1、Designation: D1160 18Standard Test Method forDistillation of Petroleum Products at Reduced Pressure1This standard is issued under the fixed designation D1160; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revisio
2、n. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the U.S. Department of Defense.1. Scope*1.1 This test method covers the determination,
3、at reducedpressures, of the range of boiling points for petroleum productsand biodiesel that can be partially or completely vaporized at amaximum liquid temperature of 400 C. Both a manual methodand an automatic method are specified.1.2 In cases of dispute, the referee test method is the manualtest
4、method at a mutually agreed upon pressure.1.3 The values stated in SI units are to be regarded asstandard. The values given in parentheses after SI units areprovided for information only and are not considered standard.1.4 This standard does not purport to address all of thesafety concerns, if any,
5、associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to use.For specific warning statements, see 6.1.4, 6.1.8.1, 10.11, andA3.2.1.1.5 This i
6、nternational standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TB
7、T) Committee.2. Referenced Documents2.1 ASTM Standards:2D613 Test Method for Cetane Number of Diesel Fuel OilD1193 Specification for Reagent WaterD1250 Guide for Use of the Petroleum Measurement TablesD1298 Test Method for Density, Relative Density, or APIGravity of Crude Petroleum and Liquid Petrol
8、eum Prod-ucts by Hydrometer MethodD4052 Test Method for Density, Relative Density, and APIGravity of Liquids by Digital Density MeterD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD6300 Practice for Determi
9、nation of Precision and BiasData for Use in Test Methods for Petroleum Products andLubricants3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 atmospheric equivalent temperature (AET), nthetemperature converted from the measured vapor temperatureusing Eq A7.1. The AET is the exp
10、ected distillate temperatureif the distillation was performed at atmospheric pressure andthere was no thermal decomposition.3.1.2 end point (EP) or final boiling point (FBP), nthemaximum vapor temperature reached during the test.3.1.3 initial boiling point (IBP), nthe vapor temperaturethat is measur
11、ed at the instant the first drop of condensate fallsfrom the lower end of the condenser section drip tip.3.1.3.1 DiscussionWhen a chain is attached to the drip tipthe first drop will form and run down the chain. In automaticapparatus, the first drop detection device shall be located asnear to the lo
12、wer end of the drip tip as practical.3.1.4 spillover point, nthe highest point of the lowerinternal junction of the distillation column and the condensingsection of the vacuum-jacketed column assembly.4. Summary of Test Method4.1 The sample is distilled at an accurately controlledpressure between 0.
13、13 kPa and 6.7 kPa (1 mm and 50 mm Hg)under conditions that are designed to provide approximatelyone theoretical plate fractionation. Data are obtained fromwhich the initial boiling point, the final boiling point, and adistillation curve relating volume percent distilled and atmo-spheric equivalent
14、boiling point temperature can be prepared.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.08 on Volatility.Current edition approved July 1, 2018. Published August 2018. Originally
15、approved in 1951. Last previous edition approved in 2015 as D1160 15. DOI:10.1520/D1160-18.2For referenced ASTM standards, 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 Su
16、mmary page onthe ASTM website.*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 StatesThis international standard was developed in accordance with internationally recognized prin
17、ciples on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.15. Significance and Use5.1 This test method is used for the determination
18、of thedistillation characteristics of petroleum products, biodiesel, andfractions that may decompose if distilled at atmosphericpressure. This boiling range, obtained at conditions designed toobtain approximately one theoretical plate fractionation, can beused in engineering calculations to design d
19、istillationequipment, to prepare appropriate blends for industrialpurposes, to determine compliance with regulatory rules, todetermine the suitability of the product as feed to a refiningprocess, or for a host of other purposes.5.2 The boiling range is directly related to viscosity, vaporpressure, h
