1、Designation: D 86 09An American National StandardStandard Test Method forDistillation of Petroleum Products at Atmospheric Pressure1This standard is issued under the fixed designation D 86; the number immediately following the designation indicates the year of originaladoption or, in the case of rev
2、ision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscriptepsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1. Scope*1.1 This test method
3、covers the atmospheric distillation ofpetroleum products using a laboratory batch distillation unit todetermine quantitatively the boiling range characteristics ofsuch products as light and middle distillates, automotivespark-ignition engine fuels, automotive spark-ignition enginefuels containing up
4、 to 10 % ethanol, aviation gasolines, avia-tion turbine fuels, 1-D and 2-D diesel fuels, biodiesel blends upto 20 %, marine fuels, special petroleum spirits, naphthas,white spirits, kerosines, and Grades 1 and 2 burner fuels.1.2 The test method is designed for the analysis of distillatefuels; it is
5、not applicable to products containing appreciablequantities of residual material.1.3 This test method covers both manual and automatedinstruments.1.4 Unless otherwise noted, the values stated in SI units areto be regarded as the standard. The values given in parenthesesare provided for information o
6、nly.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-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenc
7、ed 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 regulatory ruleswhere earlier versions of the method(s) identified
8、may berequired.2.2 ASTM Standards:2D97 Test Method for Pour Point of Petroleum ProductsD 323 Test Method for Vapor Pressure of Petroleum Prod-ucts (Reid Method)D 4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD 4177 Practice for Automatic Sampling of Petroleum andPetroleum Produ
9、ctsD 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 of Petroleum Prod-ucts (Mini Method)D 5842 Practice for Sampling and Handling of Fuels fo
10、rVolatility MeasurementD 5949 Test Method for Pour Point of Petroleum Products(Automatic Pressure Pulsing Method)D 5950 Test Method for Pour Point of Petroleum Products(Automatic Tilt Method)D 5985 Test Method for Pour Point of Petroleum Products(Rotational Method)D 6300 Practice for Determination o
11、f Precision and BiasData for Use in Test Methods for Petroleum Products andLubricantsE1 Specification for ASTM Liquid-in-Glass ThermometersE77 Test Method for Inspection and Verification of Ther-mometersE 1272 Specification for Laboratory Glass Graduated Cyl-indersE 1405 Specification for Laboratory
12、 Glass DistillationFlasks2.3 Energy Institute Standards:3IP 69 Determination of Vapour PressureReid MethodIP 123 Petroleum ProductsDetermination of DistillationCharacteristicsIP 394 Determination of Air Saturated Vapour PressureIP Standard Methods for Analysis and Testing of Petroleumand Related Pro
13、ducts 1996Appendix A3. Terminology3.1 Definitions:1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.08 on Volatility.In the IP, the equivalent test method is published under the designation IP 123
14、.It is under the jurisdiction of the Standardization Committee.Current edition approved April 15, 2009. Published April 2009. Originallyapproved in 1921. Last previous edition approved in 2008 as D 8608a.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Se
15、rvice 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.energyinst.org.uk.1*A Summary of Changes section appears at the end o
16、f this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3.1.1 charge volume, nthe volume of the specimen, 100mL, charged to the distillation flask at the temperature speci-fied in Table 1.3.1.2 decomposition, nof a hydrocarbon
17、, the pyrolysis orcracking of a molecule yielding smaller molecules with lowerboiling points than the original molecule.3.1.2.1 DiscussionCharacteristic indications of thermaldecomposition are evolution of fumes and erratic temperaturereadings that usually decrease after any attempt is made toadjust
18、 the heat.3.1.3 decomposition point, nthe corrected thermometerreading that coincides with the first indications of thermaldecomposition of the liquid in the flask.3.1.3.1 DiscussionThe decomposition point, as deter-mined under the conditions of this test method, does notnecessarily correspond to th
19、e decomposition temperature inother applications.3.1.4 dry point, nthe corrected thermometer reading thatis observed at the instant the last drop of liquid (exclusive ofany drops or film of liquid on the side of the flask or on thetemperature sensor), evaporates from the lowest point in thedistillat
