ASTM D95-2005(2010) Standard Test Method for Water in Petroleum Products and Bituminous Materials by Distillation《蒸馏法测定石油产品及沥青材料中水的试验方法》.pdf

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1、Designation: D95 05 (Reapproved 2010)Designation: Manual of Petroleum Measurement Standards (MPMS), Chapter 10.5Designation: 74/82 (88)Highway Transportation StandardAASHTO No. T55Standard Test Method forWater in Petroleum Products and Bituminous Materials byDistillation1This standard is issued unde

2、r the fixed designation D95; the number immediately following the designation indicates the year of originaladoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscriptepsilon () indicates an editorial change since the

3、last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1 This test method covers the determination of water inthe range from 0 to 25 % volume in petroleum products, tars,and other bituminous materials by the distillation method.NOTE 1Vo

4、latile water-soluble material, if present, may be measuredas water.1.2 The specific products considered during the develop-ment of this test method are listed in Table 1. For bituminousemulsions refer to Test Method D244. For crude oils, refer toTest Method D4006 (API MPMS Chapter 10.2).NOTE 2With s

5、ome types of oil, satisfactory results may be obtainedfrom Test Method D1796 (API MPMS Chapter 10.6).1.3 The values stated in SI units are to be regarded as thestandard. The values in parentheses are for information only.1.4 This standard does not purport to address all of thesafety concerns, if any

6、, 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 specific hazardstatements, see Section 6.2. Referenced Documents2.1 ASTM Standards:2D244

7、Test Methods and Practices for Emulsified AsphaltsD1796 Test Method for Water and Sediment in Fuel Oils bythe Centrifuge Method (Laboratory Procedure)D4006 Test Method for Water in Crude Oil by DistillationD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automa

8、tic Sampling of Petroleum andPetroleum ProductsD5854 Practice for Mixing and Handling of Liquid Samplesof Petroleum and Petroleum ProductsE123 Specification for Apparatus for Determination of Wa-ter by Distillation2.2 API Standards:3MPMS Chapter 8.1 Manual Sampling of Petroleum andPetroleum Products

9、 (ASTM Practice D4057)MPMS Chapter 8.2 Automatic Sampling of Petroleum andPetroleum Products (ASTM Practice D4177)MPMS Chapter 8.3 Mixing and Handling of Liquid Samplesof Petroleum and Petroleum Products (ASTM PracticeD5854)MPMS Chapter 10.2 Determination of Water in Crude Oilby the Distillation Met

10、hod (ASTM Test Method D4006)MPMS Chapter 10.6 Test Method for Water and Sediment inFuel Oils by the Centrifuge Method (Laboratory Proce-dure) (ASTM Test Method D1796)3. Terminology3.1 Definitions:3.1.1 bituminous material, nin petroleum technology,ablack or dark-colored very viscous liquid or semi-s

11、olid com-posed principally of high molecular weight condensed aro-matic, or naphthenic compounds, or both.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and the API Committee on Petroleum Measure-ment, and is the direct responsibility of Subcomm

12、ittee D02.02.0B /COMQ, the jointASTM-API Committee on Sampling, Sediment, Water.Current edition approved May 1, 2010. Published May 2010. Originallyapproved in 1921. Last previous edition approved in 2005 as D9505. DOI:10.1520/D0095-05R10.2For referenced ASTM standards, visit the ASTM website, www.a

13、stm.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.3Published as Manual of Petroleum Measurement Standards. Available fromAmerican Petroleum Institute (API), 1220 L. St., NW

14、, Washington, DC 20005-4070,http:/www.api.org1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.4. Summary of Test Method4.1 The material to be tested is heated under reflux with awater-immiscible solvent, which co-distills with the wat

15、er inthe sample. Condensed solvent and water are continuouslyseparated in a trap, the water settling in the graduated sectionof the trap and the solvent returning to the still.5. Significance and Use5.1 Aknowledge of the water content of petroleum productsis important in the refining, purchase, sale

16、, and transfer ofproducts.5.2 The amount of water as determined by this test method(to the nearest 0.05 or 0.1 volume %, depending on the trapsize used) may be used to correct the volume involved in thecustody transfer of petroleum products and bituminous mate-rials.5.3 The allowable amount of water

17、 may be specified incontracts.6. Solvent-Carrier Liquid6.1 Asolvent-carrier liquid appropriate to the material beingtested (see Table 1) shall be used.6.1.1 Aromatic SolventThe following aromatic solventsare acceptable:6.1.1.1 Industrial Grade Xylene(WarningFlammable.Vapor harmful.)6.1.1.2 Ablend of

18、 20 volume % industrial grade toluene and80 volume % industrial grade xylene. (WarningFlammable.Vapor harmful.)6.1.1.3 Petroleum Naphtha or Coal Tar Naphtha, free ofwater, yielding not more than 5% distillates at 125C (257F)and not less than 20% at 160C (320F) and with a relativedensity (specific gr

