1、Designation: D5800 10Standard Test Method forEvaporation Loss of Lubricating Oils by the Noack Method1This standard is issued under the fixed designation D5800; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revis
2、ion. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope*1.1 This test method covers three procedures for determin-ing the evaporation loss of lubricating oils (particularly engineoils). P
3、rocedure A uses the Noack evaporative tester equip-ment; Procedure B uses the automated non-Woods metalNoack evaporative apparatus; and Procedure C uses Selby-Noack volatility test equipment. The test method relates to oneset of operating conditions but may be readily adapted to otherconditions when
4、 required.1.2 Noack results determined using Procedures A and Bshow consistent differences. Procedure A gives slightly lowerresults versus Procedure B on formulated engine oils, whileProcedure A gives higher results versus Procedure B onbasestocks.1.3 The values stated in SI units are to be regarded
5、 asstandard. No other units of measurement are included in thisstandard.1.4 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 and determine t
6、he applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD6299 Practice for Applying Statistical Quality Assurancean
7、d Control Charting Techniques to Evaluate AnalyticalMeasurement System PerformanceD6300 Practice for Determination of Precision and BiasData for Use in Test Methods for Petroleum Products andLubricants2.2 DIN Standards:3DIN 1725 Specification for Aluminum AlloysDIN 12785 Specifications for Glass The
8、rmometers3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 evaporation lossof a lubricating oil by the Noackmethod, that mass of volatile oil vapors lost when the oil isheated in a test crucible through which a constant flow of air isdrawn.3.1.2 volatility, nthe tendency of a li
9、quid to form a vapor.4. Summary of Test Method4.1 A measured quantity of sample is placed in an evapo-ration crucible or reaction flask that is then heated to 250Cwith a constant flow of air drawn through it for 60 min. Theloss in mass of the oil is determined.4.2 Interlaboratory tests have shown th
10、at Procedure A,Procedure B, and Procedure C yield essentially equivalentresults, with a correlation coefficient of R2= 0.996. See theresearch report for the Selby-Noack interlaboratory study.5. Significance and Use5.1 The evaporation loss is of particular importance inengine lubrication. Where high
11、temperatures occur, portions ofan oil can evaporate.5.2 Evaporation may contribute to oil consumption in anengine and can lead to a change in the properties of an oil.5.3 Many engine manufacturers specify a maximum allow-able evaporation loss.5.4 Some engine manufacturers, when specifying a maxi-mum
12、 allowable evaporation loss, quote this test method alongwith the specifications.5.5 Procedure C, using the Selby-Noack apparatus, alsopermits collection of the volatile oil vapors for determinationof their physical and chemical properties. Elemental analysis of1This test method is under the jurisdi
13、ction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.06 on Analysis of Lubricants.Current edition approved Aug. 1, 2010. Published August 2010. Originallyapproved in 1995. Last previous edition approved in 2008 as D580008. DOI:10.1520/D5
14、800-10.2For referenced ASTM standards, visit the ASTM website, 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.3Available from Deutsches Institut fr Normunge, Beuth
15、Verlag GmbH, Burg-grafen Strasse 6, 1000 Berlin 30, Germany.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.the collected volatiles may be helpful in identifying compo
16、-nents such as phosphorous, which has been linked to prematuredegradation of the emission system catalyst.Procedure A6. Apparatus6.1 Noack Evaporative Tester, comprising the following:6.1.1 Electrically Heated Block Unit, made from a mal-leable aluminum alloy (see DIN 1725, Sheet 1), insulated at th
17、ejacket and base against loss of heat. (WarningThis block isheated to 250C.) The block is heated electrically by a base andjacket heater, having a total power consumption of 1 to 1.2 kW.In this respect the difference between both individual powerconsumption should not exceed 0.15 kW. In the center o
18、f theheating block, there is a circular recess to insert the evaporatingcrucible, the space between block and crucible being filled withWoods alloy or a suitable equivalent. Two catches on the blockprevent the crucible from rising in the liquid metal bath. Twoadditional circular recesses at equal in
19、tervals from the center ofthe block are provided for the thermometers (see Fig. 1).6.1.2 Evaporating Crucible, with screw cover. The crucibleis made of stainless steel (see Fig. 2). Above the support ringis the thread for the cover. The nickel-plated brass cover ishermetically sealed to the crucible
