1、Designation: D 1401 02An American National StandardStandard Test Method forWater Separability of Petroleum Oils and Synthetic Fluids1This standard is issued under the fixed designation D 1401; the number immediately following the designation indicates the year oforiginal adoption or, in the case of
2、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.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1 This test meth
3、od covers measurement of the ability ofpetroleum oils or synthetic fluids to separate from water.NOTE 1Although developed specifically for steam-turbine oils havingviscosities of 28.890 cSt (mm2/s) at 40C, this test method can be usedto test oils of other types having various viscosities and synthet
4、ic fluids. Itis recommended, however, that the test temperature be raised to 82 6 1Cwhen testing products more viscous than 90 cSt (mm2/s) at 40C. Forhigher viscosity oils where there is insufficient mixing of oil and water,Test Method D 2711, is recommended.Other test temperatures such as 25C can a
5、lso be used.When testing synthetic fluids whose relative densities are greater thanthat of water, the procedure is unchanged, but it should be noted that thewater will probably float on the emulsion or liquid.1.2 The values stated in SI units are to be regarded as thestandard. The values given in pa
6、rentheses 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 regulatory limita
7、tions prior to use. For specificprecautionary statements, see 6.3-6.5.2. Referenced Documents2.1 ASTM Standards:D 665 Test Method for Rust-Preventing Characteristics ofInhibited Mineral Oil in the Presence of Water2D 1141 Practice for the Preparation of Substitute OceanWater3D 1193 Specification for
8、 Reagent Water4D 2711 Test Method for Demulsibility Characteristics ofLubricating Oils2D 4057 Practice for Manual Sampling of Petroleum andPetroleum Products53. Summary of Test Method3.1 A test specimen consisting of a 40-mL sample and a40-mL quantity of distilled water (Note 3) are stirred for 5 mi
9、nat 54C (Note 1) in a graduated cylinder. The time required forthe separation of the emulsion thus formed is recorded eitherafter every 5 min or at the specification time limit. If completeseparation or emulsion reduction to 3 mL or less does not occurafter standing for 30 min or some other specific
10、ation time limit,the volumes of oil (or fluid), water, and emulsion remaining atthe time are reported.4. Significance and Use4.1 This test method provides a guide for determining thewater separation characteristics of oils subject to water con-tamination and turbulence. It is used for specification
11、of newoils and monitoring of in-service oils.5. Apparatus5.1 Cylinder, 100-mL, graduated from 5 to 100 mL in1.0-mL divisions, made of glass, heat-resistant glass,6or achemical equivalent. The inside diameter shall be no less than27 mm and no more than 30 mm throughout its length,measured from the to
12、p to a point 6 mm from the bottom of thecylinder. The overall height of the cylinder shall be 225 to 260mm. The graduation shall not be in error by more than 1 mL atany point on the scale.5.2 Heating Bath, sufficiently large and deep to permit theimmersion of at least two test cylinders in the bath
13、liquid up totheir 85-mL graduations. The bath shall be capable of beingmaintained at a temperature of 54 6 1C (Note 1), and shall befitted with clamps which hold the cylinder in a position so thatthe longitudinal axis of the paddle corresponds to the verticalcenter line of the cylinder during the st
14、irring operation. Theclamps shall hold the cylinder securely while its contents arebeing stirred.5.3 Stirring Paddle, made of chromium-plated or stainlesssteel and conforming to the following dimensions:Length, mm (in.) 120 6 1.5 (434 6116)Width, mm (in.) 19 6 0.5 (34 6164)Thickness, mm (in.) 1.5 (1
15、16)1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.C0.02 on Corrosion and Water/Air Separability.Current edition approved Nov. 10, 2002. Published December 2002. Originallyapproved in 1964. Last
16、 previous edition approved in 1998 as D 140198.2Annual Book of ASTM Standards, Vol 05.01.3Annual Book of ASTM Standards, Vol 11.02.4Annual Book of ASTM Standards, Vol 11.01.5Annual Book of ASTM Standards, Vol 05.02.6Borosilicate glass has been found satisfactory for this purpose.1Copyright ASTM Inte
17、rnational, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.It is mounted on a vertical shaft of similar metal, approxi-mately 6 mm ( in.) in diameter, connected to a drivemechanism which rotates the paddle on its longitudinal axis at1500 6 15 rpm. The apparatus is