20、ion flask.3.1.4.1 DiscussionThe end point (final boiling point),rather than the dry point, is intended for general use. The drypoint can be reported in connection with special purposenaphthas, such as those used in the paint industry. Also, it issubstituted for the end point (final boiling point) wh
21、enever thesample is of such a nature that the precision of the end point(final boiling point) cannot consistently meet the requirementsgiven in the precision section.3.1.5 dynamic holdup, nthe amount of material present inthe neck of the flask, in the sidearm of the flask, and in thecondenser tube d
22、uring the distillation.3.1.6 emergent stem effect, nthe offset in temperaturereading caused by the use of total immersion mercury-in-glassthermometers in the partial immersion mode.3.1.6.1 DiscussionIn the partial immersion mode, a por-tion of the mercury thread, that is, the emergent portion, is at
23、a lower temperature than the immersed portion, resulting in ashrinkage of the mercury thread and a lower temperaturereading.3.1.7 end point (EP) or final boiling point (FBP), nthemaximum corrected thermometer reading obtained during thetest.3.1.7.1 DiscussionThis usually occurs after the evapora-tio
24、n of all liquid from the bottom of the flask. The termmaximum temperature is a frequently used synonym.3.1.8 front end loss, nloss due to evaporation duringtransfer from receiving cylinder to distillation flask, vapor lossduring the distillation, and uncondensed vapor in the flask atthe end of the d
25、istillation.3.1.9 initial boiling point (IBP), nthe corrected thermom-eter reading that is observed at the instant the first drop ofcondensate falls from the lower end of the condenser tube.3.1.10 percent evaporated, nthe sum of the percent re-covered and the percent loss.3.1.11 percent loss (or obs
26、erved loss), none hundredminus the percent total recovery.3.1.11.1 corrected loss, npercent loss corrected for baro-metric pressure.3.1.12 percent recovered, nthe volume of condensateobserved in the receiving cylinder, expressed as a percentage ofthe charge volume, associated with a simultaneous tem
27、peraturereading.3.1.13 percent recovery, nthe maximum percent recov-ered, as observed in accordance with 10.18.3.1.13.1 corrected percent recovery, nthe percent recov-ery, adjusted for the difference between the observed loss andthe corrected loss, as described in Eq 8.3.1.13.2 percent total recover
28、y, nthe combined percentrecovery and residue in the flask, as determined in accordancewith 11.1.3.1.14 percent residue, nthe volume of residue in theflask, measured in accordance with 10.19, and expressed as apercentage of the charge volume.3.1.15 rate of change (or slope), nthe change in tempera-tu
29、re reading per percent evaporated or recovered, as describedin 13.2.3.1.16 temperature lag, nthe offset between the tempera-ture reading obtained by a temperature sensing device and thetrue temperature at that time.3.1.17 temperature measurement device, na thermometer,as described in 6.3.1, or a tem
30、perature sensor, as described in6.3.2.3.1.18 temperature reading, nthe temperature obtained bya temperature measuring device or system that is equal to thethermometer reading described in 3.1.19.TABLE 1 Preparation of Apparatus and SpecimenGroup 1 Group 2 Group 3 Group 4Flask, mL 125 125 125 125ASTM
31、 distillation thermometer 7C (7F) 7C (7F) 7C (7F) 8C (8F)IP distillation thermometer range low low low highFlask support board B B C Cdiameter of hole, mm 38 38 50 50Temperature at start of testFlask C 1318 1318 1318 not aboveF 5565 5565 5565 ambientFlask support and shield not above not above not a
32、boveambient ambient ambientReceiving cylinder and sampleC 1318 1318 1318A13ambientAF 5565 5565 5565A55ambientAASee 10.3.1.1 for exceptions.D860923.1.18.1 corrected temperature reading, nthe temperaturereading, as described in 3.1.18, corrected for barometricpressure.3.1.19 thermometer reading (or th
33、ermometer result), nthetemperature of the saturated vapor measured in the neck of theflask below the vapor tube, as determined by the prescribedthermometer under the conditions of the test.3.1.19.1 corrected thermometer reading, nthe thermom-eter reading, as described in 3.1.19, corrected for barome
34、tricpressure.4. Summary of Test Method4.1 Based on its composition, vapor pressure, expected IBPor expected EP, or combination thereof, the sample is placed inone of four groups. Apparatus arrangement, condenser tem-perature, and other operational variables are defined by thegroup in which the sampl
