1、Designation: D 1160 06An American National StandardStandard Test Method forDistillation of Petroleum Products at Reduced Pressure1This standard is issued under the fixed designation D 1160; the number immediately following the designation indicates the year oforiginal adoption or, in the case of rev
2、ision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) 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 determination, at reducedpressures, of the range of boiling points for petroleum productsthat can be partially or completely vaporized at a maximumliquid temperature of 400C. Both a manual method and anautomatic method are specified.1.2 In cases of dispute, the referee test method is the
4、 manualtest method at a mutually agreed upon pressure.1.3 The values stated in SI units are to be regarded as thestandard. The values in parentheses are for information only.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibil
5、ity 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. For specific hazardstatements, see 6.1.4, 6.1.8.1, 10.11, and A3.2.1.2. Referenced Documents22.1 ASTM Standards:D 613 Test Method for Cetane
6、 Number of Diesel Fuel OilD 1193 Specification for Reagent WaterD 1250 Guide for Use of the Petroleum MeasurementTablesD 1298 Test Method for Density, Relative Density (SpecificGravity), or API Gravity of Crude Petroleum and LiquidPetroleum Products by Hydrometer MethodD 4052 Test Method for Density
7、 and Relative Density ofLiquids by Digital Density MeterD 4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD 4177 Practice for Automatic Sampling of Petroleum andPetroleum Products3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 atmospheric equivalent tempera
8、ture (AET)the tem-perature converted from the measured vapor temperature usingEq A7.1. The AET is the expected distillate temperature if thedistillation was performed at atmospheric pressure and therewas no thermal decomposition.3.1.2 end point (EP) or final boiling point (FBP)themaximum vapor tempe
9、rature reached during the test.3.1.3 initial boiling point (IBP)the vapor temperature thatis measured at the instant the first drop of condensate falls fromthe 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
10、the chain. In automaticapparatus, the first drop detection device shall be located asnear to the lower end of the drip tip as practical.3.1.4 spillover pointthe highest point of the lower internaljunction of the distillation column and the condensing sectionof the vacuum-jacketed column assembly.4.
11、Summary of Test Method4.1 The sample is distilled at an accurately controlledpressure between 0.13 and 6.7 kPa (1 and 50 mm Hg) underconditions that are designed to provide approximately onetheoretical plate fractionation. Data are obtained from whichthe initial boiling point, the final boiling poin
12、t, and a distillationcurve relating volume percent distilled and atmosphericequivalent boiling point temperature can be prepared.5. Significance and Use5.1 This test method is used for the determination of thedistillation characteristics of petroleum products and fractionsthat may decompose if disti
13、lled at atmospheric pressure. Thisboiling range, obtained at conditions designed to obtain ap-proximately one theoretical plate fractionation, can be used inengineering calculations to design distillation equipment, toprepare appropriate blends for industrial purposes, to deter-mine compliance with
14、regulatory rules, to determine thesuitability of the product as feed to a refining process, or for ahost of other purposes.5.2 The boiling range is directly related to viscosity, vaporpressure, heating value, average molecular weight, and many1This test method is under the jurisdiction of ASTM Commi
15、ttee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.08 on Volatility.Current edition approved July 1, 2006. Published July 2006. Originally approvedin 1951. Last previous edition approved in 2003 as D 116003.2For referenced ASTM standards, visit the ASTM
16、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.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Ha
17、rbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.other 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-
18、tion limits based on data 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, consi
19、sts in part of the components 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 the
20、efficient use of the apparatus 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 glas
21、s or of quartz conforming 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 i
22、nner diameter of the connection 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 Vacu
23、um-Jacketed Column Assembly, 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 H
24、g) (Note 1). The attached 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. Altern
25、atively, instead of the metal drip-chain,a metal trough may be used to channel the distillate to the wallof the receiver. This trough may either be attached to thecondenser 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 t
26、he vacuum in thejacket once it is completely sealed.ATesla coil can be used, 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.NOTEA cold trap can be inserted before th
27、e 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 ApparatusD11600626.1.3 Vapor Temperature Measuring Device and associatedsignal conditioning and processing instr
28、uments (AnnexA1) forthe measurement of the vapor temperature. The system mustproduce readings with an accuracy of 60.5C over the range 0FIG. 2 Distillation Flask and Heating MantleFIG. 3 Distillation Flask 500MLD1160063to 400C and have a response time of less than 200 s asdescribed in Annex A2. The
29、location of the vapor temperaturesensor is extremely critical. As shown in Fig. 6, the vaportemperature measuring device shall be centered in the upperportion of the distillation column with the top of the sensing tip3 6 1 mm below the spillover point (see 3.1). The vaportemperature measuring device
