1、Designation: D1401 18D1401 18aStandard Test Method forWater Separability of Petroleum Oils and Synthetic Fluids1This standard is issued under the fixed designation D1401; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of
2、last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the U.S. Department of Defense.1. Scope*1.1 This test method covers measure
3、ment of the ability of petroleum oils or synthetic fluids to separate from water. Althoughdeveloped specifically for steam-turbine oils having viscosities of 28.8 mm2/s to 90 mm2/s at 40 C, this test method may be usedto test oils of other types having various viscosities and synthetic fluids at oth
4、er test temperatures. It is recommended, however,that the test temperature be raised to 82 C 6 1 C when testing products more viscous than 90 mm2/s at 40 C. For higherviscosity oils where there is insufficient mixing of oil and water, Test Method D2711 is recommended. Other test temperatures suchas
5、25 C may also be used. A 1 % sodium choloride (NaCl) solution or synthetic seawater may be used in place of distilled waterwhen testing certain oils or fuels used in marine applications.1.2 When testing synthetic fluids whose relative densities are greater than that of water, the procedure is unchan
6、ged, but itshould be noted that the water will probably float on the emulsion or liquid.1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.4 This standard does not purport to address all of the safety concerns, if any, asso
7、ciated with its use. It is the responsibilityof the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability ofregulatory limitations prior to use. For specific warning statements, see Section 7.1.5 This international standard was dev
8、eloped in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Docum
9、ents2.1 ASTM Standards:2D665 Test Method for Rust-Preventing Characteristics of Inhibited Mineral Oil in the Presence of WaterD1141 Practice for the Preparation of Substitute Ocean WaterD1193 Specification for Reagent WaterD2711 Test Method for Demulsibility Characteristics of Lubricating OilsD4057
10、Practice for Manual Sampling of Petroleum and Petroleum ProductsD4175 Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants2.2 ISO Standards:3BS EN ISO 3696:1995 Water for analytical laboratory useSpecification and test methods3. Terminology3.1 Definitions:3.1.1 emulsion, na suspe
11、nsion of fine globules of one or more liquids in another liquid.3.1.2 interface, na common boundary between different phases of a substance.1 This test method is under the jurisdiction ofASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcom
12、mitteeD02.C0 on Turbine Oils.Current edition approved March 1, 2018April 1, 2018. Published March 2018April 2018. Originally approved in 1964. Last previous edition approved in 20122018 asD1401 12D1401 18.1. DOI: 10.1520/D1401-18.10.1520/D1401-18A.2 For referencedASTM standards, visit theASTM websit
13、e, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 Available from International Organization for Standardization (ISO), 1, ch. de la Voie-Creuse, Case postale 56,
14、 CH-1211, Geneva 20, Switzerland, http:/www.iso.ch.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accur
15、ately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor
16、Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13.1.3 phase separation, nthe formation of two layers, an aqueous constituent and a hydrophobic constituent, separated byeither a common boundary or a layer of emulsion; typically, the aqueous portion will be the lower phase, but for
17、 certain fluidswhose relative densities are greater than that of water, the aqueous portion will be the upper phase.4. Summary of Test Method4.1 A test specimen consisting of a 40 mL sample and a 40 mL quantity of distilled water, or 1 % sodium chloride (NaCl)solution or synthetic seawater are stirr
18、ed for 5 min in a graduated cylinder at 54 C or 82 C, depending upon the viscosity of thetest specimen or sample specification. The time required for the separation of the emulsion thus formed is recorded either afterevery 5 min or at the specification time limit. If complete separation or emulsion
19、reduction to 3 mL or less does not occur afterstanding for 30 min or some other specification time limit, the volumes of oil (or fluid), water, and emulsion remaining at the timeare reported.5. Significance and Use5.1 This test method provides a guide for determining the water separation characteris
