1、Designation: D 5346 93 (Reapproved 2003)e1Standard Test Method forDetermination of the Pour Point of Petroleum Oil Used inFatliquors and Softening Compounds1This standard is issued under the fixed designation D 5346; the number immediately following the designation indicates the year oforiginal adop
2、tion 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.e1NOTEWarning notes were editorially moved into the standard text in June 2003.1. S
3、cope1.1 This test method covers the determination of the pourpoint of petroleum oils used in the softening and stuffing ofleather, and in the manufacture of fatliquors and other soften-ing and stuffing compounds. This test method was derived fromTest Method D 97 and ALCA Method H-18.1.2 This standar
4、d 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 and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM
5、 Standards:D 97 Test Method for Pour Point of Petroleum Products2E 1 Specification for ASTM Thermometers32.2 Other Document:ALCA Method H-18 Cloud and Pour Point43. Significance and Use3.1 This test method is intended to determine the pour pointof petroleum oils used in the softening and stuffing of
6、 leather,as well as those used in the manufacture of products for suchpurpose. The pour point of petroleum oils is measured for thepurpose of quality assurance.4. Apparatus (see Fig. 1)4.1 Test Jar, clear cylindrical glass, flat bottom, 30 to33.5-mm inside diameter, and 115 to 125-mm height. Toindic
7、ate sample height the jar should be marked with a line 546 3 mm above the inside bottom.4.2 Thermometers, having ranges shown below and con-forming to the requirements prescribed in Specification E 1 forthermometers:Temperature Thermometer NumberThermometer Range ASTM IPHigh cloud and pour 38 to +50
8、C 5C 1CLow cloud and pour 80 to +20C 6C 2CMelting point +32 to +127C 61C 63C4.2.1 Since separation of liquid column thermometers occa-sionally occurs and may escape detection, thermometersshould be checked immediately prior to the test and used onlyif they prove accurate within 6 1C (for example ice
9、 point).4.3 Cork, to fit the test jar, bored centrally for the testthermometer.4.4 Jacket, metal or glass, watertight, cylindrical, flat bot-tom, 115 mm in depth, 42 to 50 mm inside diameter. It must besupported firmly in a vertical position in the cooling bath of 4.7so that not more than 25 mm proj
10、ects out of the coolingmedium.4.5 Disk, cork or felt, 6 mm thick to fit loosely inside thejacket.4.6 Gasket, to fit snugly around the outside of the test jarand loosely inside the jacket. The gasket may be made ofrubber, leather, or other material that is elastic enough to clingto the test jar and h
11、ard enough to hold its shape. Its purpose isto prevent the test jar from touching the jacket.4.7 Bath or Baths, maintained at prescribed temperatureswith a firm support to hold the jacket vertical. The requiredbath temperatures may be obtained by refrigeration if avail-able, otherwise by suitable fr
12、eezing mixtures. Freezing mix-tures commonly used for temperatures down to those shownare as follows:For Temperatures DownIce and water 9CCrushed ice and sodium chloride crystals 12CCrushed ice and calcium chloride crystals 27CAcetone or petroleum naphtha (see Section 5) chilledin a covered metal be
13、aker with an ice-salt mixtureto 12C then with enough solid carbon dioxide togive the desired temperature.57CNOTE 1There are automatic pour point testers available and in usewhich may be advantageous in the saving of test time, permit the use of1This test method is under the jurisdiction of ASTM Comm
14、ittee D31 on Leatherand is the direct responsibility of Subcommittee D31.08 on Fats and Oils.Current edition approved May 10, 2003. Published June 2003. Originallyapproved in 1993. Last previous edition approved in 1997 as D 5346 93 (1997).2Annual Book of ASTM Standards, Vol 05.01.3Annual Book of AS
15、TM Standards, Vol 14.03.4Available from American Leather Chemists Assn., Texas Tech University, P.O.Box 45300, Lubbock, TX 794091Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.smaller samples, and have other factors which may merit t
16、heir use. Ifautomatic testers are used, the user must ensure that all of the manufac-turers instructions for calibration, adjustment and operation of theinstrument are followed. It must be reported that the pour point wasdetermined by an automatic instrument. Precision of automatic pour pointtesters
17、 has not been determined. In any case of dispute, the pour point asdetermined by the manual method described herein shall be considered thereference test.5. Reagents and Materials5.1 The following solvents of technical grade are appropri-ate for low-temperature bath media.5.1.1 Acetone.(WarningExtre
18、mely flammable.)5.1.2 Alcohol, Ethanol.(WarningFlammable.)5.1.3 Alcohol, Methanol.(WarningFlammable. Vaporharmful.)5.1.4 Petroleum Naphtha.(WarningCombustible. Vaporharmful.)5.1.5 Solid Carbon Dioxide.(WarningExtremelycold 78.5C.)6. Procedure6.1 Pour the oil into the test jar to the level mark. When
19、necessary, heat the oil in a water bath until it is just sufficientlyfluid to pour into the test jar.NOTE 2When it is known that a sample has been heated to atemperature higher than 45C during the preceding 24 h or when thethermal history of the sample is not known, keep the sample at roomtemperatur
20、e for 24 h before testing it.6.2 Close the test jar with the cork carrying the high-pourthermometer (4.2). In the case of pour points above 36C, usea higher range thermometer such as IP 3C or ASTM 61C.Adjust the position of the cork and thermometer so the cork fitstightly, the thermometer and the ja
