1、Designation: D5846 07 (Reapproved 2017)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.1.3.1 ExceptionThe values given in parentheses are forinformation only.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
6、safety, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to use.Identified hazardous chemicals are listed in 7.3, 7.6, and 7.8.Before using this test method, refer to suppliers safety labels,Material Safety Data Sheets, and other technical literatu
7、re.1.5 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 TechnicalBarriers
8、 to Trade (TBT) Committee.2. Referenced Documents2.1 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 Metho
9、d for Oxidation Characteristics of InhibitedMineral 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 M
10、ethod for Cleanliness and Compatibility ofResidual 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 Pract
11、ice for Sampling of Petroleum Products;alternate to 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:1This test method is under the ju
12、risdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.09.0D on Oxidation of Lubricants.Current edition approved Oct. 1, 2017. Published November 2017. Originallyapproved in 1995. Last previous edition approved in 2012
13、as D584607(2012).DOI: 10.1520/D5846-07R17.2For 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 Ene
14、rgy Institute, 61 New Cavendish St., London, WIG 7AR,U.K., http:/www.energyinst.org.uk.4Available from 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
15、 2000.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of
16、 International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.13.1.1 inhibited mineral oil, na petroleum oil containingadditives to retard oxidation.3.1.2 oxidation life, nof an oil, the time in hours requiredfor degradation o
17、f the oil under test.3.1.3 universal oxidation test, nthe apparatus and proce-dures described in Guide D4871.4. Summary of Test Method4.1 An oil sample is contacted with air at 135 C in thepresence of copper and iron metals. The acid number and spotforming tendency of the oil are measured daily. The
18、 test isterminated when the oxidation life of the oil has been reached.4.2 The oil is considered 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
19、oil isplaced onto a filter paper it shows a clearly defined dark spotsurrounded by a ring 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 unf
20、it for furtheruse.5.2 This test method can be used to estimate the relativeoxidation stability 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
21、.1 Heating Block, as shown on the right in Fig. 1, and asfurther described in Guide D4871, 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
22、 The test cells shall fit into the block to a depth of225 mm 6 5 mm. When centered, the side clearance of the 38FIG. 1 Apparatus, Showing Gas Flow Control System, Temperature Control System, and Heating BlockD5846 07 (2017)2mm outside diameter glass tube to the holes in the aluminumblock shall not e
23、xceed 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 C 6 0.5 C for theduration of the test.6.3 Gas Flow Control System, as shown in the upper left inFig. 1, and as fu
24、rther described in Guide D4871, to provide dryair at a flow rate of 3.0 Lh 6 0.5 Lh to each test cell.6.3.1 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 tot
25、al system accuracy shall meet or exceed thefollowing tolerances: Inlet pressure regulator within 0.34 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 sho
26、wn in Fig. 2,and as further described in Guide D4871. This consists of a testcell of borosilicate glass, standard wall; 38 mm outsidediameter, 300 mm 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 furtherdescrib
27、ed in Guide D4871. This consists of an 8 mm outsidediameter glass tube, at least 455 long, lower end with fusedcapillary 1.5 mm to 3.5 mm inside diameter. The capillary boreshall be 15 mm 6 1 mm long. The lower tip is cut at a 45angle.6.6 Basic Head, as shown in Fig. 2, and as further describedin Gu
28、ide D4871. This is an air condenser, with 34/45 standard-taper, ground-glass inner joint, opening for gas inlet tube,septum port for sample withdrawal, and exit tube to conductoff-gases and entrained vapors. Overall length shall be125 mm 6 5 mm.6.7 Test precision was developed using the universaloxi
29、dation/thermal stability test apparatus described in GuideD4871.6,7Alternate apparatus designs for sample heating 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
30、chemicals shall be used in all tests.Unless otherwise indicated, it is intended that all reagentsconform to the 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
31、that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.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 Electr
32、olytic Copper Wire, 1.63 mm in diameter (No. 14American Wire Gage or No. 16 Imperial Standard Wire Gage),99.9 % purity, conforming to Specification B1, is preferred.7.6 Heptane, knock-test grade, conforming to the followingrequirements: (WarningnHeptane is flammable and ahealth hazard.)6The sole sou
33、rce of supply of the apparatus, including heating block, tempera-ture control system, and flow control 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 InternationalHe
34、adquarters.7If you are aware of alternative suppliers, please provide this information toASTM International 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 Specific
35、ations, AmericanChemical Society, Washington, DC. For Suggestions on the testing of reagents notlisted 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 Conventio
36、n, Inc. (USPC), Rockville,MD.FIG. 2 Test Cell, Including Oxidation Cell, Gas Inlet Tube, BasicHead, and Finished Catalyst CoilD5846 07 (2017)3Density at 20 C 0.6826 to 0.6839Refractive index at 20 C 1.3876 to 1.3879Solidification temperature, min 90.72Distillation 50 % shall distill between 98.38 an
37、d98.48. 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 preferred. Similar wire conforming t
38、oBritish Standard 1829 is also satisfactory.7.8 Propanol-2 (iso-Propyl Alcohol), reagent grade.(Warningiso-Propyl alcohol is flammable and a healthhazard.)7.9 Test Paper, chromatographic or filter paper, cellulose,medium porosity, qualitative or quantitative grade. Cut thepaper into 50 mm squares or
39、 use as larger sheets, ruled withhard pencil into 50 mm squares without cutting.7,9NOTE 1Paper sheets should be 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. Therefor
40、e, use the appli-cable apparatus and techniques described in Practice D4057 orIP 2546 to obtain suitable samples.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 directlig
41、ht. Use only samples that are homogeneous on visualinspection.9. Preparation of Apparatus9.1 Cleaning Glassware: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
42、and repeat rinses. After final cleaning by soaking witha suitable cleaning solution7,10(WarningDue to extremehazards, 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-propylalcoho
43、l or acetone will hasten drying at room temperature.9.1.2 Clean used glassware immediately following the endof 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 Cataly
44、st:9.2.1 Clean equal lengths of iron and copper wire with wadsof absorbent cotton wet with heptane or other saturatedparaffinic solvent of comparable boiling point. Follow byabrasion with 100-grit silicon carbide abrasive cloth until freshmetal surfaces are exposed. Wipe with dry absorbent cotton to
45、remove loose particles of metal and abrasives. Repeat withfresh cotton until no particles are visible. In the followingoperations, 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
46、tocut 0.50 m 6 0.01 m lengths of wire. Hold one end of the wiretightly with a pair of clean pliers or in a vise while cleaningwith the abrasive cloth. Reverse ends of the wire and repeat.9.2.3 Alternately, clean a longer length of wire (3 m to 5 m)and then cut 0.50 m 6 0.01 m lengths from the clean
47、wire.9.3 Preparation of Catalyst Coil:9.3.1 Twist the iron and copper wires tightly together at oneend for three twists. With the two wires parallel, wind the wiresaround a cylindrical mandrel to produce a single coil15.9 mm to 16.5 mm in inside diameter. The mandrel de-scribed in Test Method D943 i
48、s satisfactory, but other cylin-drical metal or wood stock can be used. Remove the coil fromthe mandrel and secure the free ends with three twists. Bendthe twisted ends to conform to the shape of the spiral coil.Stretch the coil to produce a finished coil with an overall lengthof 80 mm 6 8 mm as sho
49、wn 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 stored 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 C 6 0.5 C.10.1.1 Other test temperatures can be used but should bespecified.10.2 Weigh 100 g 6 1 g of test fluid into the
