1、Designation: D1401 121Standard 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 rev
2、ision. 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.1NOTESubsection 11.1 was corrected editorially in Oc
3、tober 2015.1. Scope*1.1 This test method covers measurement of the 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 h
4、aving variousviscosities and synthetic fluids at other test temperatures. 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 D27
5、11 isrecommended. Other test temperatures such as 25 C may alsobe used. A1% 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 greate
6、r than that of water, the procedure is unchanged, butit should 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 addres
7、s 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 use. For specificwarning statements, see Section 6.2. Reference
8、d Documents2.1 ASTM Standards: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 OilsD4
9、057 Practice for Manual Sampling of Petroleum andPetroleum Products2.2 ISO Standards:3BS EN ISO 3696:1995 Water for analytical laboratory use Specification and test methods3. Summary of Test Method3.1 A test specimen consisting of a 40 mL sample and a40 mL quantity of distilled water, or 1 % sodium
10、chloride(NaCl) solution or synthetic seawater are stirred for 5 min in agraduated cylinder at 54 C or 82 C, depending upon theviscosity of the test specimen or sample specification. The timerequired for the separation of the emulsion thus formed isrecorded either after every 5 min or at the specific
11、ation 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.1This test method is under the jurisdiction of ASTM Commit
12、tee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.C0.02 on Corrosion and Water/Air Separability.Current edition approved May 15, 2012. Published August 2012. Originallyapproved in 1964. Last previous edition approved in 2010 as D140110. DO
13、I:10.1520/D1401-12E01.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from International Organizat
14、ion 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 appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United State
15、s14. 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 of newoils and monitoring of in-service oils.5. Apparatus5.1 Cylinder, 100 mL, graduated from 5 mL t
16、o 100 mL in1.0 mL divisions, 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 o
17、f thecylinder shall be 225 mm to 260 mm. The graduation shall notbe in error by more than 1 mL at any point on the scale.5.2 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 b
18、eingmaintained at a test 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
19、 side that allows forclear visual inspection of the oil (fluid), water, and emulsionlayer volumes while the cylinder remains immersed in the bath.5.3 Stirring Paddle, made of chromium-plated or stainlesssteel and conforming to the following dimensions:Length, mm 120 1.5Width, mm 19 0.5Thickness, mm
20、1.5 0.15Radius of curvature 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 c
21、lamped in position and 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
22、 mm from the axis of 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.)5.4 Spatula or Wip
23、er, with or without inert rod support,composed of a material such as rubber, that is resistant to theoil or fluid.6. Reagents6.1 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
24、 Commit-tee on Analytical 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.6.2 Reagent Water
25、Unless otherwise indicated, 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 3696:1995.6.3 Acetone, (Warning Health hazard, Flammable.)6.4 Toluene, (Warning Flammable.) Solvents with simi-lar cleanin
26、g and solvency characteristics may be substituted fortoluene.6.5 Detergent, free rinsing, anionic detergent with a pH of9.5 to 11.7. Sampling7.1 The test is very sensitive to small amounts of contami-nation. Take samples in accordance with Practice D4057.8. Preparation of Apparatus8.1 Clean the grad
27、uated cylinder by removing 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 (6.5). Rinse with tap water.Soak the cylin
28、der in the detergent for at least 24 h. Rinsethoroughly with tap water and then with reagent water.8.1.1 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
29、glassware is clean for use. An additional soakin a mildly acidic solution may be necessary.NOTE 1Alternately, new glassware may be used, provided that theyare thoroughly rinsed with reagent water and meet the cleanliness definedby the sheeting action as described in 8.1.1.8.2 Clean the stirring padd
30、le and shaft with absorbent 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.9. Procedure9.1 Heat the bath liquid to 54 C 6 1 C, 82 C 6 1Corspecified
31、test temperature and maintain it at that temperaturethroughout the test. Add reagent water to the graduatedcylinder to reach the 40 mL mark when at test temperature.Typically 39.5 mL of water at room temperature will expand tothe 40 mL mark once the cylinder is placed in the bath at54 C; 39 mL if he
32、ating the sample to 82 C. Invert the sampleseveral times in the original container. Do not pour, shake, or4Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For Suggestions on the testing of reagents notlisted by the American Chemical Society, see
33、 Annual Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.D1401 1212stir samples to any greater extent than necessary to prevent airentrainment. Pour the oil (or fluid)
34、under test into the samecylinder until the top level of the oil reaches the 80 mL markon the cylinder when at test temperature.9.2 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
35、 be atotal volumetric 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
36、 tomake the initial volumetric measurements at the test tempera-ture.9.3 A1 % 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.9.4 Secure the
37、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 rpm 6 15 rpm. At the end of 5 min, stop the stirrer andraise th
38、e stirring assembly 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 utili
39、zed, lift thecylinder 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 inspec
40、tion of the sample.9.5 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.10. Report10.1 Record Measur
41、ements at 5 min 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
42、.10.1.1 In addition 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.10.1.2 When the test method is performed to deter
43、mine ifthe sample 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
44、and 60 min at82 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)10.1.3 Some samples may produce a hazy oil layer withoutan emulsion layer. In situations where the water layer is
45、37 mL, report the upper layer as the oil layer. If there are twolayers, and the water layer is 43 mL, report the upper layer as the emulsion layer.10.2 For uniformity, test results may be reported in themanner shown in the examples provided in 10.1.40-40-0 (20) Complete separation occurred in 20 min
46、. 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 separation h
47、ad not occurred but theemulsion layer reduced to 3 mL or less after 20 min.43-37-0 (30) The emulsion layer reduced to 3 mL or less after30 min. The emulsion layer at 25 min exceeded3 mL, for example, 0-36-44 or 43-33-4.10.3 The appearance of each layer may be described in thefollowing terms:10.3.1 O
48、il (or Oil Rich) Layer:10.3.1.1 Clear.10.3.1.2 Hazy (Note 2).10.3.1.3 Cloudy (or milky) (Note 2).10.3.1.4 Combinations of 10.3.1.1 10.3.1.3.10.3.2 Water or Water-Rich Layer:10.3.2.1 Clear.10.3.2.2 Lacy or bubbles present, or both.10.3.2.3 Hazy (Note 2).10.3.2.4 Cloudy (or milky) (Note 2).10.3.2.5 Co
49、mbinations of 10.3.2.1 10.3.2.4.10.3.3 Emulsion:10.3.3.1 Loose and lacy.10.3.3.2 Cloudy (or milky) (Note 3).10.3.3.3 Creamy (like mayonnaise) (Note 3).10.3.3.4 Combinations of 10.3.3.1 10.3.3.3.NOTE 2Ahazy layer is defined as being translucent and a cloudy layeropaque.NOTE 3The 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 inclined graduate while a creamy emuls
