, 99 % purity. (WarningExtremelyflammable. Harmful if inhaled. Skin irritant on repeatedc

43、ontact. Aspiration hazard.)7.4 Chemicals of at least 99 % purity shall be used in thecalibration procedure (see 10.2). Unless otherwise indicated, itis intended that all reagents conform to the specifications of theCommittee on Analytical Reagents of the American ChemicalSociety.77.5 Granular Pumice

44、 Stones, clean and dry fine gradepumice stones of diameter 0.8 mm to 3.0 mm, approximately10 grains are necessary for each test.7.6 Sample Drying AgentAnhydrous sodium sulfate hasbeen found to be suitable.8. Sampling, Storage, and Sample Conditioning8.1 Sampling:8.1.1 The extreme sensitivity of vola

45、tility measurements tolosses through evaporation and the resulting changes in com-position is such as to require the utmost precaution in thedrawing and handling of volatile product samples.8.1.2 Obtain a sample and test specimen in accordance withPractice D4057, D4177,orD5854 when appropriate. At l

46、east50 mL of sample is recommended.8.1.3 Sample shall be free from any suspended solids orother insoluble contaminations. Obtain another sample orremove solid particle by filtration. During filtration operationtake care to minimize any loss of light ends.8.2 Sample Storage:8.2.1 All samples shall be

47、 stored in a tightly closed andleak-free container away from direct sunlight or sources ofdirect heat.8.2.2 Protect samples containing light materials havingexpected initial boiling point lower than 100 C from excessivetemperatures prior to testing. This can be accomplished bystorage of the sample c

48、ontainer in an appropriate ice bath orrefrigerator at a temperature below 10 C. Other samples canbe stored at ambient or lower temperature.8.2.3 If the sample has partially or completely solidifiedduring storage, it is to be carefully heated to a temperaturewhen it is completely fluid. It shall be v

49、igorously shaken aftermelting, prior to opening the sample container, to ensurehomogeneity.8.3 Wet Samples:6The sole source of supply of the apparatus known to the committee at this timeis ISL /PAC, B.P. 70285 Verson, 14653 CARPIQUET FRANCE. If you are awareof alternative suppliers, please provide this information to ASTM InternationalHeadquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee,1which you may attend.7Reagent Chemicals, American Chemical Society Specifications, AmericanChemical So

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