1、Designation: D 5763 95 (Reapproved 2006)1An American National StandardStandard Test Method forOxidation and Thermal Stability Characteristics of Gear OilsUsing Universal Glassware1This standard is issued under the fixed designation D 5763; the number immediately following the designation indicates t
2、he year oforiginal 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.1NOTEAdded research report to existing footnote for Section 1
3、3 editorially in December 2008.1. Scope1.1 This test method covers the determination of the oxida-tion characteristics of extreme pressure and non-extreme pres-sure gear oils and includes the quantitative determination oftotal sludge, viscosity change, and oil loss.NOTE 1While the round-robin tests
4、used ISO VG 220 extremepressure gear oils for developing precision data, the test method can beextended to other viscosity grades and to non-extreme pressure gear oils.Refer to Classification D 2422 for viscosity grades.1.2 The values stated in SI units are to be regarded as thestandard. The values
5、given in parentheses are for informationonly.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 and health practices and determine the applica-bility of regula
6、tory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 445 Test Method for Kinematic Viscosity of Transparentand Opaque Liquids (and Calculation of Dynamic Viscos-ity)D 2422 Classification of Industrial Fluid Lubricants byViscosity SystemD 2893 Test Methods for Oxidation Characte
7、ristics ofExtreme-Pressure Lubrication OilsD 4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD 4871 Guide for Universal Oxidation/Thermal StabilityTest ApparatusE1 Specification for ASTM Liquid-in-Glass Thermometers3. Terminology3.1 Definitions of Terms Specific to This Standard:
8、3.1.1 adherent sludge, nsludge that is formed on the wallsof a container and is not easily removed.3.1.2 aliquot, nportion of sample being tested that is arepresentative portion of the whole.3.1.3 extreme pressure gear oil, ngear oil that containschemical additives, such as sulfur and phosphorus com
9、pounds,which produce a protective film on the metal surface to provideanti-scuffing and anti-scoring properties.3.1.4 filterable sludge, nsludge that is formed in the oil.3.1.5 non-extreme pressure gear oil, n, ngear oil thatcontains no extreme pressure additives.3.1.6 oxidation, nthe process by whi
10、ch oxygen chemi-cally reacts with materials.3.1.7 sludge, nin gear oils, a precipitate that sometimesforms as the oil ages or oxidizes.3.1.8 universal glassware, nthe glassware that is de-scribed in the universal oxidation thermal stability test. Referto Guide D 4871.4. Summary of Test Method4.1 The
11、 viscosity of the gear oil being tested is determined.A100-g aliquot of the oil in a weighed apparatus is subjected toa temperature of 120C for 312 h while dry air is passedthrough the aliquot at 3 L/h.4.2 At the end of the stress period, the aliquot is cooled toroom temperature. The apparatus is re
12、weighed to determine oilloss. Filterable sludge is recovered by vacum filtration using a2.8-m glass fiber filter medium. The viscosity of the filteredoil is determined. Sludge adhering to the oxidation cell andassociated glassware is rinsed with heptane and the washingspassed through the same filter
13、 used to filter the filterablesludge. The filter is dried in an oven to a constant weight todetermine the total filterable sludge.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.09.0D on Oxidati
14、on of Lubricants.Current edition approved Nov. 1, 2006. Published January 2007. Originallyapproved in 1995. Last previous edition approved in 2001 as D 5763 95 (2001).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual
15、Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.4.3 The apparatus is dried and weighed to determine theamount of adherent sludg
16、e. The sum of the filterable sludge andadherent sludge is reported as total sludge. The percentagechange in viscosity and percent oil loss are also reported.5. Significance and Use5.1 Degradation of gear oils by oxidation or thermal break-down, or both, can result in sludge buildup and render the oi
17、lunsuitable for further use as a lubricant.5.2 This is the only test method that employs glassware tomeasure the amount of sludge produced during oxidation andthermal degradation. This test method is a modification of TestMethod D 2893 which measures the viscosity increase andprecipitation number of
18、 the oil stressed at 95C, but does notmeasure the amount of sludge formed.5.3 This test method can be used to evaluate the oxidation/thermal stability of gear oils. However, the test results may notcorrelate with the performance of gear oils in field service.6. Apparatus6.1 Heating Bath or Block,3th
