1、Designation: D1401 10Standard 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 Department of Defense.1. Scope*1.1 This test method covers measurement of the ab
3、ility ofpetroleum oils or synthetic fluids to separate from water.Although developed specifically for steam-turbine oils havingviscosities of 28.890 mm2/s at 40C, this test method may beused to test oils of other types having various viscosities andsynthetic fluids at other test temperatures. It is
4、recommended,however, that the test temperature be raised to 82 6 1C whentesting products more viscous than 90 mm2/s at 40C. Forhigher viscosity oils where there is insufficient mixing of oiland water, Test Method D2711 is recommended. Other testtemperatures such as 25C may also be used. A1% sodiumch
5、oloride (NaCl) solution or synthetic seawater may be used inplace of distilled water when testing certain oils or fuels usedin marine applications.1.2 When testing synthetic fluids whose relative densitiesare greater than that of water, the procedure is unchanged, butit should be noted that the wate
6、r 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. It is theresponsibility
7、 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. Referenced Documents2.1 ASTM Standards:2D665 Test Method for Rust-Preventing Characteristics o
8、fInhibited 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 Sampling of Petroleum andPetroleum Products2.2 ISO Standards:
9、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 chloride(NaCl) solution or synthetic seawater are stirred for 5 min in agraduated cyli
10、nder at 54C or 82C, 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 specification timelimit. If complete separation or emulsion reduction to 3 mL orless does not oc
11、cur after standing for 30 min or some otherspecification time limit, the volumes of oil (or fluid), water, andemulsion remaining at the 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-tami
12、nation and turbulence. It is used for specification 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, likeborosilicate glass, or a chemical equivalent. The inside diam-eter shall be no le
13、ss 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 be 225 to 260 mm. The graduation shall not bein error by more than 1 mL at any point on the scale.1This test method is under the ju
14、risdiction 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 July 1, 2010. Published July 2010. Originally approvedin 1964. Last previous edition approved in 2009 as D14
15、0109. DOI: 10.1520/D1401-10.2For 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 Org
16、anization for Standardization (ISO), 1, ch. dela Voie-Creuse, Case postale 56, CH-1211, Geneva 20, Switzerland, http:/www.iso.ch.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, Unit
17、ed States.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 beingmaintained at a test temperature to within 61C. The cylindershall be secured in a position so that the long
18、itudinal 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 forclear visual inspection of the oil (fluid), water, and emulsionlayer volumes while the cyli
19、nder remains immersed in the bath.5.3 Stirring Paddle, made of chromium-plated or stainlesssteel and conforming to the following dimensions:Length, mm 120 6 1.5Width, mm 19 6 0.5Thickness, mm 1.5 6 0.15Radius of curvature ofpaddle corners, mm1.6 maxIt is mounted on a vertical shaft of similar metal,
20、 approxi-mately 6 mm in diameter, connected to a drive mechanismwhich rotates the paddle on its longitudinal axis at 1500 6 15rpm. The apparatus is of such design that, when the cylinder isclamped in position and the paddle assembly is lowered intothe cylinder, a positive stop engages and holds the
21、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 than 1 mmfrom the axis of rotation. When not in operation, the paddleassembly can be lifted vertically to clear the
22、 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 Wiper, with or without inert rod support,composed of a material such as rubber, that is resistant to theoil or fl
23、uid.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 Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.4O
24、ther 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 WaterUnless otherwise indicated, referenceto water shall be understood to mean distilled, deionized wateras defined
25、 by Type I or Type II in Specification D1193 or Grade3inBS EN ISO 3696:1995.6.3 Acetone,(WarningHealth hazard, Flammable.)6.4 Toluene,(WarningFlammable.) Solvents with similarcleaning and solvency characteristics may be substituted fortoluene.6.5 Detergent, free rinsing, anionic detergent with a pH
26、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 graduated cylinder by removing any film ofoil (or fluid) with a thorough rinsing with toluene or solventwith similar clean
27、ing 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 cylinder in the detergent for at least 24 h. Rinsethoroughly with tap water and then with reagent water.8.1.1 Check the gla
28、ssware 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 for use. An additional soakin a mildly acidic solution may be necessary.NOTE 1Alternately, new glas
29、sware 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 paddle and shaft with absorbent cottonor tissue wet with toluene or solvent with similar cleaning andsolvency characterist
30、ics 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 6 1C, 82 6 1C or specifiedtest temperature and maintain it at that temperature throughoutthe test. Add reagent water to the graduated cylinder to re
31、achthe 40-mLmark when at test temperature. Typically 39.5 mLofwater at room temperature will expand to the 40-mL mark oncethe cylinder is placed in the bath at 54C; 39 mL if heating thesample to 82C. Invert the sample several times in the originalcontainer. Do not pour, shake, or stir samples to any
32、 greaterextent than necessary to prevent air entrainment. Pour the oil(or fluid) under test into the same cylinder until the top level ofthe oil reaches the 80-mL mark on the cylinder when at testtemperature.9.2 If initial volumetric measurements are made at roomtemperature, expansion occurring at t
33、he elevated test tempera-ture will have to be considered. For example, there will be atotal volumetric expansion of about 2 to 3 mL at 82C.Corrections to each volume reading at 82C, therefore, shouldbe made so that the total of the volume readings made for oils(or fluid), water, and emulsion does no
34、t exceed 80 mL. Analternative procedure which would avoid the corrections is 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 w
35、hen testing certain oilsor fuels used in marine applications.9.4 Secure the cylinder in place directly under the stirringpaddle. Lower the paddle into the cylinder until the stop4Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For Suggestions on
36、 the testing of reagents notlisted by the American Chemical Society, see 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 102engages at the required depth.
37、 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 and raisethe stirring assembly until it is just clear of the graduate. Wipethe paddle with a spatula or wiper, allowing the liquid thusremoved to d
38、rop back into the cylinder. At 5-min intervals, orat the specification time limit identified for the product beingtested, depending on the type of heating bath utilized, lift thecylinder out of the bath or inspect the sample through the glasspanel of the heating bath, and record the volumes of the o
39、il (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 sample.9.5 Several samples may be placed in the bath at thebeginning of the first analysis. While the first sample is being
40、observed, additional samples may be stirred. At no time duringa sample inspection shall an additional sample be added to theheating bath.10. Report10.1 Record Measurements at 5min IntervalsReport thefollowing information:(1) Type of water used.(2) Test temperature.(3) Time, in minutes, to reach 3 mL
41、 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.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
42、 mL water mL emulsion time, min! (1)The test may be aborted after 30 min when testing at 54C and60 min at 82C.10.1.2 When the test method is performed to determine ifthe sample meets a specification, report the test temperature.Report the time when either:(1) The product passes the product separabil
43、ity require-ments against which it is being tested, or(2) The test limit for water separability is exceeded (usually3mLemulsion or less for 30 min at 54C and 60 min at 82C).In addition to reporting the time, report the volume of eachlayer in millilitres. In both cases, report results as follows:mL o
44、il mL water 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$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.1
45、0.2 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. 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 wa
46、s ended.39-35-6 (60) More than 3 mL of emulsion 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. Th
47、e emulsion layer at 25 min exceeded 3 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 Oil (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
48、 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 Combinations 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) (Not
49、e 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 emulsion will not.10.4 The appearance of the oil/emulsion and water/emulsion interfaces may be described in the following terms:10.4.1 Well-defined, sharp.10.4.