35、e falls.4.2 A 100-mL specimen of the sample is distilled underprescribed conditions for the group in which the sample falls.The distillation is performed in a laboratory batch distillationunit at ambient pressure under conditions that are designed toprovide approximately one theoretical plate fracti
36、onation. Sys-tematic observations of temperature readings and volumes ofcondensate are made, depending on the needs of the user of thedata. The volume of the residue and the losses are alsorecorded.4.3 At the conclusion of the distillation, the observed vaportemperatures can be corrected for baromet
37、ric pressure and thedata are examined for conformance to procedural require-ments, such as distillation rates. The test is repeated if anyspecified condition has not been met.4.4 Test results are commonly expressed as percent evapo-rated or percent recovered versus corresponding temperature,either i
38、n a table or graphically, as a plot of the distillationcurve.5. Significance and Use5.1 The basic test method of determining the boiling rangeof a petroleum product by performing a simple batch distilla-tion has been in use as long as the petroleum industry hasexisted. It is one of the oldest test m
39、ethods under the jurisdic-tion of ASTM Committee D02, dating from the time when itwas still referred to as the Engler distillation. Since the testmethod has been in use for such an extended period, atremendous number of historical data bases exist for estimatingend-use sensitivity on products and pr
40、ocesses.5.2 The distillation (volatility) 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.
41、 Volatility is themajor determinant of the tendency of a hydrocarbon mixture toproduce potentially explosive vapors.5.3 The distillation characteristics are critically importantfor both automotive and aviation gasolines, affecting starting,warm-up, and tendency to vapor lock at high operatingtempera
42、ture 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.5.4 Volatility, as it affects rate of evaporation, is an impor-tant factor in the application of many solvents, parti
43、cularlythose used in paints.5.5 Distillation limits are often included in petroleum prod-uct specifications, in commercial contract agreements, processrefinery/control applications, and for compliance to regulatoryrules.6. Apparatus6.1 Basic Components of the Apparatus:6.1.1 The basic components of
44、the distillation unit are thedistillation flask, the condenser and associated cooling bath, ametal shield or enclosure for the distillation flask, the heatsource, the flask support, the temperature measuring device,and the receiving cylinder to collect the distillate.6.1.2 Figs. 1 and 2 are examples
45、 of manual distillation units.6.1.3 In addition to the basic components described in 6.1.1,automated units also are equipped with a system to measureand automatically record the temperature and the associatedrecovered volume in the receiving cylinder.6.2 Adetailed description of the apparatus is giv
46、en inAnnexA2.6.3 Temperature Measuring Device:6.3.1 Mercury-in-glass thermometers, if used, shall be filledwith an inert gas, graduated on the stem and enamel backed.They shall conform to Specification E1 or IP StandardMethods for Analysis and Testing of Petroleum and RelatedProducts 1996AppendixA,
47、or both, for thermometersASTM7C/IP 5C and ASTM 7F for the low range thermometers, andASTM 8C/IP 6C and ASTM 8F for the high range thermom-eters.FIG. 1 Apparatus Assembly Using Gas BurnerD860931Condenser bath 11Distillation flask2Bath cover 12Temperature sensor3Bath temperature sensor 13Flask support
48、 board4Bath overflow 14Flask support platform5Bath drain 15Ground connection6Condenser tube 16Electric heater7Shield 17Knob for adjusting level8Viewing window of support platform9aVoltage regulator 18Power source cord9bVoltmeter or ammeter 19Receiver cylinder9cPower switch 20Receiver cooling bath9dP
49、ower light indicator 21Receiver cover10VentFIG. 2 Apparatus Assembly Using Electric HeaterD860946.3.1.1 Thermometers that have been exposed for an ex-tended period above an observed temperature of 370C shallnot be reused without a verification of the ice point or checkedas prescribed in Specification E1and Test Method E77.NOTE 1At an observed thermometer reading of 370C, the tempera-ture of the bulb is approaching a critical range in the glass and thethermometer may lose its calibration.6.3.2 Temperature
