1、Designation: D 611 07Designation: 2/98An American National StandardStandard Test Methods forAniline Point and Mixed Aniline Point of Petroleum Productsand Hydrocarbon Solvents1This standard is issued under the fixed designation D 611; the number immediately following the designation indicates the ye
2、ar oforiginal adoption or, in the case of revision, 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 Depart
3、ment of Defense.1. Scope*1.1 These test methods cover the determination of theaniline point of petroleum products and hydrocarbon solvents.Test Method A is suitable for transparent samples with aninitial boiling point above room temperature and where theaniline point is below the bubble point and ab
4、ove the solidifi-cation point of the aniline-sample mixture. Test Method B, athin-film method, is suitable for samples too dark for testing byTest MethodA. Test Methods C and D are for samples that mayvaporize appreciably at the aniline point. Test Method D isparticularly suitable where only small q
5、uantities of sample areavailable. Test Method E describes a procedure using anautomatic apparatus suitable for the range covered by TestMethods A and B.1.2 These test methods also cover the determination of themixed aniline point of petroleum products and hydrocarbonsolvents having aniline points be
6、low the temperature at whichaniline will crystallize from the aniline-sample mixture.1.3 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 an
7、d determine the applica-bility of regulatory limitations prior to use. Specific warningstatements are given in Section 7.2. Referenced Documents2.1 ASTM Standards:2D 1500 Test Method for ASTM Color of Petroleum Prod-ucts (ASTM Color Scale)E1 Specification for ASTM Liquid-in-Glass Thermometers3. Term
8、inology3.1 Definitions:3.1.1 aniline pointthe minimum equilibrium solutiontemperature for equal volumes of aniline and sample.3.1.2 mixed aniline pointthe minimum equilibrium solu-tion temperature of a mixture of two volumes of aniline, onevolume of sample, and one volume of n-heptane of specifiedpu
9、rity.4. Summary of Test Method4.1 Specified volumes of aniline and sample, or aniline andsample plus n-heptane, are placed in a tube and mixedmechanically. The mixture is heated at a controlled rate untilthe two phases become miscible. The mixture is then cooled ata controlled rate and the temperatu
10、re at which two phasesseparate is recorded as the aniline point or mixed aniline point.5. Significance and Use5.1 The aniline point (or mixed aniline point) is useful as anaid in the characterization of pure hydrocarbons and in theanalysis of hydrocarbon mixtures. Aromatic hydrocarbonsexhibit the lo
11、west, and paraffins the highest values. Cyclopar-affins and olefins exhibit values that lie between those forparaffins and aromatics. In homologous series the anilinepoints increase with increasing molecular weight. Although itoccasionally is used in combination with other physical prop-erties in co
12、rrelative methods for hydrocarbon analysis, theaniline point is most often used to provide an estimate of thearomatic hydrocarbon content of mixtures.1These test methods are under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and are the direct responsibility of D02.04.0
13、Don Physical and Chemical Methods.Current edition approved Nov. 1, 2007. Published November 2007. Originallyapproved in 1941. Last previous edition approved in 2004 as D 61104.These test methods were adopted as a joint ASTM-IP standard in 1964.2For referenced ASTM standards, visit the ASTM website,
14、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 Harbor Driv
15、e, PO Box C700, West Conshohocken, PA 19428-2959, United States.6. Apparatus6.1 For details of the aniline point apparatus required foreach method see:Annex A1 for Test Method AAnnex A2 for Test Method BAnnex A3 for Test Method CAnnex A4 for Test Method DAnnex A5 for Test Method ENOTE 1Alternative a
16、pparatus may be used, such as the U-tubemethod for dark oils, provided it has been shown to give results of thesame precision and accuracy as those described in the annexes.6.2 Heating and Cooling BathA suitable air bath, anonvolatile, transparent liquid bath, or an infrared lamp (250 to375 W), prov
17、ided with means for controlling the rate ofheating.NOTE 2Water should not be used as either a heating or coolingmedium since aniline is hygroscopic and moist aniline will give erroneoustest results. For example, the aniline point of the n-heptane reagent asmeasured with aniline containing 0.1 volume
18、 % water is approximately0.5C (0.9F) higher than that measured with dry aniline. If the anilinepoint is below the dew point of the atmosphere, pass a slow stream of dryinert gas into the aniline point tube to blanket the aniline-sample mixture.6.3 Thermometers, or other temperature sensing devices,s
