1、Designation: D5346 17Standard Test Method forDetermination of the Pour Point of Petroleum Oil Used inFatliquors and Softening Compounds1This standard is issued under the fixed designation D5346; the number immediately following the designation indicates the year oforiginal adoption or, in the case o
2、f 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.1. Scope1.1 This test method covers the determination of the pourpoint of petroleum oils used in the softe
3、ning and stuffing ofleather, and in the manufacture of fatliquors and other soften-ing and stuffing compounds.This test method was derived fromTest Method D97 and ALCA Method H-18.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstand
4、ard.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, health and environmental practices and deter-mine the applicability of regulatory limitations prior to
5、use.1.4 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarrier
6、s to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D97 Test Method for Pour Point of Petroleum ProductsE1 Specification for ASTM Liquid-in-Glass ThermometersE2251 Specification for Liquid-in-Glass ASTM Thermom-eters with Low-Hazard Precision Liquids2.2 Other Document:ALCA Method H
7、-18 Cloud and Pour Point33. Significance and Use3.1 This test method is intended to determine the pour pointof petroleum oils used in the softening and stuffing of leather,as well as those used in the manufacture of products for suchpurpose. The pour point of petroleum oils is measured for thepurpos
8、e 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. Toindicate 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 c
9、on-forming to the requirements prescribed in Specifications E1 orE2251 for thermometers:Temperature Thermometer NumberThermometer Range ASTM IPHigh cloud and pour 38 to +50C 5C or S5C 1CLow cloud and pour 80 to +20C 6C 2CMelting point +32 to +127C 61C 63C4.2.1 Since separation of liquid column therm
10、ometers 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 point).4.3 Cork, to fit the test jar, bored centrally for the testthermometer.4.4 Jacket, metal or glass, watertight, cy
11、lindrical, flatbottom, 115 mm in depth, 42 to 50 mm inside diameter. It mustbe supported firmly in a vertical position in the cooling bath of4.7 so that not more than 25 mm projects out of the coolingmedium.4.5 Disk, cork or felt, 6 mm thick to fit loosely inside thejacket.4.6 Gasket, to fit snugly
12、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 hard enough to hold its shape. Its purpose isto prevent the test jar from touching the jacket.4.7 Bath or Baths, maintained
13、at prescribed temperatureswith a firm support to hold the jacket vertical. The requiredbath temperatures may be obtained by refrigeration if1This test method is under the jurisdiction ofASTM Committee D31 on Leatherand is the direct responsibility of Subcommittee D31.08 on Fats and Oils.Current edit
14、ion approved Sept. 1, 2017. Published October 2017. Originallyapproved in 1993. Last previous edition approved in 2009 as D5346 93 (2009).DOI: 10.1520/D5346-17.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of
15、 ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from American Leather Chemists Assn., Texas Tech University, P.O.Box 45300, Lubbock, TX 79409.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-29
16、59. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical
17、Barriers to Trade (TBT) Committee.1available, otherwise by suitable freezing mixtures. Freezingmixtures commonly used for temperatures down to thoseshown are as follows:For Temperatures DownIce and water 9CCrushed ice and sodium chloride crystals 12CCrushed ice and calcium chloride crystals 27CAceto
18、ne or petroleum naphtha (see Section 5) chilledin a covered metal beaker 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, permi
19、t the use ofsmaller samples, and have other factors which may merit their 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
20、 by an automatic instrument. Precision of automatic pour pointtesters 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 ap
21、propri-ate for low-temperature bath media.5.1.1 Acetone. (WarningExtremely 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.
22、5C.)6. Procedure6.1 Pour the oil into the test jar to the level mark. Whennecessary, 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 thethe
23、rmal history of the sample is not known, keep the sample at roomtemperature 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 th
24、e cork and thermometer so the cork fitstightly, the thermometer and the jar 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 treatm
25、ent:NOTE 1Dimensions are in millimetres.FIG. 1 Apparatus for Pour Point TestD5346 1726.3.1 Oils Having Pour Points Above 33CHeat the oilwithout stirring to 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 t
26、est 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 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
27、cloudand pour thermometer in position.6.4 See that the disk, gasket, 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 med
28、ium.6.5 After the oil has cooled to allow the formation ofparaffin 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 i
29、ntegers that are positive ornegative multiples of 3C. Begin to examine 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
30、jar from the jacket. Toremove condensed moisture that limits visibility, 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 replacemen
31、t shall require not more than3s.6.6.1 If the oil has not ceased 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
32、, move to 51C bath,Oil is at 42C, move to 69C bath.6.6.2 As soon 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
33、repeat a test for flow at the next temperature, 3C lower.6.7 Continue 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 sp
34、ecifications havingpour point limits at temperatures not divisible 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. Continueo
35、bservations at 3C intervals as described in 6.6 and 6.7 until thespecification 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 isthe upper (ma
36、ximum) pour point. If required, determine thelower (minimum) pour point by heating the sample whilestirring, to 105C, pouring it into the jar, and determining thepour point as 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 pou
37、r point, ASTM D5346. For black oil, etc.,add 3C to the temperature 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
38、successive testresults, obtained by the same operator using the 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 con
39、sidered suspect.8.1.2 ReproducibilityThe difference between two 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 twe
40、nty. Differencesgreater than this should be considered suspect.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 assort
41、edfuel oils tested by twelve cooperators. The mineral oil basedlubricants 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.
42、876.432.526.599. Keywords9.1 fatliquors; leather; petroleum oil pour point; softeningand stuffing compoundsD5346 173ASTM 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 a
43、dvised that determination of the validity of any such patent rights, and 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, eith
44、er reapproved or withdrawn. Your comments are invited either for revision 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.
45、 If you feel that your comments have not received a fair hearing you shouldmake 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. Indi
46、vidual 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). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 174
