1、Designation:D576395 (Reapproved 2006)1Designation: D5763 11Standard Test Method forOxidation and Thermal Stability Characteristics of Gear OilsUsing Universal Glassware1This standard is issued under the fixed designation D5763; the number immediately following the designation indicates the year ofor
2、iginal 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 13 editoriall
3、y in December 2008.1. Scope*1.1 This test method covers the determination of the oxidation characteristics of extreme pressure and non-extreme pressuregear oils and includes the quantitative determination of total sludge, viscosity change, and oil loss.NOTE 1While the round-robin tests used ISO VG 2
4、20 extreme pressure gear oils for developing precision data, the test method can be extended toother viscosity grades and to non-extreme pressure gear oils. Refer to Classification D2422 for viscosity grades.1.2The values stated in SI units are to be regarded as the standard. The values given in par
5、entheses are for information only.1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the us
6、er of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D445 Test Method for Kinematic Viscosity of Transparent and Opaque Liquids (and Calculation of Dynamic Viscosity)D
7、2422 Classification of Industrial Fluid Lubricants by Viscosity SystemD2893 Test Methods for Oxidation Characteristics of Extreme-Pressure Lubrication OilsD4057 Practice for Manual Sampling of Petroleum and Petroleum ProductsD4871 Guide for Universal Oxidation/Thermal Stability Test ApparatusE1Speci
8、fication for ASTM Liquid-in-Glass Thermometers Guide for Universal Oxidation/Thermal Stability Test Apparatus3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 adherent sludge, nsludge that is formed on the walls of a container and is not easily removed.3.1.2 aliquot, nportion of
9、 sample being tested that is a representative portion of the whole.3.1.3 extreme pressure gear oil, ngear oil that contains chemical additives, such as sulfur and phosphorus compounds, whichproduce a protective film on the metal surface to provide anti-scuffing and anti-scoring properties.3.1.4 filt
10、erable sludge, nsludge that is formed in the oil.3.1.5 non-extreme pressure gear oil, n, ngear oil that contains no extreme pressure additives.3.1.6 oxidation, nthe process by which oxygen chemically reacts with materials.3.1.7 sludge, nin gear oils, a precipitate that sometimes forms as the oil age
11、s or oxidizes.3.1.8 universal glassware, nthe glassware that is described in the universal oxidation thermal stability test. Refer to GuideD4871.4. Summary of Test Method4.1 The viscosity of the gear oil being tested is determined. A 100-g aliquot of the oil in a weighed apparatus is subjected to1Th
12、is test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.09.0Don Oxidation of Lubricants.Current edition approved Nov. 1, 2006. Published January 2007. Originally approved in 1995. Last previous edition a
13、pproved in 2001 as D576395 (2001). DOI:10.1520/D5763-95R06E01.Current edition approved Dec. 1, 2011. Published March 2012. Originally approved in 1995. Last previous edition approved in 2006 as D576395(2006)1. DOI:10.1520/D5763-11.2For referencedASTM standards, visit theASTM website, www.astm.org, o
14、r contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.1This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes h
15、ave been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official d
16、ocument.*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.a temperature of 120C for 312 h while dry air is passed through the aliquot at 3 L/h.4.2 At the end of the stres
17、s period, the aliquot is cooled to room temperature. The apparatus is reweighed to determine oil loss.Filterable sludge is recovered by vacuum filtration using a 2.8-m glass fiber filter medium. The viscosity of the filtered oil isdetermined. Sludge adhering to the oxidation cell and associated glas
18、sware is rinsed with heptane and the washings passed throughthe same filter used to filter the filterable sludge. The filter is dried in an oven to a constant weight to determine the total filterablesludge.4.3 The apparatus is dried and weighed to determine the amount of adherent sludge. The sum of
19、the filterable sludge andadherent sludge is reported as total sludge. The percentage change in viscosity and percent oil loss are also reported.5. Significance and Use5.1 Degradation of gear oils by oxidation or thermal breakdown, or both, can result in sludge buildup and render the oilunsuitable fo
