1、Designation: D1160 12D1160 13Standard 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
2、 revision. 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 Department of Defense.1. Scope*1.1 This test method covers the determinatio
3、n, at reduced pressures, of the range of boiling points for petroleum products andbiodiesel that can be partially or completely vaporized at a maximum liquid temperature of 400C. Both a manual method and anautomatic method are specified.1.2 In cases of dispute, the referee test method is the manual
4、test method at a mutually agreed upon pressure.1.3 The values stated in SI units are to be regarded as the standard. The values in parentheses are for information only.1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityo
5、f the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use. For specific warning statements, see 6.1.4, 6.1.8.1, 10.11, and A3.2.1.2. Referenced Documents2.1 ASTM Standards:2D613 Test Method for Cetane Number
6、 of Diesel Fuel OilD1193 Specification for Reagent WaterD1250 Guide for Use of the Petroleum Measurement TablesD1298 Test Method for Density, Relative Density, or API Gravity of Crude Petroleum and Liquid Petroleum Products byHydrometer MethodD4052 Test Method for Density, Relative Density, and API
7、Gravity of Liquids by Digital Density MeterD4057 Practice for Manual Sampling of Petroleum and Petroleum ProductsD4177 Practice for Automatic Sampling of Petroleum and Petroleum ProductsD6300 Practice for Determination of Precision and Bias Data for Use in Test Methods for Petroleum Products and Lub
8、ricants3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 atmospheric equivalent temperature (AET), nthe temperature converted from the measured vapor temperature using EqA7.1. The AET is the expected distillate temperature if the distillation was performed at atmospheric pressur
9、e and there was nothermal decomposition.3.1.2 end point (EP) or final boiling point (FBP),nthe maximum vapor temperature reached during the test.3.1.3 initial boiling point (IBP), nthe vapor temperature that is measured at the instant the first drop of condensate falls fromthe lower end of the conde
10、nser section drip tip.3.1.3.1 DiscussionWhen a chain is attached to the drip tip the first drop will form and run down the chain. In automatic apparatus, the first dropdetection device shall be located as near to the lower end of the drip tip as practical.1 This test method is under the jurisdiction
11、 of ASTM Committee D02 on Petroleum Products Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.08 on Volatility.Current edition approved Dec. 1, 2012Oct. 1, 2013. Published March 2013October 2013. Originally approved in 1951. Last previous edition approved in
12、 20062012 asD1160D1160 12.06. DOI: 10.1520/D1160-12.10.1520/D1160-13.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM
13、website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult p
14、rior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 1
15、9428-2959. United States13.1.4 spillover point, nthe highest point of the lower internal junction of the distillation column and the condensing sectionof the vacuum-jacketed column assembly.4. Summary of Test Method4.1 The sample is distilled at an accurately controlled pressure between 0.13 and 6.7
16、 kPa (1 and 50 mm Hg) under conditionsthat are designed to provide approximately one theoretical plate fractionation. Data are obtained from which the initial boilingpoint, the final boiling point, and a distillation curve relating volume percent distilled and atmospheric equivalent boiling pointtem
17、perature can be prepared.5. Significance and Use5.1 This test method is used for the determination of the distillation characteristics of petroleum products products, biodiesel,and fractions that may decompose if distilled at atmospheric pressure. This boiling range, obtained at conditions designed
18、to obtainapproximately one theoretical plate fractionation, can be used in engineering calculations to design distillation equipment, toprepare appropriate blends for industrial purposes, to determine compliance with regulatory rules, to determine the suitability ofthe product as feed to a refining
19、process, or for a host of other purposes.5.2 The boiling range is directly related to viscosity, vapor pressure, heating value, average molecular weight, and many otherchemical, physical, and mechanical properties. Any of these properties can be the determining factor in the suitability of theproduc
