1、Designation: D 95 05e1Designation: Manual of Petroleum Measurement Standards (MPMS), Chapter 10.5Designation: 74/82 (88)An American National StandardAmerican Association StateHighway Transportation StandardAASHTO No. T55Standard Test Method forWater in Petroleum Products and Bituminous Materials byD
2、istillation1This standard is issued under the fixed designation D 95; 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 (e
3、) indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.e1NOTETable 4 formatting and the last sentence of 7.1 were updated editorially in August 2005.1. Scope*1.1 This test method covers the determination
4、of water inthe range from 0 to 25 % volume in petroleum products, tars,and other bituminous materials by the distillation method.NOTE 1Volatile 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 T
5、able 1. For bituminousemulsions refer to Test Method D 244. For crude oils, refer toTest Method D 4006 (API MPMS Chapter 10.2).NOTE 2With some types of oil, satisfactory results may be obtainedfrom Test Method D 1796 (API MPMS Chapter 10.6).1.3 The values stated in SI units are to be regarded as the
6、standard. The values in parentheses are for information only.1.4 This standard does not purport to address 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-
7、bility of regulatory limitations prior to use. For specific hazardstatements, see Section 6.2. Referenced Documents2.1 ASTM Standards:2D 244 Test Methods for Emulsified AsphaltsD 1796 Test Method for Water and Sediment in Fuel Oils bythe Centrifuge Method (Laboratory Procedure) (APIMPMS Chapter 10.6
8、)D 4006 Test Method for Water in Crude Oil by Distillation(API MPMS Chapter 10.2)D 4057 Practice for Manual Sampling of Petroleum andPetroleum Products (API MPMS Chapter 8.1)D 4177 Practice for Automatic Sampling of Petroleum andPetroleum Products (API MPMS Chapter 8.2)D 5854 Practice for Mixing and
9、 Handling of LiquidSamples of Petroleum and Petroleum Products (APIMPMS Chapter 8.3)E 123 Specification for Apparatus for Determination ofWater by Distillation2.2 API Standards:3MPMS Chapter 8.1 Manual Sampling of Petroleum andPetroleum Products (ASTM Practice D 4057)MPMS Chapter 8.2 Automatic Sampl
10、ing of Petroleum andPetroleum Products (ASTM Practice D 4177)MPMS Chapter 8.3 Mixing and Handling of Liquid Samplesof Petroleum and Petroleum Products (ASTM PracticeD 5854)MPMS Chapter 10.2 Determination of Water in Crude Oilby the Distillation Method (ASTM Test Method D 4006)MPMS Chapter 10.6 Test
11、Method for Water and Sediment inFuel Oils by the Centrifuge Method (Laboratory Proce-dure) (ASTM Test Method D 1796)3. Terminology3.1 Definitions:1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and the API Committee on Petroleum Measure-ment, and
12、 is the direct responsibility of Subcommittee D02.02 /COMQ, the jointASTM-API Committee on Static Petroleum Measurement.Current edition approved June 1, 2005. Published July 2005. Originally approvedin 1921. Last previous edition approved in 1999 as D 9599e1.2For referenced ASTM standards, visit the
13、 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.3Published as Manual of Petroleum Measurement Standards. Available from theAmerican Petroleum Institut
14、e (API), 1220 L St., NW, Washington, DC 20005.1*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.3.1.1 bituminous material, nin petroleum technology,ablack or dark-colore
15、d very viscous liquid or semi-solid com-posed principally of high molecular weight condensed aro-matic, or naphthenic compounds, or both.4. Summary of Test Method4.1 The material to be tested is heated under reflux with awater-immiscible solvent, which co-distills with the water inthe sample. Conden
16、sed 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, and transfer ofproduc
17、ts.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 may be specified incon
18、tracts.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 20 volume % industrial
19、 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 gravity) not lower than 0
20、.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. Percentmay be determined by mass
21、 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% purity or better. (WarningE
22、xtremely 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. The blank shall be det
23、erminedto 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 by any suitablemethod t
24、hat 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 assembly, care shallbe
25、 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. Vessels of 500, 1000, an
26、d 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 that it may be movedup and
27、 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 E 123.NOTE 3Instead of standardizing on a particular apparatus specifica-tion with respect t
28、o dimensions and style, a given apparatus will bedeemed satisfactory when accurate results are obtained by the standardTABLE 1 Type of Solvent-Carrier Liquid Versus Material to BeTestedType of Solvent-Carrier Liquid Material to be TestedAromatic asphalt, tar, coal tar, water gas tar, roadtar, cut-ba
29、ck bitumin, liquid asphalt, taracidPetroleum distillate road oil, fuel oil, lubricating oil, petroleumsulfonatesVolatile spirits lubricating greaseFIG. 1 Typical Assembly with Glass StillD9505e12addition technique described in Section 9.8. Sampling8.1 Sampling is defined as all steps required to obt
30、ain 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 PracticesD 4057 (API MPMS Chapter 8.1) and D 4177 (API MPMSChapter 8.2) shall be used for this test method.8.2 The size of t
31、he 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 D 5854 (API MPMS Chapter 8.3) containsinf
32、ormation on sampling and homogenization efficiency ofunknown mixers. This test method should not be followedwithout strict adherence to Practice D 5854 (API MPMSChapter 8.3).9. Verification9.1 The accuracy of the graduation marks on the trap shallbe certified or verified, using only national or inte
33、rnationalstandards, 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 Specification E 123), e
34、ach 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, each majorsubdivision (0
35、.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 Put 400 mL of dry (0.02 %
36、 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 distillation flask and test
37、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 the permissible limits
38、 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 waterdroplets adhering t
39、o 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 cleaning is recommended
40、 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 thecylinder with one 50-
41、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 casesof material with a l
42、ow-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, Fig. 2, and Fig. 3, choos
43、ing 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 tube and trap must be ch
44、emically 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, adjusting the rate of boil
45、ing 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 the4National Institute of Standards and Technology, U.S. Department of Com-merce, Gaithersburg, MD 20899.F
46、IG. 2 Two-millilitre Receiver Showing Alternative Connections toGlass StillD9505e13NOTETrap shall be 15 to 16 mm in inside diameter.FIG. 3 Typical Assemblies with Metal StillTABLE 2 Specifications and Sizes of TrapsDescriptionStyleTop ofGraduatedTubeBottom ofGraduatedTubeBottom ofVapor TubeSize of T
47、rapmLRangemLSmallestScaleDivision,mLScale ErrorMaximum,mLA ST Joint Conical ST Joint 10 0 to 1.0 0.1 0.051.0 to 10.0 0.2 0.1B 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
48、.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 0.025D9505e14bottom of the still and gradually lower the burner as thedistillation proceeds. Continue distillation until no water isvisible in any part of the apparatus except in the trap and thevolume of water
49、 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, 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 blan
