ASTM D1401-2012 Standard Test Method for Water Separability of Petroleum Oils and Synthetic Fluids《石油和合成液体的水分离性的标准试验方法》.pdf

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1、Designation:D140110D140112 Standard Test Method for Water Separability of Petroleum Oils and Synthetic Fluids 1 This standard is issued under the xed designation D1401; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of l

2、ast revision.Anumber in parentheses indicates the year of last reapproval.A superscript 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

3、of the ability of petroleum oils or synthetic uids to separate from water.Although developed specically for steam-turbine oils having viscosities of 28.890 mm 2 /s at 40C, this test method may be used to test oils of other types having various viscosities and synthetic uids at other test temperature

4、s. It is recommended, however, that the testtemperatureberaisedto8261Cwhentestingproductsmoreviscousthan90mm 2 /sat40C.Forhigherviscosityoilswhere there is insufficient mixing of oil and water,Test Method D2711 is recommended. Other test temperatures such as 25C may also beused.A1%sodiumcholoride(Na

5、Cl)solutionorsyntheticseawatermaybeusedinplaceofdistilledwaterwhentestingcertain oils or fuels used in marine applications. 1.2 When testing synthetic uids whose relative densities are greater than that of water, the procedure is unchanged, but it should be noted that the water will probably oat on

6、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, associated with its use. It is the responsibility of the user of th

7、is standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specic warning statements, see Section 6. 2. Referenced Documents 2.1 ASTM Standards: 2 D665Test Method for Rust-Preventing Characteristics of Inhibited Minera

8、l Oil in the Presence of Water D1141Practice for the Preparation of Substitute Ocean Water D1193Specication for Reagent Water D2711Test Method for Demulsibility Characteristics of Lubricating Oils D4057Practice for Manual Sampling of Petroleum and Petroleum Products 2.2 ISO Standards: 3 BS EN ISO 36

9、96:1995Water for analytical laboratory use Specication and test methods 3. Summary of Test Method 3.1 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 stirred for 5 min in a graduated cylinder at 54C

10、 or 82C, depending upon the viscosity of the test specimen or sample specication. The time required for the separation of the emulsion thus formed is recorded either after every 5 min or at the specication time limit. If complete separation or emulsion reduction to 3 mL or less does not occur after

11、standingfor30minorsomeotherspecicationtimelimit,thevolumesofoil(oruid),water,andemulsionremainingatthetime are reported. 4. Signicance and Use 4.1 Thistestmethodprovidesaguidefordeterminingthewaterseparationcharacteristicsofoilssubjecttowatercontamination and turbulence. It is used for specication o

12、f new oils and monitoring of in-service oils. 1 This test method is under the jurisdiction ofASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.C0.02 on Corrosion and Water/Air Separability. Current edition approved July 1, 2010May 15, 2012.

13、Published July 2010August 2012. Originally approved in 1964. Last previous edition approved in 20092010 as D140109.10. DOI: 10.1520/D1401-10.10.1520/D1401-12. 2 ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,orcontactASTMCustomerServiceatserviceastm.org.ForAnnualBookofASTMStandards volu

14、me 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, CH-1211, Geneva 20, Switzerland, http:/www.iso.ch. This document is not anASTM standard and is intended

15、only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because it may not be technically possible to adequately depict all changes accurately,ASTM recommends that users consult prior editions as appropriate. In all cases only the current ver

16、sion of the standard as published by ASTM is to be considered the official document. *ASummary 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 15. Apparatus 5.1 Cylinder, 100-mL,

17、graduated from 5 to 100 mL in 1.0-mL divisions, made of glass, heat-resistant glass, like borosilicate glass, or a chemical equivalent. 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.