21、r are coaxial, and thethermometer bulb is immersed so the beginning of the capillaryis 3 mm below the surface of the oil.6.3 For the measurement of pour point, subject the oil in thetest jar to the following preliminary treatment:6.3.1 Oils Having Pour Points Above 33CHeat the oilwithout stirring to
22、 9C above the expected pour point, but to atleast 45C, in a bath maintained at 12C above the expectedpour point, but at least 48C. Transfer the test jar to a waterbath maintained at 24C and commence observations for pourpoint.6.3.2 Oils Having Pour Points of 33C and BelowHeatthe oil without stirring
23、 to 45C in a bath maintained at 48Cand cool to 15C in a water bath maintained at 6C. Removethe high cloud and pour thermometer and place the low cloudand pour thermometer in position.NOTE 1Dimensions are in millimetres.FIG. 1 Apparatus for Pour Point TestD 5346 93 (2003)e126.4 See that the disk, gas
24、ket, and the inside of the jacket areclean and dry. Place the disk in the bottom of the jacket. Placethe gasket around the test jar, 25 mm from the bottom. Insertthe test jar in the jacket. Never place a jar directly into thecooling medium.6.5 After the oil has cooled to allow the formation ofparaff
25、in wax crystals, take great care not to disturb the mass ofoil nor permit the thermometer to shift in the oil; anydisturbance of the spongy network of wax crystals will lead tolow and erroneous results.6.6 Pour points are expressed in integers that are positive ornegative multiples of 3C. Begin to e
26、xamine the appearance ofthe oil when the temperature of the oil is 9C above theexpected pour point (estimated as a multiple of 3C). At eachtest thermometer reading that is a multiple of 3C below thestarting temperature, remove the test jar from the jacket. Toremove condensed moisture that limits vis
27、ibility, wipe thesurface with a clean cloth moistened in alcohol (ethanol ormethanol). Tilt the jar just enough to ascertain whether there isa movement of the oil in the test jar. The complete operation ofremoval, wiping, and replacement shall require not more than3s.6.6.1 If the oil has not ceased
28、to flow when its temperaturehas reached 27C, transfer the test jar to the next lowertemperature bath per the following schedule:Oil is at +27C, move to 0C bath,Oil is at +9C, move to 18C bath,Oil is at 6C, move to 33C bath,Oil is at 24C, move to 51C bath,Oil is at 42C, move to 69C bath.6.6.2 As soon
29、 as the oil in the jar does not flow when tilted,hold the jar in a horizontal position for 5 s, as noted by anaccurate timing device and observe carefully. If the oil showsany movement, replace the test jar immediately in the jacketand repeat a test for flow at the next temperature, 3C lower.6.7 Con
30、tinue in this manner until a point is reached at whichthe oil shows no movement when the test jar is held in ahorizontal position for 5 s. Record the observed reading of thetest thermometer.NOTE 3To determine compliance with existing specifications havingpour point limits at temperatures not divisib
31、le by 3C, it is acceptablepractice to conduct the pour point measurement according to the followingschedule: Begin to examine the appearance of the oil when the tempera-ture of the oil is 9C above the specification pour point. Continueobservations at 3C intervals as described in 6.6 and 6.7 until th
32、especification temperature is reached. Report the sample as passing orfailing the specification limit.6.8 For black oil, cylinder stock and nondistillate fuel oil,the result obtained by the procedure described in 6.1-6.7 is theupper (maximum) pour point. If required, determine the lower(minimum) pou
33、r point by heating the sample while stirring, to105C, pouring it into the jar, and determining the pour pointas described in 6.4-6.7 .7. Calculation and Report7.1 Add 3C to the temperature recorded in 6.7 and reportthe result as the pour point, ASTM D5346. For black oil, etc.,add 3C to the temperatu
34、re recorded in 6.7 and report the resultas upper pour point, ASTM D5346, or lower pour point, ASTMD5346, as required.8. Precision and Bias8.1 Lubricating Oils and Distillate and Residual Fuel Oil:8.1.1 RepeatabilityThe difference between successive testresults, obtained by the same operator using th
35、e same apparatusunder constant operating conditions on identical test material,would in the long run, in the normal and correct operation ofthis test method, exceed 3C only in one case in twenty.Differences greater than this should be considered suspect.8.1.2 ReproducibilityThe difference between tw
36、o singleand independent test results, obtained by different operatorsworking in different laboratories on identical test material,would in the long run, in normal and correct operation of thistest method, exceed 6C only in one case in twenty. Differencesgreater than this should be considered suspect
37、.8.2 BiasThere being no criteria for measuring bias inthese test-product combinations, no statement of bias can bemade.8.3 The precision statements were prepared with data on tennew (unused) mineral oil based lubricants and sixteen assortedfuel oils tested by twelve cooperators. The mineral oil base
38、dlubricants had pour points ranged from 48C to 6C whilethe fuel oils had pour points ranging from 33C to + 51C.The following precision data were obtained:95 % Confidence Mineral Oil Lubricants Fuel OilsRepeatability, CReproducibility, C2.876.432.526.599. Keywords9.1 fatliquors; leather; petroleum oi
39、l pour point; softeningand stuffing compoundsASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, an
40、d the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revisi
41、on of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you sh
42、ouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).D 5346 93 (2003)e13
