1、Designation: D1401 18Standard 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 last revi
2、sion. 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 measurement of t
3、he ability ofpetroleum oils or synthetic fluids to separate from water.Although developed specifically for steam-turbine oils havingviscosities of 28.8 mm2/s to 90 mm2/s at 40 C, this testmethod may be used to test oils of other types having variousviscosities and synthetic fluids at other test temp
4、eratures. It isrecommended, however, that the test temperature be raised to82 C 6 1 C when testing products more viscous than90 mm2/s at 40 C. For higher viscosity oils where there isinsufficient mixing of oil and water, Test Method D2711 isrecommended. Other test temperatures such as 25 C may alsob
5、e used. A 1 % sodium choloride (NaCl) solution or syntheticseawater may be used in place of distilled water when testingcertain oils or fuels used in marine applications.1.2 When testing synthetic fluids whose relative densitiesare greater than that of water, the procedure is unchanged, butit should
6、 be noted that the water will probably float on theemulsion or liquid.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use.
7、It is theresponsibility of the user of this standard to establish appro-priate safety, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to use.For specific warning statements, see Section 7.1.5 This international standard was developed in accor-dan
8、ce 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 to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Sta
9、ndards:2D665 Test Method for Rust-Preventing Characteristics ofInhibited Mineral Oil in the Presence of WaterD1141 Practice for the Preparation of Substitute OceanWaterD1193 Specification for Reagent WaterD2711 Test Method for Demulsibility Characteristics ofLubricating OilsD4057 Practice for Manual
10、 Sampling of Petroleum andPetroleum ProductsD4175 Terminology Relating to Petroleum Products, LiquidFuels, 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 suspension of fine globule
11、s of one ormore liquids in another liquid.3.1.2 interface, na common boundary between differentphases of a substance.3.1.3 phase separation, nthe formation of two layers, anaqueous constituent and a hydrophobic constituent, separatedby either a common boundary or a layer of emulsion; typically,the a
12、queous portion will be the lower phase, but for certainfluids whose relative densities are greater than that of water, theaqueous portion will be the upper phase.4. Summary of Test Method4.1 A test specimen consisting of a 40 mL sample and a40 mL quantity of distilled water, or 1 % sodium chloride(N
13、aCl) solution or synthetic seawater are stirred for 5 min in agraduated cylinder at 54 C or 82 C, depending upon the1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.C0 on Turbine O
14、ils.Current edition approved March 1, 2018. Published March 2018. Originallyapproved in 1964. Last previous edition approved in 2012 as D1401 121. DOI:10.1520/D1401-18.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual
15、 Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from International Organization for Standardization (ISO), 1, ch. dela Voie-Creuse, Case postale 56, CH-1211, Geneva 20, Switzerland, http:/www.iso.ch.*A Summary of Changes section a
16、ppears at the end of this standardCopyright 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 Prin
17、ciples for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.1viscosity of the test specimen or sample specification. The timerequired for the separation of the emulsion thus formed isrecorded eith
18、er after every 5 min or at the specification timelimit. If complete separation or emulsion reduction to 3 mL orless does not occur after standing for 30 min or some otherspecification time limit, the volumes of oil (or fluid), water, andemulsion remaining at the time are reported.5. Significance and
19、 Use5.1 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 of newoils and monitoring of in-service oils.6. Apparatus6.1 Cylinder, 100 mL, graduated from 5 mL to 100 mL in1.0 mL div
20、isions, made of glass, heat-resistant glass, likeborosilicate glass, or a chemical equivalent. The inside diam-eter shall be no less than 27 mm and no more than 30 mmthroughout its length, measured from the top to a point 6 mmfrom the bottom of the cylinder. The overall height of thecylinder shall b
21、e 225 mm to 260 mm. The graduation shall notbe in error by more than 1 mL at any point on the scale.6.2 Heating 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 t
22、est temperature to within 61 C. The cylindershall be secured in a position so that the longitudinal axis of thepaddle corresponds to the vertical center line of the cylinderduring the stirring operation. It is recommended that the bathbe constructed with at least one transparent side that allows for
23、clear visual inspection of the oil (fluid), water, and emulsionlayer volumes while the cylinder remains immersed in the bath.6.3 Stirring Paddle, made of chromium-plated or stainlesssteel and conforming to the following dimensions:Length, mm 120 1.5Width, mm 19 0.5Thickness, mm 1.5 0.15Radius of cur
24、vature ofpaddle corners, mm1.6 maxIt is mounted on a vertical shaft of similar metal, approxi-mately 6 mm in diameter, connected to a drive mechanismwhich rotates the paddle on its longitudinal axis at 1500 rpm 615 rpm. The apparatus is of such design that, when the cylinderis clamped in position an
25、d the paddle assembly is lowered intothe cylinder, a positive stop engages and holds the assemblywhen the lower edge of the paddle is 6 mm from the bottom ofthe cylinder. During the operation of the stirrer, the center ofthe bottom edge of the paddle shall not deviate more than1 mm from the axis of
26、rotation. When not in operation, thepaddle assembly can be lifted vertically to clear the top of thegraduated cylinder. (WarningPaddle edges may be verysharp. Handle with care.) (WarningA protective shield maybe used to cover the rotating shaft of the stirrer.)6.4 Spatula or Wiper, with or without i
27、nert rod support,composed of a material such as rubber, that is resistant to theoil or fluid.7. Reagents7.1 Purity of ReagentsReagent 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 Analyt