18、 The overall height of the cylinder shall be 225 to 260 mm. The graduation shall not be in error by more than 1 mL at any point on the scale. 5.2 Heating Bath, sufficiently large and deep to permit the immersion of at least two test cylinders in the bath liquid up to their 85-mL graduations. The bat

19、h shall be capable of being maintained at a test temperature to within 61C. The cylinder shall be secured in a position so that the longitudinal axis of the paddle corresponds to the vertical center line of the cylinder during the stirring operation. It is recommended that the bath be constructed wi

20、th at least one transparent side that allows for clear visual inspection of the oil (uid), water, and emulsion layer volumes while the cylinder remains immersed in the bath. 5.3 Stirring Paddle, made of chromium-plated or stainless steel and conforming to the following dimensions: COLSPEC/colname=“c

21、ol2“ align=“center“ Length, mm 120 1.5 Length, mm 120 1.5 Width, mm 19 0.5 Width, mm 19 0.5 Thickness, mm 1.5 0.15 Thickness, mm 1.5 0.15 Radius of curvature of paddle corners, mm 1.6 max Itismountedonaverticalshaftofsimilarmetal,approximately6mmindiameter,connectedtoadrivemechanismwhichrotates thep

22、addleonitslongitudinalaxisat1500615rpm.Theapparatusisofsuchdesignthat,whenthecylinderisclampedinposition and the paddle assembly is lowered into the cylinder, a positive stop engages and holds the assembly when the lower edge of the paddle is 6 mm from the bottom of the cylinder. During the operatio

23、n of the stirrer, the center of the bottom edge of the paddle shall not deviate more than 1 mm from the axis of rotation. When not in operation, the paddle assembly can be lifted vertically to clear the top of the graduated cylinder. (WarningPaddle edges may be very sharp. Handle with care.) (Warnin

24、gA protective shield may be used to cover the rotating shaft of the stirrer.) 5.4 SpatulaorWiper,withorwithoutinertrodsupport,composedofamaterialsuchasrubber,thatisresistanttotheoiloruid. 6. Reagents 6.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated

25、, it is intended that all reagents shall conform to the specications of the Committee on Analytical Reagents of the American Chemical Society, where such specications are available. 4 Other grades may be used, provided it is rst ascertained that the reagent is of sufficiently high purity to permit i

26、ts use without lessening the accuracy of the determination. 6.2 Reagent WaterUnless otherwise indicated, reference to water shall be understood to mean distilled, deionized water as dened by Type I or Type II in Specication D1193 or Grade 3 in BS EN ISO 3696:1995. 6.3 Acetone, (Warning Health hazard

27、, Flammable.) 6.4 Toluene, (Warning Flammable.) Solvents with similar cleaning and solvency characteristics may be substituted for toluene. 6.5 Detergent, free rinsing, anionic detergent with a pH of 9.5 to 11. 7. Sampling 7.1 The test is very sensitive to small amounts of contamination. Take sample

28、s in accordance with Practice D4057. 8. Preparation ofApparatus 8.1 Clean the graduated cylinder by removing any lm of oil (or uid) with a thorough rinsing with toluene or solvent with similar cleaning and solvency characteristics followed by a wash rst with acetone and then with tap water. Clean th

29、e glassware with a suitable detergent (6.5). Rinse with tap water. Soak the cylinder in the detergent for at least 24 h. Rinse thoroughly with tap water and then with reagent water. 8.1.1 Checktheglasswareforcleanlinessbyaddingreagentwatertothecylinderandinvertingittodrainthewater.Ifthewater drains

30、with a smooth sheeting action and leaves behind no droplets, the glassware is clean for use.An additional soak in a mildly acidic solution may be necessary. NOTE1Alternately,newglasswaremaybeused,providedthattheyarethoroughlyrinsedwithreagentwaterandmeetthecleanlinessdenedbythe sheeting action as de

31、scribed in 8.1.1. 4 Reagent Chemicals, American Chemical Society Specications,American Chemical Society, Washington, DC. For Suggestions on the testing of reagents not listed by the American Chemical Society, see Annual Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the Unite

32、d States Pharmacopeia and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD. D140112 28.2 Clean the stirring paddle and shaft with absorbent cotton or tissue wet with toluene or solvent with similar cleaning and solvencycharacteristicsandairdry.Careshallbetakennottobendor

33、misalignthepaddleassemblyduringthecleaningoperation. 9. Procedure 9.1 Heat the bath liquid to 546 1C, 826 1C or specied test temperature and maintain it at that temperature throughout the test.Add reagent water to the graduated cylinder to reach the 40-mL mark when at test temperature. Typically 39.