19、uch as thermocouples or platinum resistance thermometersthat cover the temperamental range of interest and can provideequivalent or better accuracy and precision, may be used inplace of the thermometers having the following ranges andconforming to the requirements of the designated ASTM or IPspecifi
20、cation:RangeASTM(Specification E1)IP38 to + 42C (36.5 to + 107.5F) 33C, 33F 20C25 to 105C (77 to 221F) 34C, 34F 21C90 to 170C (194 to 338F) 35C, 35F 59C6.4 Pipets, or equivalent volume dispensing devices, ca-pable of delivering volumes with capacities of 10 6 0.04 mLand 5 6 0.02 mL, for use in the t
21、est.6.5 BalanceA laboratory balance sensitive to 0.01 g,suitable for weighing the tube and sample when the samplecannot be pipetted conveniently.6.6 Safety Goggles.6.7 Plastic Gloves, impervious to aniline.7. Reagents7.1 Aniline (WarningAniline should not be pipetted di-rectly by mouth because of it
22、s extreme toxicity. Aniline is alsotoxic by absorption through the skin even in very smallquantities, and should be handled with great caution.) Theaniline shall be sufficiently pure such that when tested withn-heptane according to Section 9, it shall give an aniline pointof 69.3 6 0.2C (156.7 6 0.4
23、F) as determined from theaverage of two independent tests having a difference of notmore than 0.1C (0.2F). If the aniline point of heptane ishigher than this specification, the aniline may be dried bydistillation, where the first and last 10 % are discarded. If theaniline point is lower, water may b
24、e added until the anilinemeets the specification.NOTE 3It is estimated that approximately 400 to 1400 ppm of waterin aniline is required to meet the heptane specification.NOTE 4As an alternative to distilling the aniline on the day of use, theaniline may be distilled as described in 7.1, collecting
25、the distillate inampoules, sealing the ampoules under vacuum or dry nitrogen, and storingin a cool dark place for future use. Alternatively, distillate may be storedunder dry nitrogen in a glass bottle or in single use ampoules kept in acool, dark place. In either case, rigid precaution must be take
26、n to avoidcontamination from atmospheric moisture (Note 2). It is believed thatunder these conditions the aniline will remain unchanged for a periodexceeding 6 months.7.2 Calcium Sulfate, anhydrous.7.3 n-Heptane, spectroscopic or HPLC grade. (WarningFlammable. Harmful if inhaled. Keep away from heat
27、, sparks,and open flame. Keep container closed. Use with adequateventilation. Avoid prolonged breathing of vapor or spray mist.Avoid prolonged or repeated skin contact.)8. Sample8.1 Dry the sample by shaking vigorously for 3 to 5 minwith about 10 volume % of a suitable drying agent such asanhydrous
28、calcium sulfate or anhydrous sodium sulfate. Re-duce the viscosity of viscous samples by warming to atemperature below that which would cause the loss of lightends or the dehydration of the drying agent. Remove anysuspended drying agent by use of a centrifuge or by filtration.Heat samples containing
29、 separated wax until they are homo-geneous and keep heated during filtration or centrifugation toensure against separation of wax. When suspended water isvisibly present and the sample material is known to dissolveless than 0.03 mass % of water, the use of a centrifuge for theremoval of suspended wa
30、ter is an acceptable procedure.9. Procedure for Aniline Point9.1 The following methods, to be used as applicable, arecovered as follows:9.1.1 Test Method A, described in detail in Annex A1,isapplicable to clear samples or to samples not darker than No.6.5 ASTM color, as determined by Test Method D 1
31、500,having initial boiling points well above the expected anilinepoint.9.1.2 Test Method B, described in detail in Annex A2,isapplicable to light-colored samples, moderately dark samples,and to very dark samples. It is suitable for samples that are toodark to be tested by Test Method A.9.1.3 Test Me
32、thod C, described in detail in Annex A3,isapplicable to clear samples or to samples not darker than No.6.5 ASTM color, as determined by Test Method D 1500,having initial boiling points sufficiently low as to give incorrectaniline point readings by Test Method A, for example, aviationgasoline.9.1.4 T
33、est Method D, described in detail in Annex A4,isapplicable to the same type of sample as Test Method C. It isparticularly useful when only limited quantities of sample areavailable.9.1.5 Test Method E is applicable when using automaticapparatus in accordance with the instructions in Annex A5.D611072
34、10. Procedure for Mixed Aniline Point10.1 This procedure is applicable to samples having anilinepoints below the temperature at which aniline crystallizes fromthe mixture. Deliver 10 mL of aniline (WarningSee 7.1), 5mL of sample, and 5 mL of n-heptane into a clean, dryapparatus. Determine the anilin