19、avity) not lower than 0.8545 at 15.56/15.56C (60/60F). (WarningExtremely flammable. Harm-ful if inhaled. Vapors may cause fire.)6.1.2 Petroleum Distillate SolventA petroleum distillatesolvent, 5% boiling between 90 and 100C (194 and 212F)and 90% distilling below 210C (410F), shall be used. Percentma

20、y be determined by mass or by volume. (WarningFlammable. Vapor harmful.)6.1.3 Volatile Spirits SolventThe following volatile spiritssolvents are acceptable:6.1.3.1 Petroleum Spirit, with a boiling range from 100 to120C (212 to 248F). (WarningFlammable. Vapor harm-ful.)6.1.3.2 Iso-octane, of 95% puri

21、ty or better. (WarningExtremely flammable. Harmful if inhaled. Vapors may causefire.)6.2 Solvent BlankThe water content of the solvent shallbe determined by distilling an equivalent amount of the samesolvent used for the test sample in the distillation apparatus andtesting as outlined in Section 10.

22、 The blank shall be determinedto the nearest scale division and used to correct the volume ofwater in the trap in Section 11.7. Apparatus7.1 GeneralThe apparatus comprises a glass or metalstill, a heater, a reflux condenser, and a graduated glass trap.The still, trap, and condenser may be connected

23、by any suitablemethod that produces a leakproof joint. Preferred connectionsare ground joints for glass and O-rings for metal to glass.Typical assemblies are illustrated in Fig. 1, Fig. 2, and Fig. 3.The stills and traps should be chosen to cover the range ofmaterials and water contents expected. On

24、 assembly, care shallbe taken to prevent the joints from freezing or sticking.Alwaysapply a very thin film of stopcock grease to prevent theglassware joints from seizing.7.2 StillA glass or metal vessel with a short neck andsuitable joint for accommodating the reflux tube of the trapshall be used. V

25、essels of 500, 1000, and 2000-mL nominalcapacity have proved satisfactory.7.3 HeaterA suitable gas burner or electric heater may beused with the glass still. A gas ring burner with ports on theinside circumference shall be used with the metal still. The gasring burner shall be of such dimensions tha

26、t it may be movedup and down the vessel when testing materials that are likely tofoam or solidify in the still.7.4 GlasswareDimensions and descriptions of typicalglassware for use in this test method are provided in Specifi-cation E123.NOTE 3Instead of standardizing on a particular apparatus specifi

27、ca-tion with respect to dimensions and style, a given apparatus will bedeemed satisfactory when accurate results are obtained by the standardaddition technique described in Section 9.TABLE 1 Type of Solvent-Carrier Liquid Versus Material to BeTestedType of Solvent-Carrier Liquid Material to be Teste

28、dAromatic asphalt, tar, coal tar, water gas tar, roadtar, cut-back bitumin, liquid asphalt, taracidPetroleum distillate road oil, fuel oil, lubricating oil, petroleumsulfonatesVolatile spirits lubricating greaseFIG. 1 Typical Assembly with Glass StillD95 05 (2010)28. Sampling8.1 Sampling is defined

29、as all steps required to obtain analiquot of the contents of any pipe, tank, or other system and toplace the sample into the laboratory test container. Onlyrepresentative samples obtained as specified in PracticesD4057 (API MPMS Chapter 8.1) and D4177 (API MPMSChapter 8.2) shall be used for this tes

30、t method.8.2 The size of the test portion should be based on theexpected water content of the sample, such that the water yielddoes not exceed the capacity of the trap (unless a trap with astopcock is used permitting excess water to be withdrawn intoa graduated cylinder).8.3 Practice D5854 (API MPMS

31、 Chapter 8.3) containsinformation on sampling and homogenization efficiency ofunknown mixers. This test method should not be followedwithout strict adherence to Practice D5854 (API MPMSChapter 8.3).9. Verification9.1 The accuracy of the graduation marks on the trap shallbe certified or verified, usi

32、ng only national or internationalstandards, such as National Institute of Standards and Technol-ogy (NIST)4traceable equipment. Verification shall be with atraceable 5 mL Micro Burette or Micro Pipette, readable to thenearest 0.01 mL.9.1.1 In styles A, B, C, and D, as specified in Table 2(Table 1 in

33、 Specification E123), each subdivision (that is, 0.1mL through 1.0 mL) in the conical portion of the tube shall beverified. Thereafter, each major subdivision (that is, 2.0 mL,3.0 mL, 4.0 mL, and up to the total volume of the trap) shall beverified.9.1.2 In styles E and F, as specified in Table 2, e

34、ach majorsubdivision (0.1 mL, 1.0 mL, 2.0 mL, 4.0 mL, and 5.0 mL inthe case of Style E; 0.05 mL, 0.5 mL, 1.0 mL, 1.5 mL, and 2.0mL in the case of Style F) shall be verified.9.2 The entire glassware assembly shall be verified prior tofirst use and at a regular frequency thereafter as follows.9.2.1 Pu