20、 by an internal conicalsealing surface (see Fig. 3). Three nozzles of hardened steelpermit the air stream to pass through the cover. The extractiontube, which slopes downward, leads from a threaded and sealedconnection in the center of the cover.6.2 Balance, capable of weighing at least 200 g to the
21、nearest 0.01 g.6.3 Crucible Clamp and Spanner.6.4 Reamer, 2-mm diameter.6.5 Ball Bearing, 3.5-mm diameter.6.6 Thermometer, M260 (see DIN 12785) or temperaturesensing device capable of reading temperature to 0.1C. Thethermometer should be calibrated with appropriate procedureat appropriate frequency
22、(generally every six months).6.7 Contact Type Control Thermometer (for manual).6.8 Glass Y-piece, an internal diameter of 4 mm. The uprightarms, each 45-mm long, should form an angle such that the armconnected to the crucible extraction tube and the Y-piece forma straight line. The vertical arm is 6
23、0-mm long and beveled at45.6.9 Glass Delivery Tubes, an internal diameter of 4 mm,each arm length 100 mm, beveled at 45 at ends entering andleaving the bottles.6.9.1 Bent at an angle of approximately 80.6.9.2 Bent at an angle of approximately 100, length to 20mm of bottle base.6.9.3 Bent at an angle
24、 of approximately 90.6.10 Two Glass Bottles, approximately 2-L capacity, fittedwith rubber bungs bored to receive inlet and outlet tubes (seeFig. 4).6.11 Manometer, inclined form, water-filled, precision 0.2mm H2O or suitable pressure sensor capable of measuring 206 0.2 mm of H2O (a 0 to 50-mm H2O p
25、ressure transducer hasbeen found to be satisfactory).NOTE 1Some manometers use water as the reference fluid, othersmay use a lower density fluid correlated to read in millimetres of water.Users should ensure that the manometer is filled with the correct densityreference fluid.6.12 Glass T-Piece, wit
26、h bleed valve attached.6.13 Vacuum Pump.6.14 Timer, with accuracy of 0.2 s.6.15 Silicone Rubber Tubing, cut to size, with an internaldiameter of 4 mm.6.15.1 40-mm long; three pieces required,6.15.2 300-mm long, and6.15.3 100-mm long.NOTE 2The use of automated equipment is permissible as long as itgi
27、ves equivalent results specified in this test method. All hardwaredimensions, make-up of the block, crucible, heat capacity, and so forth,and glassware must conform to the specifications given in this testmethod.7. Reagents and Materials7.1 Cleaning SolventA mixture of naphtha and toluene isrecommen
28、ded for the cleaning of the crucible. (WarningFlammable, vapor harmful.) Overnight soaking may be neces-sary.7.2 Oils having a known evaporative loss, the value ofwhich is provided by the oil supplier. Some examples of suchoils include RL-N, RL 172, and RL 223, supplied by CEC.Other oils supplied by
29、 other vendors may also be used.7.3 Insulated Gloves.7.4 Paint Brush, such as a tinnerps acid brush (15 to 25-mmwidth).7.5 Woods Metal4or Suitable Heat Transfer Material(WarningWoods metal contains lead (25 %), bismuth(50 %), antimony (12.5 %), and cadmium (12.5 %); these havebeen found to be health
30、 hazardous. Avoid contact with skin atall times.)8. Hazards8.1 Safety HazardsIt is assumed that anyone using thistest method will either be fully trained and familiar with allnormal laboratory practices, or will be under the direct super-vision of such a person. It is the responsibility of the opera
31、torto ensure that all local legislative and statutory requirementsare met.8.2 (WarningThough the test method calls for a draft-free area, the exhaust fumes from the evaporating oil must beventilated to an outside source. Precaution shall be taken toavoid any possibility of fire or explosion.)NOTE 3O
32、ne way to achieve a draftfree environment and greatersafety in operation for the instruments used in this test method is describedin Appendix X3.8.3 An alternate means for preventing draft described inAppendix X3 was not used in the development of the testmethod precision statement.4The sole source
33、of supply of Woods metal known to the committee at this timeis Sigma-Aldrich, Customer Support, P.O. Box 14508, St. Louis, MO 63178. If youare aware of alternative suppliers, please provide this information to ASTMInternational Headquarters. Your comments will receive careful consideration at ameeti
34、ng of the responsible technical committee,1which you may attend.D5800 102NOTEAll dimensions in millilitres.FIG. 1 Heating BlockD5800 1039. Preparation of Apparatus9.1 Astandard assembly of the apparatus is shown in Fig. 5.To avoid disturbing the thermal equilibrium, the apparatusshall be assembled i