20、eating value, average molecular weight, and manyother chemical, physical, and mechanical properties. Any ofthese properties can be the determining factor in the suitabilityof the product in its intended application.5.3 Petroleum product specifications often include distilla-tion limits based on data
21、 by this test method.5.4 Many engineering design correlations have been devel-oped on data by this test method.These correlative methods areused extensively in current engineering practice.6. Apparatus6.1 The vacuum distillation apparatus, shown schematicallyin Fig. 1, consists in part of the compon
22、ents described belowplus others that appear in Fig. 1 but are not specified, either asto design or performance. Some of these parts are not essentialfor obtaining satisfactory results from the tests but are desirablecomponents of the assembly for the purpose of promoting theefficient use of the appa
23、ratus and ease of its operation. Bothmanual and automatic versions of the apparatus must conformto the following requirements. Additional requirements for theautomatic apparatus can be found in Annex A9.6.1.1 Distillation Flask, of 500 mL capacity, made of boro-silicate glass or of quartz conforming
24、 to the dimensions givenin Fig. 2 or Fig. 3, and having a heating mantle with insulatingtop. These dimensions can vary slightly by manufacturer, andare not considered critical dimensions, with the exception ofthe position of the end of the temperature sensing probe, andthe inner diameter of the conn
25、ection to the distillation columnnot being less than the inner diameter of the distillationcolumn. The use of the thermowell can be replaced by anencased temperature probe and the second side neck is presenton commercially available flasks used in this test method.6.1.2 Vacuum-Jacketed Column Assemb
26、ly, of borosilicateglass, consisting of a distilling head and an associated con-denser section as illustrated in the lettered drawing, Fig. 4 andTable 1. The head shall be enclosed in a completely silveredglass vacuum jacket with a permanent vacuum of less than105Pa (107mm Hg) (Note 1). The attached
27、 condensersection shall be enclosed in water jackets as illustrated andhave an adapter at the top for connection to the vacuum source.Alight drip-chain shall hang from the drip tip of the condenserto a point 5 mm below the 10 mL mark of the receiver asshown in Fig. 5. Alternatively, instead of the m
28、etal drip-chain,a metal trough may be used to channel the distillate to the wallof the receiver. This trough may either be attached to theNOTE 1A cold trap can be inserted before the pressure transducer in Option No. 2, if desired, or if the design of the transducer, such as a mercuryMcCleod gauge,
29、would require vapor protection.FIG. 1 Assembly of Vacuum Distillation ApparatusD1160 182condenser drip tip as shown in Fig. 5 or it may also be locatedin the neck of the receiver.NOTE 1There is no simple method to determine the vacuum in thejacket once it is completely sealed. ATesla coil can be use
30、d, but the sparkcan actually create a pinhole in a weak spot in the jacket. Even theslightest pinhole or crack not readily detectable by sight alone will negatethe vacuum in the jacket.6.1.3 Vapor Temperature Measuring Device and associatedsignal conditioning and processing instruments (AnnexA1) for
31、the measurement of the vapor temperature. The system mustproduce readings with an accuracy of 60.5 C over the range0 C to 400 C and have a response time of less than 200 s asdescribed in Annex A2. The location of the vapor temperaturesensor is extremely critical. As shown in Fig. 6, the vaportempera
32、ture measuring device shall be centered in the upperportion of the distillation column with the top of the sensing tip3mm6 1 mm below the spillover point (see 3.1). The vaportemperature measuring device can consist of different configu-rations depending if it is a platinum resistance in glass or met
33、al,or if it is a thermocouple in glass or metal. Figs. 7 and 8 showthe proper positioning of these two types in relation to thespillover point. In glass platinum resistance devices the top ofthe spiral winding is the top of the sensing tip, in thermo-couples it is the top of the thermocouple junctio
34、n, in metaljacketed devices it is 1 mm 6 1 mm above the bottom of thedevice. An alignment procedure is described in Appendix X1.The vapor temperature measuring device shall be mountedthrough a compression ring type seal mounted on the top of theglass temperature sensor/vacuum adapter or fused into a
35、ground taper joint matched to the distillation column. In somedistillation apparatus configurations, the vacuum adapter at thetop of the distillation column can be omitted. In these cases, theposition of the vapor temperature measuring device shall beadjusted accordingly. The boiler temperature meas