20、tics of oils subject to water contaminationand turbulence. It is used for specification of new oils and monitoring of in-service oils.6. Apparatus6.1 Cylinder, 100 mL, graduated from 5 mL to 100 mL in 1.0 mL divisions, made of glass, heat-resistant glass, like borosilicateglass, or a chemical equiva
21、lent. The inside diameter shall be no less than 27 mm and no more than 30 mm throughout its length,measured from the top to a point 6 mm from the bottom of the cylinder. The overall height of the cylinder shall be 225 mm to260 mm. The graduation shall not be in error by more than 1 mL at any point o
22、n the scale.6.2 Heating Bath, sufficiently large and deep to permit the immersion of at least two test cylinders in the bath liquid up to their85 mL graduations. The bath shall be capable of being maintained at a test temperature to within 61 C. The cylinder shall besecured in a position so that the
23、 longitudinal axis of the paddle corresponds to the vertical center line of the cylinder during thestirring operation. It is recommended that the bath be constructed with at least one transparent side that allows for clear visualinspection of the oil (fluid), water, and emulsion layer volumes while
24、the cylinder remains immersed in the bath.6.3 Stirring Paddle, made of chromium-plated or stainless steel and conforming to the following dimensions:Length, mm 120 1.5Width, mm 19 0.5Thickness, mm 1.5 0.15Radius of curvature ofpaddle corners, mm1.6 maxIt is mounted on a vertical shaft of similar met
25、al, approximately 6 mm in diameter, connected to a drive mechanism which rotatesthe paddle on its longitudinal axis at 1500 rpm 6 15 rpm. The apparatus is of such design that, when the cylinder is clamped inposition and the paddle assembly is lowered into the cylinder, a positive stop engages and ho
26、lds the assembly when the lower edgeof the paddle is 6 mm from the bottom of the cylinder. During the operation of the stirrer, the center of the bottom edge of thepaddle shall not deviate more than 1 mm from the axis of rotation. When not in operation, the paddle assembly can be liftedvertically to
27、 clear the top of the graduated cylinder. (WarningPaddle edges may be very sharp. Handle with care.) (WarningAprotective shield may be used to cover the rotating shaft of the stirrer.)6.4 Spatula or Wiper, with or without inert rod support, composed of a material such as rubber, that is resistant to
28、 the oil or fluid.7. Reagents7.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that allreagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, wheresuch specifications ar
29、e available.4 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently highpurity to permit its use without lessening the accuracy of the determination.7.2 Reagent WaterUnless otherwise indicated, reference to water shall be understood to mean distilled, deioniz
30、ed water asdefined by Type I or Type II in Specification D1193 or Grade 3 in BS EN ISO 3696:1995.7.3 Acetone, (Warning Health hazard, Flammable.)7.4 Toluene, (Warning Flammable.) Solvents with similar cleaning and solvency characteristics may be substituted fortoluene.7.5 Detergent, free rinsing, an
31、ionic detergent with a pH of 9.5 to 11.4 Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For Suggestions on the testing of reagents not listed bythe American Chemical Society, see Annual Standards for Laboratory Chemicals, BDH Ltd., Poole, Dors
32、et, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.D1401 18a28. Sampling8.1 The test is very sensitive to small amounts of contamination. Take samples in accordance with Practice D4057.9. Preparation of Apparatus9.1 Clean the
33、 graduated cylinder by removing any film of oil (or fluid) with a thorough rinsing with toluene or solvent withsimilar cleaning and solvency characteristics followed by a wash first with acetone and then with tap water. Clean the glasswarewith a suitable detergent (7.5). Rinse with tap water. Soak t
34、he cylinder in the detergent for at least 24 h. Rinse thoroughly withtap water and then with reagent water.9.1.1 Check the glassware for cleanliness by adding reagent water to the cylinder and inverting it to drain the water. If the waterdrains with a smooth sheeting action and leaves behind no drop
35、lets, the glassware is clean for use. An additional soak in a mildlyacidic solution may be necessary.NOTE 1Alternatively, new glassware may be used, provided that they are thoroughly rinsed with reagent water and meet the cleanliness defined bythe sheeting action as described in 9.1.1.9.2 Clean the
