1、Designation: D1160 13D1160 15Standard 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 U.S. Department of Defense.1. Scope*1.1 This test method covers the determi
3、nation, 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.400 C. Both a manual methodand an automatic method are specified.1.2 In cases of dispute, the referee test method is
4、the manual 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 resp
5、onsibilityof 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 Ce
6、tane Number 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 Densit
7、y, and API 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 Produ
8、cts and Lubricants3. 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 atmosphe
9、ric pressure 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 o
10、f the condenser 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 j
11、urisdiction ofASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of SubcommitteeD02.08 on Volatility.Current edition approved Oct. 1, 2013Feb. 1, 2015. Published October 2013February 2015. Originally approved in 1951. Last previous edition approve
12、d in 20122013 asD1160 12.D1160 13. DOI: 10.1520/D1160-13.10.1520/D1160-15.2 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
13、ASTM 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 cons
14、ult prior 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,
15、 PA 19428-2959. 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 an
16、d 6.7 kPa (1 0.13 kPa and 6.7 kPa (1 mm and50 mm Hg) under conditions that are designed to provide approximately one theoretical plate fractionation. Data are obtained fromwhich the initial boiling point, the final boiling point, and a distillation curve relating volume percent distilled and atmosph
17、ericequivalent boiling point temperature can be prepared.5. Significance and Use5.1 This test method is used for the determination of the distillation characteristics of petroleum products, biodiesel, andfractions that may decompose if distilled at atmospheric pressure. This boiling range, obtained
18、at conditions designed 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
19、 as feed to a refining 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 s
20、uitability of theproduct 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 cur
21、rent engineering practice.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 forobtainin
22、g satisfactory results 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
23、automatic apparatus can 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,gauge, would require vapor protection.FIG. 1 Assembly of Vacuum Distillation ApparatusD1160 152
24、6.1.1 Distillation Flask, of 500-mL500 mLcapacity, made of borosilicate glass or of quartz conforming to the dimensions givenin Fig. 2 or Fig. 3, and having a heating mantle with insulating top. These dimensions can vary slightly by manufacturer, and arenot considered critical dimensions, with the e
25、xception of the position of the end 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 nec
26、k is present on commercially availableflasks 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 completel
27、y silvered glass vacuumjacket with a permanent vacuum of less than 105 Pa Pa (107 mm mm Hg) (Note 1). The attached condenser section shall beenclosed in water jackets as illustrated and have an adapter at the top for connection to the vacuum source.Alight drip-chain shallhang from the drip tip of th
28、e condenser to a point 5 mm 5 mm below the 10-mL10 mL mark of the receiver as shown in Fig. 5.Alternatively, instead of the metal drip-chain, a metal trough may be used to channel the distillate to the wall of the receiver. Thistrough may either be attached to the condenser drip tip as shown in Fig.