30、 can consist of different configu-rations 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 showthe proper positioning of these two types in relation to thespillover point. In glass platinum resistance devices the top ofthe spiral
31、winding is the top of the sensing tip, in thermo-couples 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. Thevapor temperature measuring device shall be mounted througha compression
32、ring type seal mounted on the top of the glasstemperature sensor/vacuum adapter or fused into a groundtaper joint matched to the distillation column. In some distil-lation apparatus configurations, the vacuum adapter at the topof the distillation column can be omitted. In these cases, theposition of
33、 the vapor temperature measuring device shall beadjusted accordingly. The boiler temperature measuring devicemay be either a thermocouple or PRT and shall also becalibrated as above.6.1.4 Receiver of borosilicate glass, conforming to the di-mensions shown in Fig. 9. If the receiver is part of an aut
34、omaticunit and is mounted in a thermostatted chamber, the jacket isnot required. (WarningThe glass parts of the apparatus aresubjected to severe thermal conditions and, to lessen thechances of failure during a test, only equipment shown to bestrain-free under polarized light should be used.)6.1.5 Va
35、cuum Gage, capable of measuring absolute pres-sures with an accuracy of 0.01 kPa in the range below 1 kPaabsolute and with an accuracy of 1 % above this pressure. TheMcLeod gage can achieve this accuracy when properly used,FIG. 4 Vacuum-Jacketed ColumnD1160064but a mercury manometer will permit this
36、 accuracy only downto a pressure of about 1 kPa and then only when read with agood cathetometer (an instrument based on a telescopemounted on a vernier scale to determine levels very accu-rately). An electronic gage such as the Baratron is satisfactorywhen calibrated from a McLeod gage but must be r
37、echeckedperiodically as described in Annex A3. A suitable pressurecalibration setup is illustrated in Fig. A3.1. Vacuum gagesbased on hot wires, radiation, or conductivity detectors are notrecommended.NOTE 2Suitable instruments for measuring the pressure of the systemduring the test are the tensimet
38、er or an electronic pressure gage, providedthe output is traceable to a primary gage, such as the non-tilting McLeodgage.6.1.5.1 Connect the vacuum gage to the side tube of thetemperature sensor/vacuum adapter of the distillation column(preferred location) or to the side tube of the sensor/vacuumada
39、pter 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.6.1.6 Pressure Regulating System, capable of maintainingthe pressure of the system constant within 0.01 kPa at pressuresof 1 kPa absolute and below an
40、d within 1 % of the absolutepressure at 1 kPa or higher. Suitable equipment for this purposeis described in Annex A4. Connect the pressure regulatingTABLE 1 Vacuum-Jacketed Column Assembly DimensionsNOTE 1These dimensions are for guidance for verifying the appropriate construction of the assembly. T
41、he actual dimensions used by glassmakersvary to some extent, and the dimensions they use to construct the assembly are not easily obtained after the assembly is fused together. Those dimensionsnoted as critical shall be adhered to within the tolerance listed. The dimensions listed in this chart have
42、 been gathered from users of the variousmanufactured manual and automatic apparatus who participated in the interlaboratory program to produce the precision for this test method.NOTE 2ImportantFurther study will progress to produce a set of dimensions which will be more restrictive in range of dimen
43、sion, since it isbelieved that the current wide variance in dimensions has resulted in precision for this test method to be significantly high. The target dimensions forthis assembly and other components of the apparatus are expected to be available within the next year, with implementation expected
44、 to occur after fiveyears of initial revised test method publication date.Component Critical DimensionsANotesA no 265 6 10 .B yes 99 6 4 Spillover pointC yes 85 6 3 Internal measurement difficult, used by manufacturer for assembly. Dimension is wherecenter of angled inner tube intersects with the in
45、ner wall of the vertical columnD (OD) no 64.5 6 2 .E no 14/23 or 19/38 Tapered ground joint femaleBF no 35/25 Spherical ground joint maleBGn356 10 This area to be covered by the insulating top of the heating mantleH (ID) yes 24.7 6 1.2 Use of 28 mm OD tubing achieves this dimensionI no 2 12 Window a
46、llows observation of boil-up rate and column cleanliness, but also allows detri-mental heat lossJn06 20 .Kn 6 7 .L (OD) no 8 Minimum, cooling medium connectionsM yes 230 6 13 This dimension determines condensed vapor run down time and affects temperature/recovery resultsN (OD) no 38 6 2 .O yes 140 6
47、 20 This dimension affects vapor condensing efficiency which influences temperature/recovery resultsP (ID) yes 18.7 6 1.1 Use of 22 mm OD tubing achieves this dimensionQ yes 60 6 2 .R no not applicable Connection to vacuum system; any suitable means is allowedS no not applicable Extension above cond
48、ensing section; must maintain minimum or greater internal diam-eter of condensing sectionT (ID) yes 18.7 6 1.1 Use of 22 mm OD tubing achieves this dimensionU yes 140 6 5 This dimension affects vapor condensing efficiency which influences temperature/recovery resultsV no not applicable Extensions on
49、 the upper and lower portions of the condensing section vary by manufac-turer and have no influence on the testWn126 7 .X yes 50 6 8 .Y yes 30 6 7 Distance to end of drip tipAAll dimensions are in millimetres.BGround glass joints from different sources may have one of a number of diameter to length ratios. For purposes of this test method, any are suitable, and in someinstances, the diameter itself is not critical. However, it is critical that the male and female parts of each joint are from the same series to avoid recession or protuberance.FIG. 5 Detail of D