36、stirring paddle and shaft with absorbent cotton or tissue wet with toluene or solvent with similar cleaning andsolvency characteristics and air dry. Care shall be taken not to bend or misalign the paddle assembly during the cleaning operation.10. Procedure10.1 Heat the bath liquid to 54 C 6 1 C, 82
37、C 6 1 C or specified test temperature and maintain it at that temperaturethroughout the test. Add reagent water to the graduated cylinder to reach the 40 mL mark when at test temperature. Typically39.5 mL of water at room temperature will expand to the 40 mL mark once the cylinder is placed in the b
38、ath at 54 C; 39 mL ifheating the sample to 82 C. Invert the sample several times in the original container. Do not pour, shake, or stir samples to anygreater extent than necessary to prevent air entrainment. Pour the oil (or fluid) under test into the same cylinder until the top levelof the oil reac
39、hes the 80 mL mark on the cylinder when at test temperature.10.2 If initial volumetric measurements are made at room temperature, expansion occurring at the elevated test temperature willhave to be considered. For example, there will be a total volumetric expansion of about 2 mLto 3 mLat 82 C. Corre
40、ctions to eachvolume reading at 82 C, therefore, should be made so that the total of the volume readings made for oils (or fluid), water, andemulsion does not exceed 80 mL.An alternative procedure whichthat would avoid the corrections is to make the initial volumetricmeasurements at the test tempera
41、ture. Oils with high surface tension can create a highly curved meniscus with the reagent waterresulting in a reagent water level falling below the 40 mL line after the oil is added. For those types of oils, the original readingof 40 mL (without the addition of the oil) is valid and shall be used. D
42、o not adjust the reagent water volume.10.3 A 1 % sodium chloride (NaCl) solution or synthetic seawater, as described in Practice D1141 or Test Method D665, maybe used in place of distilled water when testing certain oils or fuels used in marine applications.10.4 Secure the cylinder in place directly
43、 under the stirring paddle. Lower the paddle into the cylinder until the stop engagesat the required depth. Start the stirrer and a stop watch simultaneously and adjust the stirrer, as required, to a speed of 1500 rpm6 15 rpm.At the end of 5 min, stop the stirrer and raise the stirring assembly unti
44、l it is just clear of the graduate. Wipe the paddlewith a spatula or wiper, allowing the liquid thus removed to drop back into the cylinder. At 5 min intervals, or at the specificationtime limit identified for the product being tested, depending on the type of heating bath utilized, lift the cylinde
45、r out of the bathor inspect the sample through the glass panel of the heating bath, and record the volumes of the oil (or fluid), water, and emulsionlayers. If necessary, additional lighting, such as a backlight or an indoor flood light, may be used to aid the analyst in the inspectionof the sample.
46、10.5 Several samples may be placed in the bath at the beginning of the first analysis. While the first sample is being observed,additional samples may be stirred. At no time during a sample inspection shall an additional sample be added to the heating bath.11. Report11.1 Record Measurements at 5 min
47、 IntervalsReport the following information:(1) Type of water used.(2) Test temperature.(3) Time, in minutes, to reach 3 mL or less of emulsion.(4) Time, in minutes, to reach 37 mL of water.(5) Time, in minutes, to reach a complete break of 0 mL emulsion, 40 mL of oil, and 40 mL of water.11.1.1 In ad
48、dition to reporting the time, report the volume of each layer in millilitres. In all cases, report results as follows:mL oil2mL water2mL emulsion time,min! (1)The test may be aborted after 30 min when testing at 54 C and 60 min at 82 C.11.1.2 When the test method is performed to determine if the sam
49、ple meets a specification, report the test temperature. Reportthe time when either:D1401 18a3(1) The product passes the product separability requirements against which it is being tested, or(2) The test limit for water separability is exceeded (usually 3 mL emulsion or less for 30 min at 54 C and 60 min at 82 C).In addition to reporting the time, report the volume of each layer in millilitres. In both cases, report results as follows:mL oil2mL water2mL emulsion time,min! (2)11.1.3 Some samples can produce only two layers. In situations