28、ical Reagents of the American Chemical Society,where such specifications are available.4Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.7.2 Reagent WaterUnless otherwise indi
29、cated, referenceto water shall be understood to mean distilled, deionized wateras defined by Type I or Type II in Specification D1193 or Grade3 in BS EN ISO 3696:1995.7.3 Acetone, (Warning Health hazard, Flammable.)7.4 Toluene, (Warning Flammable.) Solvents with simi-lar cleaning and solvency charac
30、teristics may be substituted fortoluene.7.5 Detergent, free rinsing, anionic detergent with a pH of9.5 to 11.8. Sampling8.1 The test is very sensitive to small amounts of contami-nation. Take samples in accordance with Practice D4057.9. Preparation of Apparatus9.1 Clean the graduated cylinder by rem
31、oving any film ofoil (or fluid) with a thorough rinsing with toluene or solventwith similar cleaning and solvency characteristics followed bya wash first with acetone and then with tap water. Clean theglassware with a suitable detergent (7.5). Rinse with tap water.Soak the cylinder in the detergent
32、for at least 24 h. Rinsethoroughly with tap water and then with reagent water.9.1.1 Check the glassware for cleanliness by adding reagentwater to the cylinder and inverting it to drain the water. If thewater drains with a smooth sheeting action and leaves behindno droplets, the glassware is clean fo
33、r use. An additional soakin a mildly acidic solution may be necessary.NOTE 1Alternatively, new glassware may be used, provided that theyare thoroughly rinsed with reagent water and meet the cleanliness definedby the sheeting action as described in 9.1.1.9.2 Clean the stirring paddle and shaft with a
34、bsorbent cottonor tissue wet with toluene or solvent with similar cleaning andsolvency characteristics and air dry. Care shall be taken not tobend or misalign the paddle assembly during the cleaningoperation.10. Procedure10.1 Heat the bath liquid to 54 C 6 1 C, 82 C 6 1Corspecified test temperature
35、and maintain it at that temperaturethroughout the test. Add reagent water to the graduated4Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For Suggestions on the testing of reagents notlisted by the American Chemical Society, see Annual Standard
36、s for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.D1401 182cylinder to reach the 40 mL mark when at test temperature.Typically 39.5 mL of water at room temperature will expand t
37、othe 40 mL mark once the cylinder is placed in the bath at54 C; 39 mL if heating the sample to 82 C. Invert the sampleseveral times in the original container. Do not pour, shake, orstir samples to any greater extent than necessary to prevent airentrainment. Pour the oil (or fluid) under test into th
38、e samecylinder until the top level of the oil reaches the 80 mL markon the cylinder when at test temperature.10.2 If initial volumetric measurements are made at roomtemperature, expansion occurring at the elevated test tempera-ture will have to be considered. For example, there will be atotal volume
39、tric expansion of about 2 mL to 3 mL at 82 C.Corrections to each volume reading at 82 C, therefore, shouldbe made so that the total of the volume readings made for oils(or fluid), water, and emulsion does not exceed 80 mL. Analternative procedure which would avoid the corrections is tomake the initi
40、al volumetric measurements at the test tempera-ture.10.3 A 1 % sodium chloride (NaCl) solution or syntheticseawater, as described in Practice D1141 or Test Method D665,may be used in place of distilled water when testing certain oilsor fuels used in marine applications.10.4 Secure the cylinder in pl
41、ace 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 rpm 6 15 rpm. At the end of 5 min, stop the stirrer andraise the stirring ass
42、embly until it is just clear of the graduate.Wipe the paddle with a spatula or wiper, allowing the liquidthus removed to drop back into the cylinder.At 5 min intervals,or at the specification time limit identified for the product beingtested, depending on the type of heating bath utilized, lift thec
43、ylinder out of the bath or inspect the sample through the glasspanel of the heating bath, and record the volumes of the oil (orfluid), water, and emulsion layers. If necessary, additionallighting, such as a backlight or an indoor flood light, may beused to aid the analyst in the inspection of the sa
44、mple.10.5 Several samples may be placed in the bath at thebeginning of the first analysis. While the first sample is beingobserved, additional samples may be stirred. At no time duringa sample inspection shall an additional sample be added to theheating bath.11. Report11.1 Record Measurements at 5 m
45、in IntervalsReport thefollowing 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 mLemulsion, 40 mL of oil, and 40 mL of water.11.1.1 In ad
46、dition to reporting the time, report the volume ofeach layer in millilitres. In all cases, report results as follows:mL oil 2 mL water 2 mL emulsion time,min! (1)The test may be aborted after 30 min when testing at 54 Cand 60 min at 82 C.11.1.2 When the test method is performed to determine ifthe sa
47、mple meets a specification, report the test temperature.Report the time when either:(1) The product passes the product separability require-ments against which it is being tested, or(2) The test limit for water separability is exceeded (usu-ally 3 mL emulsion or less for 30 min at 54 C and 60 min at
48、82 C).In addition to reporting the time, report the volume of eachlayer in millilitres. In both cases, report results as follows:mL oil 2 mL water 2 mL emulsion time,min! (2)11.1.3 Some samples can produce only two layers. Insituations where the aqueous layer is 37 mL, report thesecond layer as the
49、oil layer. However, if the volume of theaqueous layer is 43 mL and is to be reported as emulsion.11.2 For uniformity, test results may be reported in themanner shown in the examples provided in 11.1.40-40-0 (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 emulsion remained after60 min39 mL of oil, 35 mL of water, and 6 mL ofemulsion.41-37-2 (20) Complete separat