18、 of such design that, when thecylinder is clamped in position and the paddle assembly islowered into the cylinder, a positive stop engages and holds theassembly when the lower edge of the paddle is 6 mm from thebottom of the cylinder. During the operation of the stirrer, thecenter of the bottom edge
19、 of the paddle shall not deviate morethan 1 mm from the axis of rotation. When not in operation, thepaddle assembly can be lifted vertically to clear the top of thegraduated cylinder.6. Reagents6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is
20、 intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.7Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use
21、 without lessening theaccuracy of the determination.6.2 Purity of WaterUnless otherwise indicated, referenceto water shall be understood to mean reagent water as definedby Type II in Specification D 1193.6.3 Cleaning Solvents, Light-Hydrocarbon, such as precipi-tation naphtha (WarningHealth hazard)
22、for petroleum oils.Use other appropriate solvents for dissolving synthetic fluids.6.4 Acetone,(WarningHealth hazard, Flammable.)6.5 Cleaning Reagent, Cleaning by either hot NOCHRO-MIX8(WarningCorrosive. Health hazard oxidizer), or a24-h soak at room temperature in MICRO9solution gaveacceptable, stat
23、istically equivalent results in round-robin test-ing.7. Sampling7.1 The test is very sensitive to small amounts of contami-nation. Take samples in accordance with Practice D 4057.8. Preparation of Apparatus8.1 Clean the graduated cylinder by removing any film ofoil (or fluid) with cleaning solvent f
24、ollowed by a wash firstwith acetone and then with tap water. The glassware shall befurther cleaned with a suitable cleaning reagent. Rinse thor-oughly with tap water and then with reagent water. Inspect thecylinders for any residue or water droplets adhering to theinside walls. Both conditions indic
25、ate a need for additionalcleaning.8.2 Clean the stirring paddle and shaft with absorbent cottonor tissue wet with cleaning solvent and air dry. Care must betaken not to bend or misalign the paddle assembly during thecleaning operation.9. Procedure9.1 Heat the bath liquid to 54 6 1C (Note 1) and main
26、tainit at that temperature throughout the test. Add reagent water(Note 2 and Note 3) to the graduated cylinder up to the 40-mLmark and then add to the same cylinder a representative sampleof the oil (or fluid) under test until the top level of the oilreaches the 80-mL mark on the cylinder. Place the
27、 cylinder inthe bath and allow the contents to reach bath temperature.Heating time may vary with type of equipment and can reachup to 30 min.NOTE 2If initial volumetric measurements are made at room tempera-ture, expansion occurring at the elevated test temperature will have to beconsidered. For exa
28、mple, there will be a total volumetric expansion ofabout 2 to 3 mL at 82C. Corrections to each volume reading at 82C,therefore, should be made so that the total of the volume readings madefor oils (or fluid), water, and emulsion does not exceed 80 mL. Analternative procedure which would avoid the co
29、rrections is to make theinitial volumetric measurements at the test temperature.NOTE 3A 1 % sodium chloride (NaCl) solution or synthetic sea water,as described in Practice D 1141 or Test Method D 665, can be used inplace of distilled water when testing certain oils or fuels used in marineapplication
30、s.9.2 Clamp the cylinder in place directly under the stirringpaddle. Lower the paddle into the cylinder until the stopengages at the required depth. Start the stirrer and a stop watchsimultaneously and adjust the stirrer, as required, to a speed of1500 6 15 rpm. At the end of 5 min, stop the stirrer
31、 and raisethe stirring assembly until it is just clear of the graduate. Wipethe paddle with a policeman (Note 4), allowing the liquid thusremoved to drop back into the cylinder. Remove the cylinderfrom the retaining clamps and transfer it carefully to anothersection of the bath. At 5-min intervals,
32、or at the specificationtime limit identified for the product being tested, lift thecylinder out of the bath (see Note 5), inspect, and record thevolumes of the oil (or fluid), water, and emulsion layers.NOTE 4The policeman should be made of material resistant to the oilor fluid.NOTE 5It is not neces
33、sary to lift the cylinders out of the bath forinspection if the heating bath is constructed with at least one transparentside that allows for clear visual inspection of the oil (fluid), water, andemulsion layer volumes while the cylinder remains immersed in the bath.10. Report10.1 Recording Measurem
34、ents at 5min IntervalsRecordthe time until either (1) the product passes the water separa-bility requirements it is being tested against, or (2) the test limitfor water separability is exceeded (usually 3-mL emulsion orless for 30 min at 54C and 60 min at 82C). The maximumvolume to be reported as th
