1、Designation: D611 12 (Reapproved 2016)Designation: 2/98Standard Test Methods forAniline Point and Mixed Aniline Point of Petroleum Productsand Hydrocarbon Solvents1This standard is issued under the fixed designation D611; the number immediately following the designation indicates the year oforiginal
2、 adoption or, in the case of revision, the year of last 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 D
3、efense.1. Scope1.1 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 above the so
4、lidifi-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 quantities
5、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 below the te
6、mperature at whichaniline will crystallize from the aniline-sample mixture.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 WARNINGMercury has been designated by manyregulatory agencies as a hazardous material that can ca
7、usecentral nervous system, kidney and liver damage. Mercury, orits vapor, may be hazardous to health and corrosive tomaterials. Caution should be taken when handling mercury andmercury containing products. See the applicable product Ma-terial Safety Data Sheet (MSDS) for details and EPAswebsitehttp:
8、/www.epa.gov/mercury/faq.htmfor addi-tional information. Users should be aware that selling mercuryand/or mercury containing products into your state or countrymay be prohibited by law.1.5 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is the
9、responsibility 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. Specific warningstatements are given in Section 7.2. Referenced Documents2.1 ASTM Standards:2D1500 Test Method for ASTM Color of
10、Petroleum Products(ASTM Color Scale)E1 Specification for ASTM Liquid-in-Glass Thermometers3. Terminology3.1 Definitions:3.1.1 aniline point, nthe minimum equilibrium solutiontemperature for equal volumes of aniline and sample.3.1.2 mixed aniline point, nthe minimum equilibriumsolution temperature of
11、 a mixture of two volumes of aniline,one volume of sample, and one volume of n-heptane ofspecified purity.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
12、untilthe two phases become miscible. The mixture is then cooled ata controlled rate and the temperature 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
13、 of pure hydrocarbons and in the1These test methods are under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and are the direct responsibilityof D02.04.0D on Physical and Chemical Methods.Current edition approved Oct. 1, 2016. Published November 2016. Origi
14、nallyapproved in 1941. Last previous edition approved in 2012 as D611 12. DOI:10.1520/D0611-12R16.These test methods were adopted as a joint ASTM-IP standard in 1964.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual B
15、ook of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1analysis of hydrocarbon mixtures. Aromatic hydrocarbonsexhibit the lowest, and pa
16、raffins 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 correlative me
17、thods for hydrocarbon analysis, theaniline point is most often used to provide an estimate of thearomatic hydrocarbon content of mixtures.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 Metho
18、d CAnnex A4 for Test Method DAnnex A5 for Test Method ENOTE 1Alternative apparatus may be used, such as the U-tube methodfor dark oils, provided it has been shown to give results of the sameprecision and accuracy as those described in the annexes.6.2 Heating and Cooling BathA suitable air bath, anon
19、volatile, transparent liquid bath, or an infrared lamp(250 W to 375 W), provided with means for controlling therate of heating.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
20、point of the n-heptane reagent asmeasured with aniline containing 0.1 % by volume water is approximately0.5 C (0.9 F) 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 th
21、e aniline-sample mixture.6.3 Thermometers, or other temperature sensing devices,such 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 follo
22、wing ranges andconforming to the requirements of the designated ASTM or IPspecification:RangeASTM(Specification E1)IP38 C to + 42 C (36.5 Fto + 107.5 F)33C, 33F 20C25 C to 105 C (77 F to 221 F) 34C, 34F 21C90 C to 170 C (194 F to 338 F) 35C, 35F 59C6.4 Pipets, or equivalent volume dispensing devices
23、, ca-pable of delivering volumes with capacities of 10 mL 60.04 mL and 5 mL 6 0.02 mL, for use in the test.6.5 BalanceA laboratory balance sensitive to 0.01 g, suit-able for weighing the tube and sample when the sample cannotbe pipetted conveniently.6.6 Safety Goggles.6.7 Plastic Gloves, impervious
24、to aniline.7. Reagents7.1 Aniline (WarningAniline should not be pipetted di-rectly by mouth because of its 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 wh
25、en tested withn-heptane according to Section 9, it shall give an aniline pointof 69.3 C 6 0.2 C (156.7 F 6 0.4 F) as determined fromthe average of two independent tests having a difference of notmore than 0.1 C (0.2 F). If the aniline point of heptane ishigher than this specification, the aniline ma
26、y be dried bydistillation, where the first and last 10 % are discarded. If theaniline point is lower, water may be added until the anilinemeets the specification.NOTE 3It is estimated that approximately 400 ppm to 1400 ppm ofwater in aniline is required to meet the heptane specification.NOTE 4As an