35、e point of the mixture by TestMethod A or B as described in Annex A1 or Annex A2.11. Report11.1 If the range of three successive observations of theaniline point temperature is not greater than 0.1C (0.2F) forlight-colored samples or 0.2C (0.4F) for dark samples, reportthe average temperature of the
36、se observations, corrected forthermometer calibration errors, to the nearest 0.05C (0.1F) asthe aniline point.11.2 If such a range is not obtained after five observations,repeat the test using fresh quantities of aniline and sample in aclean, dry apparatus, and if consecutive temperature observa-tio
37、ns show a progressive change, or if the range of observationsis greater than the repeatability given in 12.1, report the testmethod as being inapplicable.12. Precision and Bias12.1 The precision of these test methods as obtained bystatistical examination of interlaboratory test results is asfollows:
38、12.1.1 RepeatabilityThe difference between successivetest results (two average temperatures obtained in a series ofobservations as described in Section 11 obtained by the sameoperator with the same apparatus under constant operatingconditions on identical test material, would in the long run, inthe
39、normal and correct operation of the test method, exceed thefollowing values only in one case in twenty:RepeatabilityAniline point of:Clear, light-colored samples 0.16C (0.3F)Moderately dark to very dark samples 0.3C (0.6F)AMixed aniline point of:Clear, light-colored samples 0.16C (0.3F)AModerately d
40、ark to very dark samples_0.3C (0.6F)AANot determined from recent cooperative tests; however, the ratios with thosegiven in the 1953 version are believed to apply.12.1.2 ReproducibilityThe difference between two singleand independent results, obtained by different operators, work-ing in different lab
41、oratories on identical test material, would inthe long run, in the normal and correct operation of the testmethod, exceed the following values only in one case intwenty:ReproducibilityAniline point of:Clear, light-colored samples 0.5C (0.9F)Moderately dark to very dark samples 1.0CA(1.8F)Mixed anili
42、ne point of:Clear, light-colored samples 0.7C (1.3F)AModerately dark to very dark samples_1.0C (1.8F)AANot determined from recent cooperative tests; however, the ratios with thosegiven in the 1953 version are believed to apply.12.2 BiasA statement of bias is now being developed bythe subcommittee.12
43、.3 The precision of this test was not obtained in accor-dance with Committee D02 Research Report RR:D02-1007,“Manual on Determining Precision Data for ASTM Methodson Petroleum Products and Lubricants.”13. Keywords13.1 aniline point; aromatics; mixed aniline pointANNEXES(Mandatory Information)A1. TES
44、T METHOD AA1.1 ApparatusA1.1.1 The apparatus shown in Fig.A1.1 shall consist of thefollowing:A1.1.1.1 Test Tube, approximately 25 mm in diameter and150 mm in length, made of heat-resistant glass.A1.1.1.2 Jacket, approximately 37 to 42 mm in diameterand 175 mm in length, made of heat-resistant glass.
45、A1.1.1.3 Stirrer, manually operated, metal, approximately 2mm in diameter (14 B the tube containssufficient light transformer oil to cover the bulb of thethermometer. The inner tube is held in the top of the aniline-point tube by a tightly fitting stopper, and a clamp is providedto hold the stopper
46、in position to prevent loss of vapor from thesample.NOTE A3.1Any other suitable arrangement, such as a screwed plasticgland carrying the thermometer, that will prevent the loss of vapor fromthe apparatus, may be used. In such cases it may be possible to omit thethermometer tube and immerse the therm
47、ometer bulb in the aniline-sample mixture.A3.1.2 Guard, of stout metal gauze and surrounding theaniline point tube. It should preferably be combined with theclamp for holding the thermometer tube in place.A3.2 ProcedureA3.2.1 Clean and dry the apparatus. Deliver 5 mL of aniline(WarningPut on goggles
48、 of safety glass and plastic glovesimpervious to aniline. Also see 7.1) and 5 mL of the driedsample (8.1), both cooled to a temperature at which the samplemay be measured without loss of vapor. Close the tube bymeans of the stopper and fit the thermometer tube centrally sothat the bottom is 5 mm fro
49、m the bottom of the aniline pointtube. Clamp the stopper in position and attach the guard.A3.2.2 Follow the procedure described inA1.2.2 andA1.2.3but mix the sample and aniline by shaking the tube. If the rateof change of temperature is greater than 1C (2F)/min whenthe aniline point is being approached, place the tube in a jacketthat has previously been warmed or cooled to an appropriatetemperature.A3.2.3 Repeat the observation of aniline point by heatingand cooling repeatedly until a report as directed in Section