35、e oil layer is 43 mL (see Note 6).For uniformity, test results may be reported in the mannershown in the following examples:7Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Che
36、mical 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.8The sole source of supply of NOCHROMIX known to the committee at thistime is Godax Laborator
37、ies Inc., 720B Erie Ave., Takoma Park, MD 20912. If youare aware of alternative suppliers, please provide this information to ASTMInternational Headquarters. Your comments will receive careful consideration at ameeting of the responsible technical committee1, which you may attend.9The sole source of
38、 supply of MICRO known to the committee at this time isInternational Products Corp., P.O. Box 70, Burlington, NJ 08016. If you are awareof alternative suppliers, please provide this information to ASTM InternationalHeadquarters. Your comments will receive careful consideration at a meeting of theres
39、ponsible technical committee1, which you may attend.D140102240-40-0 (20) Complete separation occurred in 20 min. More than3 mL of emulsion had remained at 15 min.39-38-3 (20) Complete separation had not occurred, but theemulsion reduced to 3 mL so the test was ended.39-35-6 (60) More than 3 mL of em
40、ulsion remained after 60min39 mL of oil, 35 mL of water, and 6 mL ofemulsion.41-37-2 (20) Complete separation had not occurred but the emul-sion layer reduced to 3 mL or less after 20 min.43-37-0 (30) The emulsion layer reduced to 3 mL or less after 30min. The emulsion layer at 25 min exceeded 3 mL,
41、for example, 0-36-44 or 43-33-4.10.1.1 Recording Measurements at the Specification TimeRequirement OnlyRecord the volumes for oil (or fluid),water, and emulsion layers at the specification time limit anddetermine whether (1) the product passes the water separabilityrequirements it is being tested ag
42、ainst, or (2) the test limit forwater separability is exceeded (usually 3mL emulsion or lessfor 30 min at 54C and 60 min at 82C). The maximum volumeto be reported as the oil layer is 43 mL (see Note 6). Foruniformity, test results may be reported in the manner shown inthe examples provided in 10.1.1
43、0.2 The appearance of each layer may be described in thefollowing terms:10.2.1 Oil (or Oil Rich) Layer:10.2.1.1 Clear.10.2.1.2 Hazy (Note 7).10.2.1.3 Cloudy (or milky) (Note 7).10.2.1.4 Combinations of 10.2.1.1-10.2.1.3.10.2.2 Water or Water-Rich Layer:10.2.2.1 Clear.10.2.2.2 Lacy or bubbles present
44、, or both.10.2.2.3 Hazy (Note 7).10.2.2.4 Cloudy (or milky) (Note 7).10.2.2.5 Combinations of 10.2.2.1-10.2.2.4.10.2.3 Emulsion:10.2.3.1 Loose and lacy.10.2.3.2 Cloudy (or milky) (Note 8).10.2.3.3 Creamy (like mayonnaise) (Note 8).10.2.3.4 Combinations of 10.2.3.1-10.2.3.3.NOTE 6Certain oils may pro
45、duce a hazy oil layer. In situations wherethe measurement of the oil and water layer indicates essentially completeseparation, the upper layer should be reported as oil. If there are two layersand if the upper layer is more than 43 mL, this layer should be consideredthe emulsion layer.NOTE 7A hazy l
46、ayer is defined as being translucent and a cloudy layeropaque.NOTE 8The principal difference between cloudy and creamy emul-sions is that the former is quite fluid and probably unstable while the latterhas a thick consistency and is probably stable. A cloudy emulsion willreadily flow from an incline
47、d graduate while a creamy emulsion will not.10.3 The appearance of the oil/emulsion and water/emulsion interfaces may be described in the following terms:10.3.1 Well-defined, sharp.10.3.2 Ill-defined, bubbles.10.3.3 Ill-defined, lace.10.4 Report the test temperature if other than 54C and theaqueous
48、medium if other than distilled water.11. Precision and Bias11.1 PrecisionThe precision of this test method wasobtained on steam-turbine oils having viscosities of 28.8 to 90cSt (mm2/s) at 40C and using time to 3 mL or less emulsionas the test completion. This precision is expressed graphicallyin Fig
49、. 1. The graph shows the maximum allowable deviationUse of ChartCalculate the mean test result in minutes. Enter chart at the zero point, A, on the ordinate and move to the right on the abscissa to point B. Computeand locate the deviation points C+ and C, from the mean test result. If the deviation points fall within the repeatability area, then the results are within the precision ofthe test.ExampleAn oil has emulsion of 40-40-0 (10 min) and 40-40-0 (15 min). The mean test result is 12.5 min (B) and the deviation from the mean is +2.5 (C+) an
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