1、Designation: D 7345 08An American National StandardStandard Test Method forDistillation of Petroleum Products at Atmospheric Pressure(Micro Distillation Method)1This standard is issued under the fixed designation D 7345; the number immediately following the designation indicates the year oforiginal
2、adoption 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 distill
3、ation characteristics of petroleum products havingboiling range between 20 to 400C at atmospheric pressureusing an automatic micro distillation apparatus.1.2 This test method is applicable to such products as; lightand middle distillates, automotive spark-ignition engine fuels,automotive spark-ignit
4、ion engine fuels containing up to 10 %ethanol, aviation gasolines, aviation turbine fuels, regular andlow sulfur diesel fuels, biodiesel blends up to 20 % biodiesel,special petroleum spirits, naphthas, white spirits, kerosines,burner fuels, and marine fuels.1.3 The test method is also applicable to
5、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 SI units are to be regarded as
6、standard. 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 practices and determine the
7、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 contractual agreements or re
8、gulatory ruleswhere earlier versions of the method(s) identified may berequired.2.2 ASTM Standards:2D86 Test Method for Distillation of Petroleum Products atAtmospheric PressureD 323 Test Method for Vapor Pressure of Petroleum Prod-ucts (Reid Method)D 4057 Practice for Manual Sampling of Petroleum a
9、ndPetroleum ProductsD 4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD 4953 Test Method for Vapor Pressure of Gasoline andGasoline-Oxygenate Blends (Dry Method)D 5190 Test Method for Vapor Pressure of Petroleum Prod-ucts (Automatic Method)D 5191 Test Method for Vapor Pressure
10、 of Petroleum Prod-ucts (Mini Method)D 5482 Test Method for Vapor Pressure of Petroleum Prod-ucts (Mini MethodAtmospheric)D 5854 Practice for Mixing and Handling of LiquidSamples of Petroleum and Petroleum ProductsD 6299 Practice for Applying Statistical Quality Assuranceand Control Charting Techniq
11、ues to Evaluate AnalyticalMeasurement System PerformanceD 6300 Practice for Determination of Precision and BiasData for Use in Test Methods for Petroleum Products andLubricantsD 6708 Practice for Statistical Assessment and Improve-ment of Expected Agreement Between Two Test Methodsthat Purport to Me
12、asure the Same Property of a Material2.3 Energy Institute Standards:3IP 69 Petroleum products - Determination of vapour pres-sure - Reid methodIP394 Liquid petroleum products - Vapour pressure - Part 1:Determination of air saturated vapour pressure (ASVP)1This test method is under the jurisdiction o
13、f ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.08 on Volatility.Current edition approved Oct. 15, 2008. Published November 2008. Originallyapproved in 2007. Last previous edition approved in 2007 as D 734507.2For 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.3Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR,U.K., http:/www.ene
15、rgyinst.org.uk.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.2.4 ISO Standards:4Guide 34 General requirements for the competence ofreference material producersGuide
16、35 Reference materials General and statisticalprinciples for certification3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 automatic apparatus, nmicroprocessor-controlledunit that performs the procedures of automatically controllingthe evaporation of a liquid specimen under spe
17、cific 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 industry recognized referencemethod.3.1.2 corrected temperature reading, ntemperature read-ings, as described in 3.1.12, corr
18、ected to 101.3 kPa barometricpressure.3.1.3 end point (EP) or final boiling point (FBP),nmaximum corrected temperature readings obtained duringthe test at the instant the flask internal pressure returns to theinitial pressure level registered by automatic apparatus.3.1.3.1 DiscussionThis usually occ
19、urs 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 within the distil-lation flask obtained during the test by a differential pressuresensor of automatic apparatus.3.1.4.