29、 5 or it may also be located in the neck of the receiver.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 read
30、ily detectable by sight alone will negate the vacuumin 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 60.5C60.5 C over the r
31、ange00 C to 400C400 C and have a response time of less than 200 s 200 s as described in Annex A2. The location of the vaportemperature sensor is extremely critical.As shown in Fig. 6, the vapor temperature measuring device shall be centered in the upperportion of the distillation column with the top
32、 of the sensing tip 33 mm 6 1 mm 1 mm below the spillover point (see 3.1). Thevapor temperature measuring device can consist of 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
33、of these two types in relation to the spilloverpoint. In glass platinum resistance devices the top of the spiral winding is the top of the sensing tip, in thermocouples it is the topof the thermocouple junction, in metal jacketed devices it is 11 mm 6 1 mm 1 mm above the bottom of the device. An ali
34、gnmentprocedure is described in Appendix X1. The vapor temperature measuring device shall be mounted through a compression ringtype seal mounted on the top of the glass temperature sensor/vacuum adapter or fused into a ground taper joint matched to thedistillation column. In some distillation appara
35、tus configurations, the vacuum adapter at the top of the distillation column can beomitted. In these cases, the position of the vapor temperature measuring device shall be adjusted accordingly. The boilertemperature measuring device may be either a thermocouple or PRT and shall also be calibrated as
36、 above.FIG. 2 Distillation Flask and Heating MantleD1160 1536.1.4 Receiver of borosilicate 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
37、are subjectedto severe thermal conditions and, to lessen the chances of failure during a test, only equipment shown to be strain-free underpolarized light should be used.)6.1.5 Vacuum Gage,Gauge, capable of measuring absolute pressures with an accuracy of 0.01 kPa 0.01 kPa in the range below1 kPa 1
38、kPa absolute and with an accuracy of 1 % above this pressure. The McLeod gage non-tilting McLeod gauge or otheranalogous primary standard pressure device can achieve this accuracy when properly used, but a mercury manometer will permitthis accuracy only down to a pressure of about 1 kPa 1 kPa and th
39、en only when read with a good cathetometer (an instrument basedon a telescope mounted on a vernier scale to determine levels very accurately). An electronic gage such as the Baratron issatisfactory when calibrated from a McLeod gage but must be rechecked periodically asCertified electronic sensors m
40、ay be used,provided the calibration of the sensor and its associated recording instrument can be traced back to a primary pressure standard.A basic calibration procedure is described in Annex A3. A suitable pressure calibration setup is illustrated in Fig. A3.1. Vacuumgagesgauges based on hot wires,
41、 radiation, or conductivity detectors are not recommended.NOTE 2Suitable instruments for measuring 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
42、vacuum gagegauge to the side tube of the temperature sensor/vacuum adapter of the distillation column(preferred location) or to the side tube of the sensor/vacuum adapter of the condenser when assembling the apparatus. Connectionsshall be as short in length as possible and have an inside diameter no
43、t less than 8 mm.6.1.6 Pressure Regulating System, capable of maintaining the pressure of the system constant within 0.01 kPa 0.01 kPa atpressures of 1 kPa 1 kPa absolute and below and within 1 % of the absolute pressure at 1 kPa 1 kPa or higher. Suitable equipmentfor this purpose is described in An
44、nex A4. Connect the pressure regulating system to the tube at the top of the condenser whenassembling the apparatus. Connections shall be as short in length as possible and have an inside diameter not less than 8 mm.8 mm.6.1.7 Vacuum Source, consisting of, for example, one or more vacuum pumps and s
45、everal surge tanks, capable of maintainingthe pressure constant within 1 % over the full range of operating pressures. A vacuum adapter is used to connect the source to theFIG. 3 Distillation Flask 500 MLD1160 154top of the condenser (Fig. 1) with tubing of 8 mm 8 mm ID or larger and as short as pra
46、ctical. A single stage pump with a typicalcapacity of 8585 Lmin to 130130 L L/min (3 to 4.6 cfm) capacity at 100 kPa min (3 cfm to 4.6 cfm) capacity at 100 kPa issuitable as a vacuum source, but a double stage pump of similar or better capacity is recommended if distillations are to beperformed belo
47、w 0.5 kPa. 0.5 kPa. Surge tanks of at least 5 L 5 L capacity are recommended to reduce pressure fluctuations.6.1.8 Cold Traps:6.1.8.1 Cold trap mounted between the top of the condenser and the vacuum source to recover the light boiling components inthe distillate that are not condensed in the conden
48、ser section. This trap shall be cooled with a coolant capable of maintaining thetemperature of the trap below 40C.below 40 C. Liquid nitrogen is commonly used for this purpose. (WarningIf there isa large air leak in the system and liquid nitrogen is used as the coolant, it is possible to condense ai
49、r (oxygen) in the trap. Ifhydrocarbons are also present 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 and the vacuum gagegauge to protect the gagegaugefrom contamination 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 Screen or Safety Enclosure that ade