34、5 mL of water at room temperature will expand to the 40-mLmark once the cylinder is placed in the bath at 54C; 39 mLif heating the sample to 82C. Invert the sample several times in the original container. Do not pour, shake, or stir samples to any greater extent than necessary to prevent air entrain

35、ment. Pour the oil (or uid) under test into the same cylinder until the top level of the oil reaches the 80-mL mark on the cylinder when at test temperature. 9.2 If initial volumetric measurements are made at room temperature, expansion occurring at the elevated test temperature will have to be cons

36、idered. For example, there will be a total volumetric expansion of about 2 to 3 mL at 82C. Corrections to each volume reading at 82C, therefore, should be made so that the total of the volume readings made for oils (or uid), water, and emulsion does not exceed 80 mL. An alternative procedure which w

37、ould avoid the corrections is to make the initial volumetric measurements at the test temperature. 9.3 A1%sodiumchloride(NaCl)solutionorsyntheticseawater,asdescribedinPractice D1141orTestMethod D665,maybe used in place of distilled water when testing certain oils or fuels used in marine applications

38、. 9.4 Secure the cylinder in place directly under the stirring paddle. Lower the paddle into the cylinder until the stop engages at the required depth. Start the stirrer and a stop watch simultaneously and adjust the stirrer, as required, to a speed of 1500 6 15 rpm.At the end of 5 min, stop the sti

39、rrer and raise the stirring assembly until it is just clear of the graduate.Wipe the paddle with a spatula or wiper, allowing the liquid thus removed to drop back into the cylinder.At 5-min intervals, or at the specication time limit identied for the product being tested, depending on the type of he

40、ating bath utilized, lift the cylinder out of the bath or inspect the sample through the glass panel of the heating bath, and record the volumes of the oil (or uid), water, and emulsion layers.Ifnecessary,additionallighting,suchasabacklightoranindooroodlight,maybeusedtoaidtheanalystintheinspection o

41、f the sample. 9.5 Several samples may be placed in the bath at the beginning of the rst analysis. While the rst 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. 10. Report 10.1 Record Measuremen

42、ts at 5min Intervals 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 o

43、f water. 10.1.1 In addition to reporting the time, report the volume of each layer in millilitres. In all cases, report results as follows: mLoil2mLwater2mLemulsiontime,min! (1) The test may be aborted after 30 min when testing at 54C and 60 min at 82C. 10.1.2 When the test method is performed to de

44、termine if the sample meets a specication, report the test temperature. Report the time when either: (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 3mLemulsion or less for 30 min at 54C an

45、d 60 min at 82C). In addition to reporting the time, report the volume of each layer in millilitres. In both cases, report results as follows: mLoil2mLwater2mLemulsiontime,min! (2) 10.1.3 Some samples may produce a hazy oil layer without an emulsion layer. In situations where the water layer is 37mL

46、, report the upper layer as the oil layer. If there are two layers, 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 the manner shown in the examples provided in 10.1. D140112 340-40-0 (20) Complete separation occurred i

47、n 20 min. More than 3 mL of emulsion had remained at 15 min. 39-38-3 (20) Complete separation had not occurred, but the emulsion reduced to 3 mL so the test was ended. 39-35-6 (60) More than 3 mL of emulsion remained after 60 min39 mL of oil, 35 mL of water, and 6 mL of emulsion. 41-37-2 (20) Comple

48、te separation had not occurred but the emulsion layer reduced to 3 mL or less after 20 min. 43-37-0 (30) The emulsion layer reduced to 3 mL or less after 30 min. The emulsion layer at 25 min exceeded 3 mL, for example, 0-36-44 or 43-33-4. 40-40-0 (20) Complete separation occurred in 20 min. More tha

49、n 3 mL of emulsion had remained at 15 min. 39-38-3 (20) Complete separation had not occurred, but the emulsion reduced to 3 mL so the test was ended. 39-35-6 (60) More than 3 mL of emulsion remained after 60 min39 mL of oil, 35 mL of water, and 6 mL of emulsion. 41-37-2 (20) Complete separation had not occurred but the emulsion layer reduced to 3 mL or less after 20 min. 43-37-0 (30) The emulsion layer reduced to 3 mL or less after 30 min. The emulsion layer at 25 min exceeded 3 mL, for example, 0-36-44 or 43-