27、alternative to distilling the aniline on the day of use, theaniline may be distilled as described in 7.1, collecting 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
28、 in a glass bottle or in single use ampoules kept in acool, dark place. In either case, rigid precaution must be taken 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 Sulf
29、ate, anhydrous.7.3 n-Heptane, spectroscopic or HPLC grade. (WarningFlammable. Harmful if inhaled. Keep away from heat, 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 D
30、ry the sample by shaking vigorously for 3 min to5 min with about 10 % by volume of a suitable drying agentsuch as anhydrous calcium sulfate or anhydrous sodiumsulfate. Reduce the viscosity of viscous samples by warming toa temperature below that which would cause the loss of lightends or the dehydra
31、tion of the drying agent. Remove anysuspended drying agent by use of a centrifuge or by filtration.Heat samples containing 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
32、sample material is known to dissolveless than 0.03 % by mass of water, the use of a centrifuge forthe removal of suspended water 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 detai
33、l in Annex A1,isapplicable to clear samples or to samples not darker than No.6.5ASTM color, as determined by Test Method D1500, havinginitial boiling points well above the expected aniline point.9.1.2 Test Method B, described in detail in Annex A2,isapplicable to light-colored samples, moderately da
34、rk 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 Method C, described in detail in Annex A3,isapplicable to clear samples or to samples not darker than No.6.5ASTM color, as determined by Test Method D1500, havinginitial boiling
35、points sufficiently low as to give incorrect anilinepoint readings by Test Method A, for example, aviationgasoline.D611 12 (2016)29.1.4 Test 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 sa
36、mple areavailable.9.1.5 Test Method E is applicable when using automaticapparatus in accordance with the instructions in Annex A5.10. Procedure for Mixed Aniline Point10.1 This procedure is applicable to samples having anilinepoints below the temperature at which aniline crystallizes fromthe mixture
37、. Deliver 10 mL of aniline (WarningSee 7.1),5 mL of sample, and 5 mL of n-heptane into a clean, dryapparatus. Determine the aniline 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 temperat
38、ure is not greater than 0.1 C (0.2 F) forlight-colored samples or 0.2 C (0.4 F) for dark samples,report the average temperature of these observations, correctedfor thermometer calibration errors, to the nearest 0.05 C(0.1 F) as the aniline point.11.2 If such a range is not obtained after five observ
39、ations,repeat the test using fresh quantities of aniline and sample in aclean, dry apparatus, and if consecutive temperature observa-tions 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. Precis
40、ion and Bias12.1 The precision of these test methods as obtained bystatistical examination of interlaboratory test results is asfollows:12.1.1 RepeatabilityThe difference between successivetest results (two average temperatures obtained in a series ofobservations as described in Section 11 obtained
41、by the sameoperator with the same apparatus under constant operatingconditions on identical test material, would in the long run, inthe 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.
42、16 C (0.3 F)Moderately dark to very dark samples 0.3 C (0.6 F)AMixed aniline point of:Clear, light-colored samples 0.16 C (0.3 F)AModerately dark to very dark samples 0.3 C (0.6 F)AANot determined from recent cooperative tests; however, the ratios with thosegiven in the 1953 version are believed to
43、apply.12.1.2 ReproducibilityThe difference between two singleand independent results, obtained by different operators, work-ing in different laboratories on identical test material, would inthe long run, in the normal and correct operation of the testmethod, exceed the following values only in one c
44、ase intwenty:ReproducibilityAniline point of:Clear, light-colored samples 0.5 C (0.9 F)Moderately dark to very dark samples 1.0 CA(1.8 F)Mixed aniline point of:Clear, light-colored samples 0.7 C (1.3 F)AModerately dark to very dark samples 1.0 C (1.8 F)AANot determined from recent cooperative tests;
45、 however, the ratios with thosegiven in the 1953 version are believed to apply.12.2 BiasSince there is no accepted reference materialsuitable for determining the bias for the procedure in these testmethods, bias has not been determined.12.3 The precision of this test was not obtained in accor-dance
46、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. TEST METHOD AA1.1 ApparatusA1.1.1 The apparatus shown in Fig.A1.1
47、 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 mm to 42 mm in diam-eter and 175 mm in length, made of heat-resistant glass.A1.1.1.3 Stirrer, manually operated, metal, approximately
48、2 mm 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 in position to prevent loss of vapor from thesample.NOTE
49、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 thermometer 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(War