35、t 400 mL of dry (0.02 % water maximum) xylene orthe solvent to be utilized in the analysis of unknown samplesinto the apparatus and test in accordance with Section 10.When complete, discard the contents of the trap and add thevolume of water as specified as first test in Table 3 directly tothe disti

36、llation flask and test in accordance with Section 10.9.2.2 Repeat the test in 9.2.1, and add the volume specifiedas second test in Table 3 directly to the flask. The assembly ofthe apparatus is satisfactory only if the trap readings are withinthe tolerances specified in Table 3.9.3 A reading outside

37、 the permissible limits suggests amalfunction resulting from vapor leaks, too rapid boiling,inaccuracies in calibration of the trap, or ingress of extraneousmoisture. Eliminate these factors before repeating the verifica-tion.10. ProcedureNOTE 4The precision of this test method will be affected by w

38、aterdroplets adhering to surfaces in the apparatus and therefore not settlinginto the water trap to be measured. To minimize the problem, all apparatusmust be cleaned chemically at least daily to remove surface films anddebris, which hinder free drainage of water in the test apparatus. Morefrequent

39、cleaning is recommended if the nature of samples being runcauses persistent contamination.10.1 Measure a suitable amount of sample to an accuracy of6 1% and transfer it to the still.10.2 Measure ordinary liquid samples in a graduated cylin-der of an appropriate size. Rinse the material adhering to t

40、hecylinder with one 50-mL and two 25-mL portions of thesolvent-carrier liquid (see Section 6 and Table 1). Drain thecylinder thoroughly after the sample transfer and each rinsing.10.3 Weigh solid or viscous materials directly into the stilland add 100 mL of the selected solvent-carrier liquid. In ca

41、sesof material with a low-water content when large samples mustbe used, a solvent-carrier liquid volume in excess of 100 mLmay be necessary.10.4 Glass beads or other boiling aids may be added, ifnecessary, to reduce bumping.10.5 Assemble the components of the apparatus, as illus-trated in Fig. 1, Fi

42、g. 2, and Fig. 3, choosing the trap inaccordance with the expected water content of the sample andmaking all connections vapor and liquid tight. If a metal stillwith a removable cover is used, insert a gasket of heavy paper,moistened with solvent, between the still body and the cover.The condenser t

43、ube and trap must be chemically clean toensure free drainage of water into the bottom of the trap. Inserta loose cotton plug in the top of the condenser to preventcondensation of atmospheric moisture inside it. Circulate coldwater through the jacket of the condenser.10.6 Apply heat to the still, adj

44、usting the rate of boiling sothat condensed distillate discharges from the condenser at therate of two to five drops per second. If the metal still is used,start heating with the ring burner about 76 mm (3 in.) above thebottom of the still and gradually lower the burner as thedistillation proceeds.

45、Continue distillation until no water is4National Institute of Standards and Technology (NIST), 100 Bureau Dr., Stop1070, Gaithersburg, MD 20899-1070, http:/www.nist.gov.FIG. 2 Two-millilitre Receiver Showing Alternative Connections toGlass StillD95 05 (2010)3NOTETrap shall be 15 to 16 mm in inside d

46、iameter.FIG. 3 Typical Assemblies with Metal StillTABLE 2 Specifications and Sizes of TrapsDescriptionStyleTop ofGraduatedTubeBottom ofGraduatedTubeBottom ofVapor TubeSize of TrapmLRangemLSmallestScaleDivision,mLScale ErrorMaximum,mLA ST Joint Conical ST Joint 10 0 to 1.0 0.1 0.051.0 to 10.0 0.2 0.1

47、B ST Joint Conical ST Joint 25 0 to 1.0 0.1 0.05C ST Joint Conical Plain 25 1.0 to 25 0.2 0.1D ST Joint Conical Plain 25 1.0 to 25 0.2 0.1E ST Joint Round ST Joint 5 0 to 5.0 0.1 0.055 0 to 5.0 0.05 0.02510 0 to 10.0 0.1 0.1F ST Joint Round ST Joint 2 0 to 2.0 0.05 0.025D95 05 (2010)4visible in any

48、part of the apparatus except in the trap and thevolume of water in the trap remains constant for 5 min. If thereis a persistent ring of water in the condenser tube, carefullyincrease the rate of distillation or cut off the condenser waterfor a few minutes.10.7 When the evolution of water is complete

49、, allow the trapand contents to cool to room temperature. Dislodge any dropsof water adhering to the sides of the trap with a glass orpolytetrafluoroethylene (PTFE) rod or other suitable means andtransfer them to the water layer. Read the volume of the waterin the trap to the nearest scale division.10.8 A solvent blank shall be established, as outlined in 6.2.11. Calculation11.1 Calculate the water in the sample, as weight or volumepercent, in accordance with the basis on which the sample wastaken, as follows:11.1.1 Water, % (V/V) =Volume in wa