1、Designation: D5846 07 (Reapproved 2012)Standard Test Method forUniversal Oxidation Test for Hydraulic and Turbine OilsUsing the Universal Oxidation Test Apparatus1This standard is issued under the fixed designation D5846; the number immediately following the designation indicates the year oforiginal
2、 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.1. Scope1.1 This test method covers a procedure for evaluating theoxidation sta
3、bility of petroleum base hydraulic oils and oils forsteam and gas turbines.1.2 This test method was developed to evaluate the oxida-tion stability of petroleum base hydraulic oils and oils forsteam and gas turbines.1.2.1 Rust and oxidation inhibited hydraulic, anti-wear hy-draulic and turbine oils o
4、f ISO 3268 viscosity were used todevelop the precision statement. This test method has beenused to evaluate the oxidation stability of fluids made withsynthetic basestock and in-service oils; however, these fluidshave not been used in cooperative testing to develop precisiondata.1.3 The values state
5、d in SI units are to be regarded asstandard. The values given in parentheses are for informationonly.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 hea
6、lth practices and determine the applica-bility of regulatory limitations prior to use. Identified hazard-ous chemicals are listed in 7.3, 7.6, and 7.8. Before using thistest method, refer to suppliers safety labels, Material SafetyData Sheets, and other technical literature.2. Referenced Documents2.
7、1 ASTM Standards:2A510 Specification for General Requirements for Wire Rodsand Coarse Round Wire, Carbon SteelB1 Specification for Hard-Drawn Copper WireD664 Test Method for Acid Number of Petroleum Productsby Potentiometric TitrationD943 Test Method for Oxidation Characteristics of InhibitedMineral
8、 OilsD974 Test Method for Acid and Base Number by Color-Indicator TitrationD3339 Test Method forAcid Number of Petroleum Productsby Semi-Micro Color Indicator TitrationD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4740 Test Method for Cleanliness and Compatibility ofResidual
9、Fuels by Spot TestD4871 Guide for Universal Oxidation/Thermal StabilityTest ApparatusD5770 Test Method for Semiquantitative Micro Determina-tion of Acid Number of Lubricating Oils During Oxida-tion Testing2.2 Energy Institute Standard:3IP 2546 Practice for Sampling of Petroleum Products;alternate to
10、 Practice D40572.3 British Standard:4BS 1829 Specification for Carbon Steel Wire; alternate toSpecification A5102.4 ASTM Adjuncts:Reference Spot Sheet53. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 inhibited mineral oil, na petroleum oil containingadditives to retard oxidatio
11、n.3.1.2 oxidation life, nof an oil, the time in hours requiredfor degradation of the oil under test.3.1.3 universal oxidation test, nthe apparatus and proce-dures described in Guide D4871.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the
12、 direct responsibility of SubcommitteeD02.09.0D on Oxidation of Lubricants.Current edition approved Dec. 1, 2012. Published December 2012. Originallyapproved in 1995. Last previous edition approved in 2007 as D584607. DOI:10.1520/D5846-07R12.2For referenced ASTM standards, visit the ASTM website, ww
13、w.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 Energy Institute, 61 New Cavendish St., London, WIG 7AR,U.K., http:/www.energyinst.org.uk.4Available fr
14、om British Standards Institute (BSI), 389 Chiswick High Rd.,London W4 4AL, U.K., http:/www.bsi-.5Available from ASTM International Headquarters. Order Adjunct No.ADJD4740. Original adjunct produced in 2000.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-
15、2959. United States14. Summary of Test Method4.1 An oil sample is contacted with air at 135C in thepresence of copper and iron metals. The acid number and spotforming tendency of the oil are measured daily. The test isterminated when the oxidation life of the oil has been reached.4.2 The oil is cons
16、idered to be degraded when either its acidnumber (measured by Test Methods D974 or D664) hasincreased by 0.5 mg KOH/g over that of new oil; or when theoil begins to form insoluble solids so that when a drop of oil isplaced onto a filter paper it shows a clearly defined dark spotsurrounded by a ring
17、of clear oil.5. Significance and Use5.1 Degradation of hydraulic fluids and turbine oils, becauseof oxidation or thermal breakdown, can result in the formationof acids or insoluble solids and render the oil unfit for furtheruse.5.2 This test method can be used to estimate the relativeoxidation stabi
18、lity of petroleum-base oils. It should be recog-nized that correlation between results of this test and theoxidation stability in use can vary markedly with serviceconditions and with various oils.6. Apparatus6.1 Heating Block, as shown on the right in Fig. 1, and asfurther described in Guide D4871,
