1、Designation: D 1401 09Standard Test Method forWater Separability of Petroleum Oils and Synthetic Fluids1This 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 re
2、vision. 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
3、ability 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 i
4、s 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 D 2711 is recommended. Other testtemperatures such as 25C may also be used. A 1% sodi
5、umcholoride (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
6、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. It is theresponsibi
7、lity 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:2D 665 Test Method for Rust-Preventing Characterist
8、ics ofInhibited Mineral Oil in the Presence of WaterD 1141 Practice for the Preparation of Substitute OceanWaterD 1193 Specification for Reagent WaterD 2711 Test Method for Demulsibility Characteristics ofLubricating OilsD 4057 Practice for Manual Sampling of Petroleum andPetroleum Products2.2 ISO S
9、tandards: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 agradu
10、ated cylinder 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 do
11、es 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.4. Significance and Use4.1 This test method provides a guide for determining thewater separation characteristics of oils subject to water
12、 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 to 100 mL in1.0-mL divisions, made of glass, heat-resistant glass, likeborosilicate glass, or a chemical equivalent. The inside diam-eter shall
13、 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 the1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of
14、 SubcommitteeD02.C0.02 on Corrosion and Water/Air Separability.Current edition approved July 1, 2009. Published July 2009. Originally approvedin 1964. Last previous edition approved in 2002 as D 140102.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Serv
15、ice at serviceastm.org. For Annual 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.
16、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, United States.cylinder shall be 225 to 260 mm. The graduation shall not bein error by more than 1 mL at any point on the scale.5.2
17、 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 longitudinal axis
18、 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 cylinder remains
19、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, approxi-mate
20、ly 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 assemblywhen
21、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 top of thegr
22、aduated cylinder. (WarningPaddle edges may be verysharp. Handle with care.) (WarningA protective shield maybe used to cover the rotating shaft of the stirrer.)5.4 Glass Rod (Policeman), covered with a material such asrubber, resistant to the oil or fluid.6. Reagents6.1 Purity of ReagentsReagent grad
23、e 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.4Other grades may beused, provided it is first asce
24、rtained 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 by Type I or Type II in Specification D 1193 orG
25、rade 3 in BS 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 of9.5 to 11.7. Sampling7.1 The test is very se
26、nsitive to small amounts of contami-nation. Take samples in accordance with Practice D 4057.8. Preparation of Apparatus8.1 Clean the graduated cylinder by removing any film ofoil (or fluid) with a thorough rinsing with toluene or solventwith similar cleaning and solvency characteristics followed bya
27、 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 glassware for cleanliness by adding reagentwater
28、 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 glassware may be used, provided that theyare thor
29、oughly 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 characteristics and air dry. Care shall be taken not tobe
30、nd 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 reachthe 40-mLmark when at test temperature. Ty
31、pically 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 greaterextent than necessary to prevent air
32、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 the elevated test tempera-ture will have to be
33、 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 not exceed 80 mL. Analternative procedure which
34、 would avoid the corrections is tomake the initial volumetric measurements at the test tempera-ture.9.3 A 1 % sodium chloride (NaCl) solution or syntheticseawater, as described in Practice D 1141 or Test MethodD 665, may be used in place of distilled water when testingcertain oils or fuels used in m
35、arine 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 the testing of reagents notlisted by the
36、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.D1401092engages at the required depth. Start the stirrer and a stop watchsimultan
37、eously 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 policeman, allowing the liquid thus removedto drop back into the cylinder. At 5-min intervals, or
38、 at thespecification time limit identified for the product being tested,inspect the sample through the glass panel of the heating bath,and record the volumes of the oil (or fluid), water, andemulsion layers. If necessary, additional lighting, such as abacklight or an indoor flood light, may be used
39、to aid theanalyst 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 beingobserved, additional samples may be stirred. At no time duringa sample inspection shall an additional sample be added to theheating ba
40、th.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 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
41、 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 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 met
42、hod is performed to determine 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 (usually3mLemulsion or les
43、s 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 oil mL water mL emulsion time, min! (2)10.1.3 Some samples may produce a hazy oil layer withoutan emulsion layer. In situations where t
44、he 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.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
45、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 after 60min39 mL of oil, 35 mL of water, and 6 mL ofemulsion.41-37-2 (20) Com
46、plete 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. The 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 thefoll
47、owing 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 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)
48、(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) (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 p
49、rincipal 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.10.4.2 Ill-defined, bubbles.10.4.3 Ill-defined, lace.10.5 Report the test temperature if other than 54C and theaqueous medium if other than