20、r further use as a lubricant.5.2 This is the only test method that employs glassware to measure the amount of sludge produced during oxidation and thermaldegradation. This test method is a modification of Test Method D2893 which measures the viscosity increase and precipitationnumber of the oil stre
21、ssed at 95C, but does not measure 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,3thermostatical
22、ly controlled, capable of maintaining the oil sample in the oxidation cell at a uniformtemperature of 120 6 1C and large enough to hold a minimum of two oxidation cells and sufficiently deep to allow approximately120 mm of the test tubes to extend above the heating liquid or block. The heating block
23、 is further described in Test Method D4871.6.2 Oxidation Cell,3consists of borosilicate glass; a 38- mm inside diameter and a 300 6 5-mm length is required.NOTE 2While the round-robin test used the oxidation cell from a specific equipment manufacturer in determining the precision statement, the test
24、method permits the use of other oxidation cells that meet the requirements of 6.2.6.3 Air Delivery Tube,3a borosilicate glass tube having an inside diameter of 5 mm and a minimum length of 320 mm, withthe lower tip cut at a 45 angle.NOTE 3The oxidation cell and delivery tube are further described in
25、 Test Method D4871.6.4 Flowmeters,3one for each oxidation cell, capable of measuring an air flow of 3 L/h 6 0.5 L/h.6.5 Air DryerBefore being supplied to the flowmeters, the air shall be passed through a drying tower packed with indicatinggrade anhydrous calcium sulfate or equivalent. The quantity o
26、f desiccant should be sufficient to last for the entire test. It isrecommended that the drying tower be filled with fresh 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 to the nearest centigram (0.01 g)
27、 and having the capacity to weighup to 2000 g.6.8 Filter Holder, 47 mm, consisting of a borosilicate glass funnel and a funnel base with a coarse-grade fritted glass filtersupport or stainless steel screen support such that the filter can be clamped between the ground glass sealing surfaces of the f
28、unneland its base by means of a metal clamp.6.9 Oven, explosive-proof, capable of heating from 50 to 60C and of a sufficient size to hold oxidation cells.6.10 Thermometer,ASTM solvent distillation thermometer having a range from 98 to 152C and conforming to the requirementfor Thermometer 41C in acco
29、rdance with Specification E1. , ASTM solvent distillation thermometer having a range from 98 to152C or equivalent digital contact thermometer.6.11 Vacuum Source, to provide pressure reduction to 100 6 5 mm Hg absolute pressure.7. Reagents and Materials7.1 Air Supply, dried air, oil free, at constant
30、 pressure to permit 3 L/h air flow through the system. House air supply orpressurized air cylinders can be used.7.2 Calcium Sulfate Desiccant, Anhydrous, indicating grade (desiccant that changes color when it nears saturation with water).Desiccants equivalent to calcium sulfate can be used.7.3 Hepta
31、ne, minimum purity99.75%. (Heptaneminimum purity, 99.75 %. (WarningHeptane is flammable and a healthhazard.)8. Sampling8.1 Samples for this test method can come from tanks, drums, small containers, or operating equipment. Therefore, use the3The sole source of supply of the apparatus (universal glass
32、ware and heating bath with flowmeters as a complete unit) known to the committee at this time is FalexCorp.,Corporation, 1020 Airpark Drive, Sugar Grove, IL 60554-9452. If you are aware of alternative suppliers, please provide this information to ASTM InternationalHeadquarters. Your comments will re
33、ceive careful consideration at a meeting of the responsible technical committee, which you may attend.D5763 112applicable apparatus and techniques described in Practice D4057 to obtain suitable samples.8.2 Special precautions to preserve the integrity of a sample will not normally be required. It is
34、 good practice to avoid undueexposure of samples to heat, sunlight, or strong direct light. Visibly heterogeneous samples should not be used.8.3 It is recommended that a 200-mL representative be obtained. To ensure the aliquot being tested is representative of thesample, agitation; for example, stir
