1、Designation: D 5846 02An American National StandardStandard Test Method forUniversal Oxidation Test for Hydraulic and Turbine OilsUsing the Universal Oxidation Test Apparatus1This standard is issued under the fixed designation D 5846; the number immediately following the designation indicates the ye
2、ar 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 (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers a procedure for evaluating th
3、eoxidation stability 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
4、turbine oils of 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 Th
5、e values stated in SI units are to be regarded as thestandard. 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-pri
6、ate safety and health 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. Refe
7、renced Documents2.1 ASTM Standards:A 510 Specification for General Requirements for WireRods and Coarse Round Wire, Carbon Steel2B1 Specification for Hard-Drawn Copper Wire3D 664 Test Method forAcid Number of Petroleum Productsby Potentiometric Titration4D 943 Test Method for Oxidation Characteristi
8、cs of Inhib-ited Mineral Oils4D 974 Test Method for Acid and Base Number by Color-Indicator Titration4D 3339 Test Method for Acid Number of Petroleum Prod-ucts by Semi-Micro Color Indicator Titration5D 4057 Practice for Manual Sampling of Petroleum andPetroleum Products5D 4740 Test Method for Stabil
9、ity and Compatibility ofResidual Fuels by Spot Test5D 4871 Guide for Universal Oxidation/Thermal StabilityTest Apparatus5D 5770 Test Method for Semi-Quantitative Micro Determi-nation of Acid Number of Used Lubricating Oils62.2 Institute of Petroleum Standard:7IP 2546 Practice for Sampling of Petrole
10、um Products;alternate to Practice D 40572.3 British Standard:8BS 1829 Specification for Carbon Steel Wire; alternate toSpecification A 5102.4 ASTM Adjuncts:Reference Spot Sheet (Test Method D 4740), for visualrating of blotter spots93. Terminology3.1 Definitions of Terms Specific to This Standard:3.
11、1.1 oxidation life, nof an oil, the time in hours requiredfor degradation of the oil under test.3.1.2 inhibited mineral oil, na petroleum oil containingadditives to retard oxidation.3.1.3 universal oxidation test, nthe apparatus and proce-dures described in Guide D 4871.4. Summary of Test Method4.1
12、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.1This test method is under the jurisdiction of ASTM Committee D02 on
13、Petroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.09.0D on Oxidation of Lubricants.Current edition approved Apr. 10, 2002. Published June 2002. Originallypublished as D 5846 - 95. Last previous edition D 5846 - 99.2Annual Book of ASTM Standards, Vol 01.03.3Annual
14、Book of ASTM Standards, Vol 02.03.4Annual Book of ASTM Standards, Vol 05.01.5Annual Book of ASTM Standards, Vol 05.02.6Annual Book of ASTM Standards, Vol 05.03.7Available from the Institute of Petroleum, 61 New Cavendish St., London,W1G 7AR, U.K.8Available from British Standards Institute, 389 Chisw
15、ick High Rd., London,W4 4AL, U.K.9Available from ASTM International Headquarters. Order ADJD 4740.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.4.2 The oil is considered to be degraded when either its acidnumber (measured by Test M
16、ethods D 974 or D 664) 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 of clear oil.5. Significance and Use5.1 Degradation of hydraulic f
17、luids 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 stability of petroleum-base oils. It should be recog-nized that correla
18、tion 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 D 4871, to provide a controlledconstant temperature for conducting the t
19、est.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 clearance of the 38 mmoutside diameter glass tube to the holes in
20、 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 D 4871, to maintainthe test oils in the heating block at 135 6 0.5C for the durationof the test.6.3 Gas Flow Control System, as shown in the up
21、per left inFig. 1, and as further described in Guide D 4871, to provide dryair at a flow rate of 3.0 6 0.5 L/h 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 %
22、 of fullscale.FIG. 1 Apparatus, Showing Gas Flow Control System, Temperature Control System, and Heating BlockD58460226.3.3 The total 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-
23、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 D 4871. This consists of atest cell of borosilicate glass, standard wall; 38 mm outsidediameter, 300 6 5-mm length, with o
24、pen 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 D 4871. This consists of an 8-mm outsidediameter glass tube, at least 455 long, lower end with fusedcapillary 1.5 to 3.5 mm inside diameter. The capillary bore
25、shall 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 D 4871. 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 condu
26、ctoff-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 GuideD 4871.10Alternate apparatus designs for sample heating andfor temperature and flow control shall be acceptable provide
27、dthey 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 the specifications of the Committee on AnalyticalReagents of the Amer
28、ican Chemical Society, where suchspecifications are available.11Other grades may be used,provided it is first acertained 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
29、.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 % purity, conforming to Specification B1, is preferred.7.6 Heptane, k
30、nock-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 50 % shall distill between 98.38 and98.48. Temperature rise between 20a
31、nd 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 A 510, is preferred. Similar wire conforming toBritish Standard 1829 is also sati
32、sfactory.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 use as larger sheets, ruled withha
33、rd pencil into 50 mm squares without cutting.1210A standard commercial apparatus has been found satisfactory for the purposeof this test method. This apparatus, including heating block, temperature controlsystem, flow control system, and glassware, is available from Falex Corp., 1020Airpark Dr., Sug
34、ar Grove, IL 60554. Glassware for the universal oxidation testapparatus is also available from W. A. Sales, Ltd., 419 Harvester Court, Wheeling,IL 60090.11Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents
35、 notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.12Whatman 1 grade, available in 57 by 46 cm sheets, have been f
36、oundsatisfactory for this test method. Paper sheets should be stored without folding,rolling, or bending, in a tightly closed container.FIG. 2 Test Cell, Including Oxidation Cell, Gas Inlet Tube, BasicHead, and Finished Catalyst CoilD58460238. Sampling8.1 Samples for this test can come from tanks, d
37、rums, smallcontainers, or operating equipment. Therefore, use the appli-cable apparatus and techniques described in Practice D 4057 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 u
38、ndue exposure of samples to sunlight or strong directlight. 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 v
39、isible deposits remain, soak with hot detergentsolution and repeat rinses. After final cleaning by soaking witha suitable cleaning solution13rinse thoroughly with tap waterthen distilled water and dry at room temperature or in an oven.A final rinse with iso-propyl alcohol or acetone will hastendryin
40、g 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 Catalyst:9.2.1 Clean equal lengths o
41、f 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 toremove loose particles of meta
42、l 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 tocut 0.50 6 0.01 m lengths of
43、 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 to 5 m)and then cut 0.50 6 0.01 m lengths from the clean wire.9.3 Preparation of Catalyst Coi
44、l: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 coil 15.9 to16.5 mm in inside diameter. The mandrel described in TestMethod D 943 is satisfactory, but other cylindrical me
45、tal orwood stock can be used. Remove the coil from the mandrel andsecure the free 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. 2.149.3.2 Store the catalyst coil in
46、 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 heatin
47、g block to maintain the oil in theoxidation test cell at 135 6 0.5C.10.1.1 Other 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
48、 cell so that the tip of the13Nochromix Reagent, available from Godax Laboratories, New York, NY, hasbeen found satisfactory for this purpose. Because of extreme hazards, chromic acidcleaning solution is not recommended.14Prepared catalyst coils for use with this test method are available from C and
49、P Catalyst, P.O. Box 520984, Tulsa, OK 74152.FIG. 3 Assembled Test Cell Ready to Insert Into Heating BlockD5846024gas delivery tube rests on the bottom of the test cell 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 after the test