19、ermostatically controlled,capable of maintaining the oil sample in the oxidation cell at auniform temperature of 120 6 1C and large enough to hold aminimum of two oxidation cells and sufficiently deep to allowapproximately 120 mm of the test tubes to extend above theheating liquid or block. The heat
20、ing block is further describedin Test Method D 4871.6.2 Oxidation Cell,3consists of borosilicate glass; a 38- mminside diameter and a 300 6 5-mm length is required.NOTE 2While the round-robin test used the oxidation cell from aspecific equipment manufacturer in determining the precision statement,th
21、e test method permits the use of other oxidation cells that meet therequirements of 6.2.6.3 Air Delivery Tube,3a borosilicate glass tube having aninside diameter of 5 mm and a minimum length of 320 mm,with the lower tip cut at a 45 angle.NOTE 3The oxidation cell and delivery tube are further describ
22、ed inTest Method D 4871.6.4 Flowmeters,3one for each oxidation cell, capable ofmeasuring an air flow of 3 L/h6 0.5 L/h.6.5 Air DryerBefore being supplied to the flowmeters, theair shall be passed through a drying tower packed withindicating grade anhydrous calcium sulfate or equivalent. Thequantity
23、of desiccant should be sufficient to last for the entiretest. It is recommended that the drying tower be filled withfresh desiccant prior to the test.6.6 Filter, glass fiber, 2.8-m porosity, 47 mm in diameter.6.7 Balance, electronic, top-loading, capable of weighing tothe nearest centigram (0.01 g)
24、and having the capacity to weighup to 2000 g.6.8 Filter Holder, 47 mm, consisting of a borosilicate glassfunnel and a funnel base with a coarse-grade fritted glass filtersupport or stainless steel screen support such that the filter canbe clamped between the ground glass sealing surfaces of thefunne
25、l and its base by means of a metal clamp.6.9 Oven, explosive-proof, capable of heating from 50 to60C and of a sufficient size to hold oxidation cells.6.10 Thermometer, ASTM solvent distillation thermometerhaving a range from 98 to 152C and conforming to therequirement for Thermometer 41C in accordan
26、ce with Speci-fication E1.6.11 Vacuum Source, to provide pressure reduction to 100 65 mm Hg absolute pressure.7. Reagents and Materials7.1 Air Supply, dried air, oil free, at constant pressure topermit 3 L/h air flow through the system. House air supply orpressurized air cylinders can be used.7.2 Ca
27、lcium Sulfate Desiccant,Anhydrous, indicating grade(desiccant that changes color when it nears saturation withwater). Desiccants equivalent to calcium sulfate can be used.7.3 Heptane, minimum purity99.75 %. (WarningHeptane is flammable and a health hazard.)8. Sampling8.1 Samples for this test method
28、 can come from tanks,drums, small containers, or operating equipment. Therefore,use the applicable apparatus and techniques described inPractice D 4057 to obtain suitable samples.8.2 Special precautions to preserve the integrity of a samplewill not normally be required. It is good practice to avoidu
29、ndue exposure of samples to heat, sunlight, or strong directlight. Visibly heterogeneous samples should not be used.8.3 It is recommended that a 200-mL representative beobtained. To ensure the aliquot being tested is representative ofthe sample, agitation; for example, stirring or shaking of the oil
30、prior to obtaining an aliquot, is recommended.9. Preparation of Apparatus9.1 Cleaning Glassware:9.1.1 Clean new glassware by washing with a hot detergentsolution (using a bristle brush) and rinse thoroughly with tapwater. When any visible deposits remain, soaking with a hotdetergent solution can be
31、helpful. After final cleaning bysoaking with a suitable cleaning solution rinse thoroughly withtap water and then distilled water, and allow to dry at roomtemperature or in an oven.9.1.2 Used glassware should be cleaned immediately fol-lowing the end of a test. When additional cleaning is necessary,
32、use a non-chromic acid containing cleaning solution.9.2 Heating Block or BathEnsure that the heating blockor bath is able to heat the oxidation cell at the controltemperature of 120C.9.3 FlowmeterEnsure that the flowmeter is capable ofdelivering the desired flow rate of 3.0 L of air per hour.10. Pro
33、cedure10.1 Using Test Method D 445, determine the viscosity ofthe oil at 100C. Record as V2.3The sole source of supply of the apparatus (universal glassware and heatingbath with flowmeters as a complete unit) known to the committee at this time isFalex Corp., 1020 Airpark Drive, Sugar Grove, IL 6055
34、4. If you are aware ofalternative suppliers, please provide this information to ASTM InternationalHeadquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee,1which you may attend.D 5763 95 (2006)1210.2 Adjust the heating bath or block to a tempe