19、 to provide a controlledconstant temperature for conducting the test.6.1.1 Test cells are maintained at a constant elevated tem-perature by means of a heated aluminum block which sur-rounds each test cell.6.1.2 The test cells shall fit into the block to a depth of 2256 5 mm. When centered, the side
20、clearance of the 38 mmoutside diameter glass tube to the holes in the aluminum blockshall not exceed 1 mm in any direction.6.2 Temperature Control System, as shown at lower left inFig. 1, and as further described in Guide D4871, to maintainthe test oils in the heating block at 135 6 0.5C for the dur
21、ationof the test.6.3 Gas Flow Control System, as shown in the upper left inFig. 1, and as further described in Guide D4871, to provide dryair at a flow rate of 3.0 6 0.5 L/h to each test cell.FIG. 1 Apparatus, Showing Gas Flow Control System, Temperature Control System, and Heating BlockD5846 07 (20
22、12)26.3.1 A gas flow controller is required for each test cell.6.3.2 Flowmeters shall have a scale length sufficiently longto permit accurate reading and control to within 5 % of fullscale.6.3.3 The total system accuracy shall meet or exceed thefollowing tolerances: Inlet pressure regulator within 0
23、.34 kPa(0.05 psig) of setpoint; total flow control system reproducibil-ity within 7 % of full scale; repeatability of measurementwithin 0.5 % of full scale.6.4 Oxidation Cell, borosilicate glass, as shown in Fig. 2,and as further described in Guide D4871. This consists of a testcell of borosilicate
24、glass, standard wall; 38 mm outsidediameter, 300 6 5-mm length, with open end fitted with a34/45 standard-taper, ground-glass outer joint.6.5 Gas Inlet Tube, as shown in Fig. 2, and as furtherdescribed in Guide D4871. This consists of an 8-mm outsidediameter glass tube, at least 455 long, lower end
25、with fusedcapillary 1.5 to 3.5 mm inside diameter. The capillary boreshall be 15 6 1 mm long. The lower tip is cut at a 45 angle.6.6 Basic Head, as shown in Fig. 2, and as further describedin Guide D4871. This is an air condenser, with 34/45 standard-taper, ground-glass inner joint, opening for gas
26、inlet tube,septum port for sample withdrawal, and exit tube to conductoff-gases and entrained vapors. Overall length shall be 125 65 mm.6.7 Test precision was developed using the universaloxidation/thermal stability test apparatus described in GuideD4871.6,7Alternate apparatus designs for sample hea
27、ting andfor temperature and flow control shall be acceptable providedthey are shown to maintain temperature and gas flow within thespecified limits.7. Reagents and Materials7.1 Reagent grade chemicals shall be used in all tests.Unless otherwise indicated, it is intended that all reagentsconform to t
28、he specifications of the Committee on AnalyticalReagents of the American Chemical Society, where suchspecifications are available.8Other grades may be used, pro-vided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determi
29、nation.7.2 Abrasive Cloth, silicon carbide, 100-grit with clothbacking.7.3 Acetone, reagent grade. (WarningAcetone is flam-mable and a health hazard.)7.4 Air, dry with dew point 60.7.5 Electrolytic Copper Wire, 1.63 mm in diameter (No. 14American Wire Gage or No. 16 Imperial Standard Wire Gage),99.9
30、 % purity, conforming to Specification B1, is preferred.7.6 Heptane, knock-test grade, conforming to the followingrequirements: (WarningnHeptane is flammable and ahealth hazard.)Density at 20C 0.6826 to 0.6839Refractive index at 20C 1.3876 to 1.3879Solidification temperature, min 90.72Distillation 5
31、0 % shall distill between 98.38 and98.48. Temperature rise between 20and 80 % recovered shall be 0.20 max7.7 Low-Metalloid Steel Wire, 1.59 mm in diameter (No. 16Washburn and Moen Gage). Carbon steel wire, soft brightannealed and free from rust, of Grade 1008 as described inSpecification A510, is pr
32、eferred. Similar wire conforming toBritish Standard 1829 is also satisfactory.7.8 Propanol-2 (iso-Propyl Alcohol), reagent grade.(Warningiso-Propyl alcohol is flammable and a healthhazard.)6The sole source of supply of the apparatus, including heating block, tempera-ture control system, and flow con
33、trol system, known to the committee at this timeis Falex Corp., 1020 Airpark Dr., Sugar Grove, IL 60554. If you are aware ofalternative suppliers, please provide this information to ASTM InternationalHeadquarters.7If you are aware of alternative suppliers, please provide this information toASTM Inte
34、rnational Headquarters. Your comments will receive careful consider-ation at a meeting of the responsible technical committee,1which you may attend.8Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For Suggestions on the testing of reagents notli