20、t in its intended application.5.3 Petroleum product specifications often include distillation limits based on data by this test method.5.4 Many engineering design correlations have been developed on data by this test method. These correlative methods are usedextensively in current engineering practi
21、ce.6. Apparatus6.1 The vacuum distillation apparatus, shown schematically in Fig. 1, consists in part of the components described below plusothers that appear in Fig. 1 but are not specified, either as to design or performance. Some of these parts are not essential forobtaining satisfactory results
22、from the tests but are desirable components of the assembly for the purpose of promoting the efficientuse of the apparatus and ease of its operation. Both manual and automatic versions of the apparatus must conform to the followingrequirements. Additional requirements for the automatic apparatus can
23、 be found in Annex A9.NOTE 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 gage, would require vapor protection.FIG. 1 Assembly of Vacuum Distillation ApparatusD1160 1326.1.1 Distillation Flask, of
24、500-mL capacity, made of borosilicate glass or of quartz conforming to the dimensions given in Fig.2 or Fig. 3, and having a heating mantle with insulating top. These dimensions can vary slightly by manufacturer, and are notconsidered critical dimensions, with the exception of the position of the en
25、d of the temperature sensing probe, and the innerdiameter of the connection to the distillation column not being less than the inner diameter of the distillation column. The use ofthe thermowell can be replaced by an encased temperature probe and the second side neck is present on commercially avail
26、ableflasks used in this test method.6.1.2 Vacuum-Jacketed Column Assembly, of borosilicate glass, consisting of a distilling head and an associated condensersection as illustrated in the lettered drawing, Fig. 4 and Table 1. The head shall be enclosed in a completely silvered glass vacuumjacket with
27、 a permanent vacuum of less than 105 Pa (107 mm Hg) (Note 1). The attached condenser section shall be enclosedin water jackets as illustrated and have an adapter at the top for connection to the vacuum source. A light drip-chain shall hangfrom the drip tip of the condenser to a point 5 mm below the
28、10-mL mark of the receiver as shown in Fig. 5.Alternatively, insteadof the metal drip-chain, a metal trough may be used to channel the distillate to the wall of the receiver. This trough may either beattached to the condenser drip tip as shown in Fig. 5 or it may also be located in the neck of the r
29、eceiver.NOTE 1There is no simple method to determine the vacuum in the jacket once it is completely sealed. A Tesla coil can be used, but the spark canactually create a pinhole in a weak spot in the jacket. Even the slightest pinhole or crack not readily detectable by sight alone will negate the vac
30、uumin the jacket.6.1.3 Vapor Temperature Measuring Device and associated signal conditioning and processing instruments (Annex A1) for themeasurement of the vapor temperature. The system must produce readings with an accuracy of 60.5C over the range 0 to 400Cand have a response time of less than 200
31、 s as described in Annex A2. The location of the vapor temperature sensor is extremelycritical.As shown in Fig. 6, the vapor temperature measuring device shall be centered in the upper portion of the distillation columnwith the top of the sensing tip 3 6 1 mm below the spillover point (see 3.1). The
32、 vapor temperature measuring device can consistof different configurations depending if it is a platinum resistance in glass or metal, or if it is a thermocouple in glass or metal.Figs. 7 and 8 show the proper positioning of these two types in relation to the spillover point. In glass platinum resis
33、tance devicesthe top of the spiral winding is the top of the sensing tip, in thermocouples it is the top of the thermocouple junction, in metaljacketed devices it is 1 6 1 mm above the bottom of the device. An alignment procedure is described in Appendix X1. The vaportemperature measuring device sha
34、ll be mounted through a compression ring type seal mounted on the top of the glass temperaturesensor/vacuum adapter or fused into a ground taper joint matched to the distillation column. In some distillation apparatusconfigurations, the vacuum adapter at the top of the distillation column can be omi