35、ring or shaking of the oil 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 detergent solution (using a bristle brush) and rinse thoroughly with tap water.When any visible deposits remain, soaking with a h
36、ot detergent solution can be helpful. After final cleaning by soaking with asuitable cleaning solution rinse thoroughly with tap water and then distilled water, and allow to dry at room temperature or in anoven.9.1.2 Used glassware should be cleaned immediately following the end of a test. When addi
37、tional cleaning is necessary, use anon-chromic acid containing cleaning solution.9.2 Heating Block or BathEnsure that the heating block or bath is able to heat the oxidation cell at the control temperatureof 120C.9.3 FlowmeterEnsure that the flowmeter is capable of delivering the desired flow rate o
38、f 3.0 L of air per hour.10. Procedure10.1 Using Test Method D445, determine the viscosity of the oil at 100C. Record as V2.10.2 Adjust the heating bath or block to a temperature high enough to maintain the oil in the desired number of oxidation cellsat the required temperature of 120 6 1C.10.3 Place
39、 and weigh a 1000-mL beaker on the balance. Zero the tare of the beaker and place the oxidation cell in the beaker.Insert the air delivery tube in the cell. The angled tip of the air delivery tube should rest on the bottom of the oxidation cell. Obtainthe weight of the cell and delivery tube. Record
40、 as B1.10.4 Slowly pour 100.00 6 0.1 g of oil sample into the oxidation cell which contains the air delivery tube. Obtain the weightof the oil sample, air delivery tube, and oxidation cell, A2.10.5 Place the oxidation cell containing the oil sample and air delivery tube in the heating block or bath.
41、10.6 Connect the air delivery tube to the air source from the flowmeter. Adjust the flow of dried air to 3 6 0.5 L/h.10.7 Monitor the temperature of the oil sample and adjust the heating block/bath thermostat, if necessary. Observe thetemperature of the oil sample twice during the first hour, then o
42、nce every hour for at least 3 h, making the necessary adjustmenteach time until a constant temperature of 120 6 1C is read twice in succession. Check the air flow and temperature at least twicea day and adjust the control flow, when necessary.10.8 At the end of 312 h (13 days), remove the oxidation
43、cell containing the oxidized oil and delivery tube from the bath orblock, and allow the oxidized oil to cool to room temperature. When an oil bath is used, rinse the outside of the oxidation cell withheptane and wipe dry. Place the cell and its contents in a tared 1000-mL beaker and obtain the weigh
44、t of the oil sample, oxidationcell, and delivery tube as in 10.4. Record this weight, A1.10.9 Weigh a 2.8-m glass fiber filter to the nearest 0.01 g and record, F1. Using the filter holder apparatus, vacuum filter thecooled oxidized oil through the glass filter. Determine the viscosity at 100C of th
45、e filtered oil by Test Method D445. Record theviscosity result, V1.NOTE 4The viscosity and sludge determinations for the oxidized oil should be done within four days after removing the cell from the heating bathor block. It has been found that extending storage time beyond four days can give variabl
46、e test results.10.10 Wash the oxidation cell and air delivery tube with heptane and filter the washings through the same filter. Continuewashing until the heptane is no longer colored by the oxidized oil. Draw air through the filter until the precipitate appears dry. Placethe filter in an operating
47、hood for 0.5 h to evaporate 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 oxidation cell and then place the cell in an explosive-proof oven at 50 to 60C for1 to 2 h. Dry the air delivery
48、 tube by passing air through the tube. Let the oxidation cell cool to room temperature. Weigh theoxidation cell and air delivery tube, B2.11. Calculations11.1 Determine the amount of sludge, viscosity change, and oil loss by the following equations.11.1.1 Filterable sludge on filter, g.D25 F2 F1(1)w
49、here:D2= amount of sludge on filter pad, g,F2= weight of filter pad and sludge, g, andD5763 113F1= weight of filter, g.11.1.2 Adherent sludge on oxidation cell and air delivery tube, g.D15 B2 B1(2)where:D1= amount of sludge on oxidation cell and air delivery tube, g,B2= weight of oxidation cell and air delivery tube, solvent washed 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 100C increase, mm2,%V35V1 V2V23 100 (