35、sted by the American Chemical Society, see Annual Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.FIG. 2 Test Cell, Including Oxidation Cell, Gas Inlet Tube, BasicHead
36、, and Finished Catalyst CoilD5846 07 (2012)37.9 Test Paper, chromatographic or filter paper, cellulose,medium porosity, qualitative or quantitative grade. Cut thepaper into 50 mm squares or use as larger sheets, ruled withhard pencil into 50 mm squares without cutting.7,9NOTE 1Paper sheets should be
37、 stored without folding, rolling, orbending, in a tightly closed container.8. Sampling8.1 Samples for this test can come from tanks, drums, smallcontainers, or operating equipment. Therefore, use the appli-cable apparatus and techniques described in Practice D4057 orIP 2546 to obtain suitable sample
38、s.8.2 Special precautions to preserve the integrity of a samplewill not normally be required. Follow good laboratory practice.Avoid undue exposure of samples to sunlight or strong directlight. Use only samples that are homogeneous on visualinspection.9. Preparation of Apparatus9.1 Cleaning Glassware
39、:9.1.1 Clean new glassware by washing with a hot detergentsolution, using a bristle brush; rinse thoroughly with tap water.When any visible deposits remain, soak with hot detergentsolution and repeat rinses. After final cleaning by soaking witha suitable cleaning solution7,10(WarningDue to extremeha
40、zards, chromic acid cleaning solution is not recommended.),rinse thoroughly with tap water then distilled water and dry atroom temperature or in an oven. A final rinse with iso-propylalcohol or acetone will hasten drying at room temperature.9.1.2 Clean used glassware immediately following the endof
41、a test. Drain the used oil completely. Rinse all glasswarewith heptane to remove traces of oil. Then clean the glasswareby the procedure described in 9.1.1 before re-use.9.2 Cleaning Catalyst:9.2.1 Clean equal lengths of iron and copper wire with wadsof absorbent cotton wet with heptane or other sat
42、uratedparaffinic solvent of comparable boiling point. Follow byabrasion with 100-grit silicon carbide abrasive cloth until freshmetal surfaces are exposed. Wipe with dry absorbent cotton toremove loose particles of metal and abrasives. Repeat withfresh cotton until no particles are visible. In the f
43、ollowingoperations, handle the catalyst with clean gloves (cotton,rubber, or plastic) to prevent contamination from oils on theskin.9.2.2 One procedure for preparing clean catalyst wire is tocut 0.50 6 0.01 m lengths of wire. Hold one end of the wiretightly with a pair of clean pliers or in a vise w
44、hile cleaningwith the abrasive cloth. Reverse ends of the wire and repeat.9.2.3 Alternately, clean a longer length of wire (3 to 5 m)and then cut 0.50 6 0.01 m lengths from the clean wire.9.3 Preparation of Catalyst Coil:9.3.1 Twist the iron and copper wires tightly together at oneend for three twis
45、ts. With the two wires parallel, wind the wiresaround a cylindrical mandrel to produce a single coil 15.9 to16.5 mm in inside diameter. The mandrel described in TestMethod D943 is satisfactory, but other cylindrical metal orwood stock can be used. Remove the coil from the mandrel andsecure the free
46、ends with three twists. Bend the twisted ends toconform to the shape of the spiral coil. Stretch the coil toproduce a finished coil with an overall length of 80 6 8mmasshown in Fig. 2.7,119.3.2 Store the catalyst coil in a dry, inert atmosphere untiluse. For storage up to 24 h, the coil can be store
47、d in heptane.Before use, inspect stored coils to ensure that no corrosionproducts or contaminating materials are present.9.4 Use a fresh catalyst coil for each test. Do not reuse coils.10. Procedure10.1 Adjust the heating block to maintain the oil in theoxidation test cell at 135 6 0.5C.10.1.1 Other
48、 test temperatures can be used but should bespecified.10.2 Weigh 100 6 1 g of test fluid into the oxidation testcell.10.3 Place a cleaned catalyst coil in the oil and fit the basichead and gas delivery tube into the test cell so that the tip of thegas delivery tube rests on the bottom of the test ce
49、ll inside thecatalyst coil, as shown in Fig. 3.10.4 Insert the test cell into the preheated constant tempera-ture block.Wait 0.5 to 1.0 h for the oil to warm to 135 6 0.5C.10.5 Connect an air delivery tube from the flow controlsystem to the gas inlet tube and adjust the flowmeter control todeliver dry air at 3 6 0.5 L/h. Record this time as the start ofthe test.10.6 Recheck the air flow and temperature after the test isunderway and at least once daily during the test. Adjust tomaintain the air flow and temperature as needed.NOTE 2Exhaust gases