20、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 automatic apparatus.3.1.5 initial boiling point (IBP), ncorrected temperaturereadings that corresponds to the instant o
21、f the flask internalpressure rise registered by automatic apparatus.3.1.6 liquid temperature, ntemperature of the liquidspecimen in the distillation flask during the test obtained by aliquid temperature measuring device of automatic apparatus.3.1.7 percent evaporated, npercent recovered corrected to
22、a predicted by automatic analyzer evaporation loss percent.Percent evaporated is automatically reported for ASTM 7Cthermometer correlation.3.1.8 percent recovered, nvolume percent automaticallyreported by the analyzer; expressed as a percentage of thecharge volume, associated with a simultaneous tem
23、peraturereadings. Percent recovered is reported for ASTM 8C ther-mometer correlation.3.1.9 percent recovery, npercent recovery predicted bythe automatic apparatus and expressed as a percentage of thecharge volume.3.1.10 percent residue, nvolume of residue in the distil-lation flask predicted by the
24、automatic apparatus and expressedas a percentage of the charge volume.3.1.11 reference method, nASTM D86test method or itsanalogs which is widely used for expression of the distillationcharacteristics of petroleum products in industry.3.1.12 temperature readings, nvapor and liquid tempera-ture has t
25、hrough 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 liquid-in-glass thermometer to determine the distillationcharacteristics of the material under test by industry recognizedre
26、ference 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.4. Summary of Test Method4.1 A specimen of the sample is transferred into the distil-lation flask, the distillation flas
27、k 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 liquid temperatures, and pressure in thedistillation flask as the sample gradually distills under atmo-spheric pressure
28、 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 istreated by the data processing system, converted to distillationcharacteristics and corrected for barometric pressure.4
29、.4 Test results are commonly expressed as percent recov-ered or evaporated versus corresponding temperature in com-pliance with industry recognized standard form and referencemethod either in a table or graphically, as a plot of thedistillation curve.5. Significance and Use5.1 The distillation (vola
30、tility) characteristics of hydrocar-bons have an important effect on their safety and performance,especially in the case of fuels and solvents. The boiling rangegives information on the composition, the properties, and thebehavior of the fuel during storage and use. Volatility is themajor determinan
31、t of the tendency of a hydrocarbon mixture toproduce potentially explosive vapors.5.2 The distillation characteristics are critically importantfor both automotive and aviation gasolines, affecting starting,warm-up, and tendency to vapor lock at high operatingtemperature or at high altitude, or both.
32、 The presence of highboiling point components in these and other fuels can signifi-cantly affect the degree of formation of solid combustiondeposits.5.3 Distillation limits are often included in petroleum prod-uct specifications, in commercial contract agreements, processrefinery/control application
33、s, 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 process monitoring, fuel adultera-tion control, or other purposes including use as a portableapparatus for fiel
34、d testing.4Available from International Organization for Standardization (ISO), 1 rue deVaremb, Case postale 56, CH-1211, Geneva 20, Switzerland, http:/www.iso.ch.D73450825.5 This test method uses an automatic micro distillationapparatus, provides fast results using small sample volume, andeliminate
35、s much of the operator time and subjectivity incomparison to Test Method D86.6. Apparatus6.1 Basic Components of the Automatic Apparatus:56.1.1 The basic components of the micro distillation unit arethe distillation flask, a condensate recovery area with wastebeaker, an enclosure for the distillatio
36、n flask with the heatsource and flask support, the specimen 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,
37、 and the data processingsystem for converting recorded information into typical indus-try recognized standard report form.6.2 Adetailed description of the apparatus is given inAnnexA1.6.3 Barometer for CalibrationA pressure measuring de-vice capable of measuring local station pressure with anaccurac
38、y of 0.1 kPa (1 mmHg) or better, at the same elevationrelative 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 a
39、s those used at weather stations andairports, since these are precorrected to give sea level read-ings.)6.4 Sampling DeviceGlass or plastics syringe capacity10 6 0.3 mL or constant volume dispenser capacity 10 6 0.3mL.6.5 Waste BeakerGlass approximately 200 mL capacity,outside diameter approximately
40、 70 mm and height approxi-mately 130 mm fitted with 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. (Wa
41、rningFlammable. Liquid causes eye burns. Vapor harmful. 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
42、. Harmful if inhaled. Skin irritant on repeatedcontact. 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 t
43、he American ChemicalSociety.67.5 Granular Pumice Stones, clean and dry fine gradepumice stones of diameter 0.8 to 3.0 mm, approximately 10grains are necessary for each test.7.6 Sample Drying AgentAnhydrous sodium sulfate hasbeen found to be suitable.8. Sampling, Storage, and Sample Conditioning8.1 S
44、ampling:8.1.1 The extreme sensitivity of volatility 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 withPractic
45、e D 4057, D 4177 or D 5854 when appropriate. At least50 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 e
46、nds.8.2 Sample Storage:8.2.1 All samples shall be 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 100C from excessivetemperatures prior to testing. Th
47、is can be accomplished bystorage of the sample container in an appropriate ice bath orrefrigerator at a temperature below 10C. Other samples can bestored 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 temper
48、aturewhen it is completely fluid. It shall be vigorously shaken aftermelting, prior to opening the sample container, to ensurehomogeneity.8.3 Wet Samples:8.3.1 Samples of materials that visibly contain water are notsuitable for testing by this test method. If the sample is not dry,obtain another sam
49、ple that is free from suspended water.8.3.2 If such a sample cannot be obtained, remove any freewater by placing approximately 30 mL of the sample to betested in a glass conical flask containing approximately 10 g ofthe drying agent. Stopper and shake gently. Allow the mixtureto settle for approximately 15 min. Once the sample shows novisible signs of water, use a decanted portion of the sample forthe analysis. It is recommended to filter the test portion fromthe residual or suspended drying agent. During this drying andfiltration operations take care t
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