35、tted. In these cases, the position of the vaportemperature measuring device shall be adjusted accordingly. The boiler temperature measuring device may be either athermocouple or PRT and shall also be calibrated as above.FIG. 2 Distillation Flask and Heating MantleD1160 1336.1.4 Receiver of borosilic
36、ate glass, conforming to the dimensions shown in Fig. 9. If the receiver is part of an automatic unitand is mounted in a thermostatted chamber, the jacket is not required. (WarningThe glass parts of the apparatus are subjectedto severe thermal conditions and, to lessen the chances of failure during
37、a test, only equipment shown to be strain-free underpolarized light should be used.)6.1.5 Vacuum Gage, capable of measuring absolute pressures with an accuracy of 0.01 kPa in the range below 1 kPa absoluteand with an accuracy of 1 % above this pressure. The McLeod gage can achieve this accuracy when
38、 properly used, but a mercurymanometer will permit this accuracy only down to a pressure of about 1 kPa and then only when read with a good cathetometer(an instrument based on a telescope mounted on a vernier scale to determine levels very accurately). An electronic gage such asthe Baratron is satis
39、factory when calibrated from a McLeod gage but must be rechecked periodically as described in Annex A3.A suitable pressure calibration setup is illustrated in Fig. A3.1. Vacuum gages based on hot wires, radiation, or conductivitydetectors are not recommended.NOTE 2Suitable instruments for measuring
40、the pressure of the system during the test are the tensimeter or an electronic pressure gage, provided theoutput is traceable to a primary gage, such as the non-tilting McLeod gage.6.1.5.1 Connect the vacuum gage to the side tube of the temperature sensor/vacuum adapter of the distillation column (p
41、referredlocation) or to the side tube of the sensor/vacuum adapter of the condenser when assembling the apparatus. Connections shall beas short in length as possible and have an inside diameter not less than 8 mm.6.1.6 Pressure Regulating System, capable of maintaining the pressure of the system con
42、stant within 0.01 kPa at pressures of1 kPa absolute and below and within 1 % of the absolute pressure at 1 kPa or higher. Suitable equipment for this purpose isdescribed in Annex A4. Connect the pressure regulating system to the tube at the top of the condenser when assembling theapparatus. Connecti
43、ons shall be as short in length as possible and have an inside diameter not less than 8 mm.6.1.7 Vacuum Source, consisting of, for example, one or more vacuum pumps and several surge tanks, capable of maintainingthe pressure constant within 1 % over the full range of operating pressures. A vacuum ad
44、apter is used to connect the source to thetop of the condenser (Fig. 1) with tubing of 8 mm ID or larger and as short as practical.Asingle stage pump with a typical capacityFIG. 3 Distillation Flask 500 MLD1160 134of 85 to 130 L/min (3 to 4.6 cfm) capacity at 100 kPa is suitable as a vacuum source,
45、but a double stage pump of similar or bettercapacity is recommended if distillations are to be performed below 0.5 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 condenser and the vacuum sourc
46、e to recover the light boiling components inthe distillate that are not condensed in the condenser section. This trap shall be cooled with a coolant capable of maintaining thetemperature of the trap below 40C. Liquid nitrogen is commonly used for this purpose. (Warning If there is a large air leakin
47、 the system and liquid nitrogen is used as the coolant, it is possible to condense air (oxygen) in the trap. If hydrocarbons are alsopresent in the trap, a fire or explosion can result when the trap is warmed up in step 10.12.)6.1.8.2 Cold trap mounted between the temperature sensor/vacuum adapter a
48、nd the vacuum gage to protect the gage fromcontamination by low boiling components in the distillate.6.1.9 Low Pressure Air or Carbon Dioxide Source to cool the flask and heater at the end of the distillation.6.1.10 Low Pressure Nitrogen Source to release the vacuum in the system.6.1.11 Safety Scree
49、n or Safety Enclosure that adequately shields the operator from the distillation apparatus in the event ofmishap. Reinforced glass, 6 mm thick clear plexiglass, or a clear material of equivalent strength is recommended.6.1.12 Coolant Circulating System, capable of supplying coolant to the receiver and condenser system, at a temperaturecontrolled within 63C in the range between 30 and 80C. For automatic units where the receiver is mounted in a thermostattedchamber, the coolant circulating system has to be capable of supplying coolant to the condenser system