35、n a draftfree area and comply with Fig. 5in dimensions and apparatus. (See 8.2.)9.2 Add sufficient Woods metal or equivalent material to therecesses of the heating block so that, with the crucible andthermometer in place, the remaining spaces will be filled withthe molten metal.9.3 Using the highest
36、 heating rate possible, raise the tem-perature of the heating block until the Woods metal is molten.Insert the thermometers with their bulbs touching the bottom ofthe recesses, and ensure that the contact thermometer isplugged in the back of the heating block. Adjust the powersupplied to the heating
37、 block so that the temperature can bemaintained at 250 6 0.5C.9.4 Assemble the remaining apparatus, less the crucible, asshown in Fig. 5.9.5 Place an empty crucible in the heating block, securingthe flange under the screw heads against the buoyancy of theWoods metal. The level of the molten metal sh
38、ould be such thata trace of it can be seen at the flange of the crucible and the topof the heating block.9.6 Check that the readings can be obtained on the manom-eter scale, or other measuring device, by connecting thecrucible to the assembled apparatus. A reading of 20.0 6 0.2mm shall be obtained.9
39、.7 Disconnect and remove the crucible from the assembledapparatus.9.8 Switch off the pump and the heating block and raise thecrucible and the thermometers from the molten Woods metal.Using the brush, return any Woods metal clinging to thecrucible to the heating block.9.9 Clean the Y-piece and glass
40、tubing to prevent a build upof condensate.10. Verification10.1 Switch on the pump and the heating block and ensurethat the apparatus is assembled, minus the crucible, as shownin Fig. 5.10.2 Check that the crucible and cover are free from lacquer.10.2.1 After every test, clean the crucible and cover
41、withsolvent and allow to dry. Stubborn lacquer can be cleaned byabrasion from a glass beader under pressure.10.3 Pass the reamer through each of the three nozzles in thecover to ensure that they are clear. (WarningUsing a reamerwith a diameter larger than 2 mm can enlarge the nozzles. Thiscan lead t
42、o higher losses because of increased air flow.)10.4 Run the ball bearing through the extraction tube toensure that it is clear of dirt.NOTEAll dimensions in millilitres.FIG. 2 CrucibleNOTEAll dimensions in millilitres.FIG. 3 CoverD5800 10410.5 Weigh the empty crucible without its cover to thenearest
43、 0.01 g.10.6 Weigh into the crucible 65.0 6 0.1 g of the ReferenceOil.10.7 Screw on the cover using the clamp and spanner.10.8 Ensure the temperature of the heating block is at 250 60.5C. Place the crucible in its recess in the heating block,securing the flange under the screw heads against the buoy
44、ancyof the Woods metal. Switch the control of the heating block tocompensate for the heat capacity of the crucible. Immediately(in less than 5 s), connect the extraction tube of the crucible tothe arm of the glass Y-piece, making a butt joint. Simulta-neously, start the pump and the stopwatch and ad
45、just the bleedvalve to give a pressure differential of 20 6 0.2 mm.NOTE 4When the crucible is in the test position, its flange should beflush with the top of the heating block. Any protrusion of the crucibleflange above the heating block may suggest a buildup of Woods metal slagat the bottom of the
46、heating block recess. The heating block and thethermometer recesses should be cleaned and the Woods metal replaced ona regular basis to avoid the accumulation of slag. Oxidized Woods metalwill affect the heat transfer to the crucible and hence may have adeleterious effect on the results obtained.10.
47、9 Adjust the control on the heating block to maintain theblock temperature approximately 5C below the test tempera-ture. Readjust the temperature control so that the test tempera-ture is reestablished within 3 min of the start of the test.NOTE 5Temperature and pressure will be controlled automatical
48、lywhen automated equipment is used.10.10 At the start of the test, constant attention shall be paidto maintaining the correct pressure. Once this becomes steady,usually within 10 to 15 min, check periodically that thetemperature and pressure differential remain constant through-out the period of the
49、 test.10.11 After 60 min 6 5 s, lift the crucible from the heatingblock, remove any adhering alloy, and place the crucible in awarm water bath to a depth of at least 30 mm. The time periodfrom the end of the test to immersion of the crucible shall notexceed 60 s.10.12 After 30 min, remove the crucible from the water, drythe outside, and carefully remove the lid.10.13 Reweigh the crucible without the lid to the nearest0.01 g.10.14 Calculate to the nearest 0.1 % mass/mass (M/M) theevaporation loss of the reference oil.10.15 Compare the result obtain