35、rature highenough to maintain the oil in the desired number of oxidationcells at the required temperature of 120 6 1C.10.3 Place and weigh a 1000-mL beaker on the balance.Zero the tare of the beaker and place the oxidation cell in thebeaker. Insert the air delivery tube in the cell. The angled tip o
36、fthe air delivery tube should rest on the bottom of the oxidationcell. Obtain the weight of the cell and delivery tube. Record asB1.10.4 Slowly pour 100.00 6 0.1 g of oil sample into theoxidation cell which contains the air delivery tube. Obtain theweight of the oil sample, air delivery tube, and ox
37、idation cell,A2.10.5 Place the oxidation cell containing the oil sample andair delivery tube in the heating block or bath.10.6 Connect the air delivery tube to the air source from theflowmeter. Adjust the flow of dried air to 3 6 0.5 L/h.10.7 Monitor the temperature of the oil sample and adjustthe h
38、eating block/bath thermostat, if necessary. Observe thetemperature of the oil sample twice during the first hour, thenonce every hour for at least 3 h, making the necessaryadjustment each time until a constant temperature of 120 61C is read twice in succession. Check the air flow andtemperature at l
39、east twice a day and adjust the control flow,when necessary.10.8 At the end of 312 h (13 days), remove the oxidationcell containing the oxidized oil and delivery tube from the bathor block, and allow the oxidized oil to cool to room tempera-ture. When an oil bath is used, rinse the outside of the ox
40、idationcell with heptane and wipe dry. Place the cell and its contentsin a tared 1000-mL beaker and obtain the weight of the oilsample, oxidation cell, and delivery tube as in 10.4. Record thisweight, A1.10.9 Weigh a 2.8-m glass fiber filter to the nearest 0.01 gand record, F1. Using the filter hold
41、er apparatus, vacuum filterthe cooled oxidized oil through the glass filter. Determine theviscosity at 100C of the filtered oil by Test Method D 445.Record the viscosity result, V1.NOTE 4The viscosity and sludge determinations for the oxidized oilshould be done within four days after removing the ce
42、ll from the heatingbath or block. It has been found that extending storage time beyond fourdays can give variable test results.10.10 Wash the oxidation cell and air delivery tube withheptane and filter the washings through the same filter. Con-tinue washing until the heptane is no longer colored by
43、theoxidized oil. Draw air through the filter until the precipitateappears dry. Place the filter in an operating hood for 0.5 h toevaporate heptane. Transfer the filter to a 50 to 60C explosive-proof oven for 0.5 h. Let cool to room temperature and weigh,F2.10.11 Allow heptane to evaporate from the o
44、xidation celland then place the cell in an explosive-proof oven at 50 to 60Cfor 1 to 2 h. Dry the air delivery tube by passing air through thetube. Let the oxidation cell cool to room temperature. Weighthe oxidation cell and air delivery tube, B2.11. Calculations11.1 Determine the amount of sludge,
45、viscosity change, andoil loss by the following equations.11.1.1 Filterable sludge on filter, g.D25 F2 F1(1)where:D2= amount of sludge on filter pad, g,F2= weight of filter pad and sludge, g, andF1= weight of filter, g.11.1.2 Adherent sludge on oxidation cell and air deliverytube, g.D15 B2 B1(2)where
46、:D1= amount of sludge on oxidation cell and air deliverytube, g,B2= weight of oxidation cell and air delivery tube, solventwashed and dried, g, andB1= original weight of oxidation cell and air delivery tube,g.11.1.3 Total sludge, g.D35 D11 D2(3)where:D3= total amount of sludge, g.11.1.4 Viscosity at
47、 100C increase, mm2,%V35V1 V2V23 100 (4)where:V3= viscosity increase, %,V2= original viscosity of oil sample, andV1= viscosity of oxidized oil sample.11.1.5 Oil loss, g.C35 A2 A1(5)where:C3= oil loss, g,A2= original combined weight of oil sample, oxidationcell, and air delivery tube, g, andA1= combi
48、ned weight of oxidized oil, oxidation cell, andair delivery tube, g.12. Report12.1 Report the amount of filterable sludge on the filter tothe nearest 0.01 g.12.2 Report the amount of adherent sludge on the oxidationtubes to the nearest 0.01 g.12.3 Report the total amount of sludge to the nearest 0.0
49、1 gor to the nearest 0.01 %.12.4 Report the viscosity increase in percent.D 5763 95 (2006)1312.5 Report oil loss to the nearest 0.01 g or percent.13. Precision and Bias413.1 PrecisionThe precision of this test method as deter-mined by the statistical examination of the inter-laboratory testresults is as follows.13.1.1 Total Sludge:13.1.1.1 RepeatabilityThe difference between successiveresults obtained by the same operator with the same apparatusunder constant operating conditions on identical test materialswould in the long run, in the
