ASTM D1015-2005(2015) Standard Test Method for Freezing Points of High-Purity Hydrocarbons《高纯度烃冻结点的标准试验方法》.pdf
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1、Designation: D1015 05 (Reapproved 2015)Standard Test Method forFreezing Points of High-Purity Hydrocarbons1This standard is issued under the fixed designation D1015; 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.1. Scope1.1 This test method covers a procedure for the precisemeasurement of the freezing points of high-purity hydrocar-bons.1.2 The
3、values stated in SI units are to be regarded as thestandard. The values in parentheses are for information only.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 saf
4、ety and health practices and determine the applica-bility of regulatory limitations prior to use. For specific hazardstatements, see 5.1, 6.1 and 6.2.NOTE 1For the calculation of the molal purity of essentially purecompounds from measured freezing points and for procedures to be usedfor the sampling
5、 and determination of purity of certain specificcompounds, see Test Method D1016.2. Referenced Documents2.1 ASTM Standards:2D1016 Test Method for Purity of Hydrocarbons from Freez-ing PointsD1265 Practice for Sampling Liquefied Petroleum (LP)Gases, Manual MethodD4057 Practice for Manual Sampling of
6、Petroleum andPetroleum Products3. Summary of Test Method3.1 The precise experimental measurement of the freezingpoint is made from interpretation of time-temperature freezingor melting curves.34. Significance and Use4.1 The freezing point measured by this test method, whenused in conjunction with th
7、e physical constants for the hydro-carbons listed in Test Method D1016, allows the determinationof the purity of the material under test. A knowledge of thepurity of these hydrocarbons is often needed to help controltheir manufacture and to determine their suitability for use asreagent chemicals or
8、for conversion to other chemical inter-mediates or finished products.5. Apparatus5.1 Freezing-Point Apparatus,4,5as shown in Figs. 1-3comprising a freezing tube, a metal sheath for the freezingtube, a Dewar flask for the cooling bath, a Dewar flask for thewarming bath, a stirring mechanism, suitable
9、 clamps andholders for the parts, and the absorption tubes. The outer wallsof all Dewar flasks can be covered with adhesive tape tominimize danger from glass in case of breakage. (WarningWhen using liquid nitrogen as a refrigerant, provide a means toprevent condensation of oxygen in the space betwee
10、n thefreezing tube and the metal sheath and subsequent sealing ofthe space by ice forming on the ceramic (or glass) fiber collar.Provide the metal sheath with suitable openings in the sidesand bottom. Failure to do this may result in breakage of thefreezing tube when the liquefied oxygen evaporates
11、within thesealed space.)5.2 Resistance Bridge,6Mueller type, reading from0.0001 to 50 , in steps of 0.001 .1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.04.0D on Physical and Ch
12、emical Methods.Current edition approved June 1, 2015. Published July 2015. Originally approvedin 1949. Last previous edition approved in 2010 as D1015 05 (2010). DOI:10.1520/D1015-05R15.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceas
13、tm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3For details not given here, see Glasgow, A. R., Jr., Rossini, F. D., and Streiff,A. J., “Determination of the Purity of Hydrocarbons by Measurement of FreezingPoints,” Journa
14、l of Research, JNBAA, National Institute of Standards andTechnology, Vol 35, No. 6, 1945, p. 355.4The sole source of supply of the apparatus known to the committee at this timeis Reliance Glass Works, Inc., Bensenville, IL.5If you are aware of alternative suppliers, please provide this information t
15、oASTM International Headquarters. Your comments will receive careful consider-ation at a meeting of the responsible technical committee,1which you may attend.6Apparatus described in 5.2, 5.3, 5.4, and 5.5 was manufactured by the Leedsand Northrup Co., Philadelphia, PA, under the following catalog nu
16、mbers: resistancebridge, No. 8069 B; platinum resistance thermometer, No. 8163 B; galvanometer,highest precision, No. 2284 D; galvanometer, routine precision, No. 2430 A; lampand scale, No. 2100. The galvanometer, routine precision, No. 2430-A, and the lampand scale, No. 2100, are still available fr
17、om Leeds and Northrup. The platinumresistance thermometer, No. 8163-B, is no longer available from Leeds andNorthrup, but is available with the same part number from Yellows SpringsInstrument Co., Yellow Springs, OH. The resistance bridge No. 8069-B, and thegalvanometer, highest precision, No. 2284-
18、D, are no longer available; however, theymay be obtainable from instrument exchanges or used equipment suppliers. If otheravailable instrumentation is substituted for the original, the precision statement ofSection 13 will not apply.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, W
19、est Conshohocken, PA 19428-2959. United States1ABracket for motor, with rubber pad. QCeramic (or glass) fiber collar.BMotor, with reduction gears, to give 120 r/min. RBrass cylinder, 317.5 mm (1212 in.) in length and 54 mm (218 in.) in inside diameter,with bakelite collar; when liquid nitrogen is us
20、ed, the metal shield must be provided withsuitable openings in sides and bottom (see 5.1). If liquid air is used, the metal shield shouldbe constructed so as to keep hydrocarbon from contact with liquid air (see 6.2).CCoupling. (See Fig. 3). SDewar flask, for cooling or warming bath; approximate ins
21、ide diameter, 101 mm (4 in.);approximate inside depth, 330 mm (13 in.).DWheel. (See Fig. 3). TCeramic (or glass) fiber pad at bottom of cylinder R.ESteel rod. (See Fig. 3). UWood block support.FBearing. (See Fig. 3). VTable top.GSupport for bearing. (See Fig. 3). WWall.HSupport for freezing tube. X,
22、 XSpherical joint, 18/7.IAdjustable clamp holder. YStandard metal (copper or brass) to glass taper connections soldered.JClamp for freezing tube. ZConnection to vacuum pump.KStirrer. (See Fig. 3). aAnhydrous calcium sulfate, with indicator.LThermometer. bAnhydrous magnesium perchlorate, granular.MTu
23、be for inlet of dry air, with 12/5 spherical joint. dSeparating layer of glass wool.M12/5 spherical joint connection to rotameter. eAscarite.NCork stopper, with holes as shown, plus a small holefor the “seed” wire.fAnhydrous calcium sulfate.OFreezing tube, with silvered jacket. (See Fig. 2) gTo air.
24、PStopcock on freezing tube. hTo source of compressed air.PStopcock (high vacuum) to drying tube. iFlow meter, for rates of 10 mL min to 20 mL min.P9Stopcock (high vacuum) to vacuum line.FIG. 1 Assembly of the Freezing-Point ApparatusD1015 05 (2015)25.3 Platinum Resistance Thermometer ,6precision gra
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