36、uring devicemay be either a thermocouple or PRT and shall also becalibrated as above.6.1.4 Receiver of borosilicate glass, conforming to thedimensions shown in Fig. 9. If the receiver is part of anautomatic unit and is mounted in a thermostatted chamber, thejacket is not required. (WarningThe glass
37、parts of theapparatus are subjected to severe thermal conditions and, tolessen the chances of failure during a test, only equipmentshown to be strain-free under polarized light should be used.)6.1.5 Vacuum Gauge, capable of measuring absolute pres-sures with an accuracy of 0.01 kPa in the range belo
38、w 1 kPaabsolute and with an accuracy of 1 % above this pressure. Thenon-tilting McLeod gauge or other analogous primary standardpressure device can achieve this accuracy when properly used,but a mercury manometer will permit this accuracy only downto a pressure of about 1 kPa and then only when read
39、 with agood cathetometer (an instrument based on a telescopemounted on a vernier scale to determine levels very accu-rately). Certified electronic sensors may be used, provided thecalibration of the sensor and its associated recording instru-ment can be traced back to a primary pressure standard.Aba
40、siccalibration procedure is described in Annex A3. Vacuumgauges based on hot wires, radiation, or conductivity detectorsare not recommended.6.1.5.1 Connect the vacuum gauge to the side tube of thetemperature sensor/vacuum adapter of the distillation column(preferred location) or to the side tube of
41、the sensor/vacuumadapter of the condenser when assembling the apparatus.Connections shall be as short in length as possible and have aninside diameter not less than 8 mm.FIG. 2 Distillation Flask and Heating MantleD1160 1836.1.6 Pressure Regulating System, capable of maintainingthe pressure of the s
42、ystem constant within 0.01 kPa at pressuresof 1 kPa absolute and below and within 1 % of the absolutepressure at 1 kPa or higher. Suitable equipment for this purposeis described in Annex A4. Connect the pressure regulatingsystem to the tube at the top of the condenser when assemblingthe apparatus. C
43、onnections shall be as short in length aspossible and have an inside diameter not less than 8 mm.6.1.7 Vacuum Source, consisting of, for example, one ormore vacuum pumps and several surge tanks, capable ofmaintaining the pressure constant within 1 % over the fullrange of operating pressures. A vacuu
44、m adapter is used toconnect the source to the top of the condenser (Fig. 1) withtubing of 8 mm ID or larger and as short as practical. A singlestage pump with a typical capacity of 85 Lmin to 130 Lmin(3 cfm to 4.6 cfm) capacity at 100 kPa is suitable as a vacuumsource, but a double stage pump of sim
45、ilar or better capacity isrecommended if distillations are to be performed below0.5 kPa. Surge tanks of at least 5 L capacity are recommendedto reduce pressure fluctuations.6.1.8 Cold Traps:6.1.8.1 Cold trap mounted between the top of the condenserand the vacuum source to recover the light boiling c
46、omponentsin the distillate that are not condensed in the condenser section.This trap shall be cooled with a coolant capable of maintainingthe temperature of the trap below 40 C. Liquid nitrogen iscommonly used for this purpose. (WarningIf there is a largeair leak in the system and liquid nitrogen is
47、 used as the coolant,it is possible to condense air (oxygen) in the trap. If hydrocar-bons are also present in the trap, a fire or explosion can resultwhen the trap is warmed up in step 10.12.)6.1.8.2 Cold trap mounted between the temperature sensor/vacuum adapter and the vacuum gauge to protect the
48、 gaugefrom contamination by low boiling components in the distil-late.6.1.9 Low Pressure Air or Carbon Dioxide Source to coolthe flask and heater at the end of the distillation.6.1.10 Low Pressure Nitrogen Source to release the vacuumin the system.6.1.11 Safety Screen or Safety Enclosure that adequa
49、telyshields the operator from the distillation apparatus in the eventof mishap. Reinforced glass, 6 mm thick clear plexiglass, or aclear material of equivalent strength is recommended.6.1.12 Coolant Circulating System, capable of supplyingcoolant to the receiver and condenser system, at a temperaturecontrolled within 63 C in the range between 30 C and 80 C.For automatic units where the receiver is mounted in athermostatted chamber, the coolant circulating system has to becapable of supplying coolant to the condenser system only.FIG. 3 Distillation Flask 500 M
