Standard Test Method for Water Separability of …

1 Designation: D 1401 02An American National StandardStandard Test Method forWater Separability of petroleum oils and Synthetic Fluids1 This 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 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 Standard has been approved for use by agencies of the Department of This test Method covers measurement of the ability ofpetroleum oils or synthetic fluids to separate from Although developed specifically for steam-turbine oils havingviscosities of 90 cSt (mm2/s) at 40 C, this test Method can be usedto test oils of other types having various viscosities and synthetic fluids. Itis recommended, however, that the test temperature be raised to 8261 Cwhen testing products more viscous than 90 cSt (mm2/s) at 40 C.

2 Forhigher viscosity oils where there is insufficient mixing of oil and Water ,Test Method D 2711, is test temperatures such as 25 C can also be 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 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for 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 limitations prior to specificprecautionary statements, see Referenced 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 Reagent Water4D 2711 Test Method for Demulsibility Characteristics ofLubricating Oils2D 4057 Practice for Manual Sampling of petroleum andPetroleum Products53.

3 Summary of Test A test specimen consisting of a 40-mL sample and a40-mL quantity of distilled Water (Note 3) are stirred for 5 minat 54 C (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 specification time limit,the volumes of oil (or fluid), Water , and emulsion remaining atthe time are Significance and 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 of newoils and monitoring of in-service , 100-mL, graduated from 5 to 100 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 top to a point 6 mm from the bottom of thecylinder.

4 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 Bath, sufficiently large and deep to permit theimmersion of at least two test cylinders in the bath liquid up totheir 85-mL graduations. The bath shall be capable of beingmaintained at a temperature of 5461 C (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 stirring operation. Theclamps shall hold the cylinder securely while its contents arebeing Paddle, made of chromium-plated or stainlesssteel and conforming to the following dimensions:Length, mm (in.) (43 461 16)Width, mm (in.) (3 461 64)Thickness, mm (in.) (1 16)1 This test Method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of on Corrosion and Water /Air edition approved Nov.

5 10, 2002. Published December 2002. Originallyapproved in 1964. Last previous edition approved in 1998 as D 1401 Book of ASTM Standards, Vol Book of ASTM Standards, Vol Book of ASTM Standards, Vol Book of ASTM Standards, Vol glass has been found satisfactory for this ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United 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 at1500615 rpm. The apparatus is 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 of the paddle shall not deviate morethan 1 mm from the axis of rotation.

6 When not in operation, thepaddle assembly can be lifted vertically to clear the top of thegraduated of Reagents Reagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the of Water Unless otherwise indicated, referenceto Water shall be understood to mean reagent Water as definedby Type II in Specification D Solvents, Light-Hydrocarbon, such as precipi-tation naphtha (Warning Health hazard) for petroleum other appropriate solvents for dissolving synthetic ,(Warning Health hazard, Flammable.) Reagent, Cleaning by either hot NOCHRO-MIX8(Warning Corrosive. Health hazard oxidizer), or a24-h soak at room temperature in MICRO9solution gaveacceptable, statistically equivalent results in round-robin The test is very sensitive to small amounts of contami-nation.

7 Take samples in accordance with Practice D Preparation of Clean the graduated cylinder by removing any film ofoil (or fluid) with cleaning solvent followed 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 indicate a need for 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 Heat the bath liquid to 5461 C (Note 1) and maintainit 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.

8 Place the cylinder inthe bath and allow the contents to reach bath time may vary with type of equipment and can reachup to 30 If initial volumetric measurements are made at room tempera-ture, expansion occurring at the elevated test temperature will have to beconsidered. For example, there will be a total volumetric expansion ofabout 2 to 3 mL at 82 C. Corrections to each volume reading at 82 C,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 corrections is to make theinitial volumetric measurements at the test A 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 Clamp the cylinder in place directly under the stirringpaddle.

9 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 of1500615 rpm. At the end of 5 min, stop the stirrer 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, 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 The policeman should be made of material resistant to the oilor It is not necessary 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 Measurements at 5 min Intervals Recordthe 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 54 C and 60 min at 82 C).

10 The maximumvolume to be reported as theoil layeris 43 mL (see Note 6).For uniformity, test results may be reported in the mannershown in the following examples:7 Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, seeAnalar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, , and theUnited States Pharmacopeiaand National Formulary, Pharmacopeial Convention, Inc. (USPC), Rockville, sole source of supply of NOCHROMIX known to the committee at thistime is Godax Laboratories Inc., 720 B Erie Ave., Takoma Park, MD 20912. If youare aware of alternative suppliers, please provide this information to ASTMI nternational Headquarters. Your comments will receive careful consideration at ameeting of the responsible technical committee1, which you may sole source of supply of MICRO known to the committee at this time isInternational Products Corp.