1、Designation: D95 13 (Reapproved 2018)Manual of Petroleum Measurement Standards (MPMS), Chapter 10.5Standard Test Method forWater in Petroleum Products and Bituminous Materials byDistillation1This standard is issued under the fixed designation D95; the number immediately following the designation ind
2、icates 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 last revision or reapproval.This standard has been approved for use by agencies o
3、f the U.S. Department of Defense.1. Scope1.1 This test method covers the determination of water inthe range from 0 % to 25 % by 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
4、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 some types of oil, satisfactory results may be obtainedfrom Test Method
5、D1796 (API MPMS Chapter 10.6).1.3 The values stated in SI units are to be regarded asstandard. The values given in parentheses after SI units areprovided for information only and are not considered standard.1.4 This standard does not purport to address all of thesafety concerns, if any, associated w
6、ith its use. It is theresponsibility of the user of this standard to establish appro-priate safety, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to use.For specific hazard statements, see Section 6.1.5 This international standard was developed
7、in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents
8、2.1 ASTM Standards:2D235 Specification for Mineral Spirits (Petroleum Spirits)(Hydrocarbon Dry Cleaning Solvent)D244 Test Methods and Practices for Emulsified AsphaltsD1796 Test Method for Water and Sediment in Fuel Oils bythe Centrifuge Method (Laboratory Procedure) (APIMPMS Chapter 10.6)D4006 Test
9、 Method for Water in Crude Oil by Distillation(API MPMSChapter 10.2)D4057 Practice for Manual Sampling of Petroleum andPetroleum Products (API MPMS Chapter 8.1)D4177 Practice for Automatic Sampling of Petroleum andPetroleum Products (API MPMS Chapter 8.2)D5854 Practice for Mixing and Handling of Liq
10、uid Samplesof Petroleum and Petroleum Products (API MPMS Chap-ter 8.3)E123 Specification forApparatus for Determination of Waterby Distillation2.2 API Standards:3MPMS Chapter 8.1 Manual Sampling of Petroleum andPetroleum Products (ASTM Practice D4057)MPMS Chapter 8.2 Automatic Sampling of Petroleum
11、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 Oil bythe Distillation Method (ASTM Test Method D4006)MPMS Chapter 10.6 Test Method for Water and
12、 Sediment inFuel Oils by the Centrifuge Method (Laboratory Proce-dure) (ASTM Test Method D1796)1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and the API Committee onPetroleum Measurement, and is the direct responsibility of Subco
13、mmittee D02.02/COMQ the joint ASTM-API Committee on Hydrocarbon Measurement forCustody Transfer (Joint ASTM-API). This practice has been approved by thesponsoring committees and accepted by the Cooperating Societies in accordancewith established procedures.Current edition approved Oct. 1, 2018. Publ
14、ished November 2018. Originallyapproved in 1921. Last previous edition approved in 2013 as D95 131. DOI:10.1520/D0095-13R18.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, r
15、efer 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, Washington, DC 20005-4070,http:/www.api.org Jointly copyrighted by ASTM International, 100 Barr Harbor Drive, PO
16、Box C700, West Conshohocken, PA 19428-2959, USA and the American Petroleum Institute (API), 1220 L Street NW, Washington DC 20005, USAThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for th
17、eDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.13. Terminology3.1 Definitions:3.1.1 bituminous material, nin petroleum technology,ablack or dark-colored very viscous liquid or semi-solid com-posed
18、 principally of high molecular weight condensedaromatic, 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. Condensed solvent and water are continuouslyseparated
19、 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 ofproducts.5.2 The amount of water as determined by thi
20、s test method(to the nearest 0.05 % or 0.1 % by volume, depending on thetrap size used) may be used to correct the volume involved inthe custody transfer of petroleum products and bituminousmaterials.5.3 The allowable amount of water may be specified incontracts.6. Solvent-Carrier Liquid6.1 A water-
21、immiscible solvent-carrier liquid that is mis-cible in the material being tested (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 A blend of 20 % by volume industrial grade toluenea
22、nd 80 % by 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 125 C (257 F)and not less than 20 % at 160 C (320 F) and with a relativedensity (specific gravity) not lower than 0.8545
23、 at15.56 C 15.56 C (60 F 60 F). (WarningExtremelyflammable. Harmful if inhaled. Vapors may cause fire.)6.1.2 Petroleum Distillate SolventA petroleum distillatesolvent containing at least 2 % (V/V) aromatics and with aninitial boiling point (IBP) greater than 80 C (176 F); and afinal boiling point (F
24、BP) below 250 C (482 F) shall be used.NOTE 3Examples of suitable solvents include Types I and IV andClasses A and B of Specification D235.NOTE 4It is recommended to use a wide boiling range solvent with10 % boiling below 100 C to help to ensure an even distillation rate.6.1.3 Volatile Spirits Solven
25、tThe following volatile spiritssolvents are acceptable:6.1.3.1 Petroleum Spirit, with a boiling range from 100 Cto 120 C (212 F to 248 F). (WarningFlammable. Vaporharmful.)6.1.3.2 Iso-octane, of 95 % purity or better. (WarningExtremely flammable. Harmful if inhaled. Vapors may causefire.)6.2 Solvent
26、 BlankThe water content of the solvent shall bedetermined 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 determinedto the nearest scale division and used to correct the volume ofwat
27、er in the trap in Section 11.7. Apparatus7.1 GeneralThe apparatus comprises a glass or metal still,a heater, a reflux condenser, and a graduated glass trap. Thestill, trap, and condenser may be connected by any suitablemethod that produces a leakproof joint. Preferred connectionsare ground joints fo
28、r 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 taken to prevent the joints from freezing or sticking.Alwaysapply a very
29、 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 mL, 1000 mL, and 2000 mLnominal capacity have proved satisfactory.7.3 HeaterA suit
30、able 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 movedTABLE 1 Type of Solvent-Carrier Liquid to Use Versus Material toBe Tested
31、Type of Solvent-Carrier Liquid Material to be TestedAromatic asphalt, bitumen, tar, and related productsPetroleum distillate fuel oil, lubricating oil, lubricating oil additivesVolatile spirits greasesFIG. 1 Typical Assembly with Glass StillD95 13 (2018)2up and down the vessel when testing materials
32、 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 5Instead of standardizing on a particular apparatus specifica-tion with respect to dimensions and style, a given apparatu
33、s will bedeemed satisfactory when accurate results are obtained by the standardaddition technique described in Section 9.8. Sampling8.1 Sampling is defined 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 con
34、tainer. Onlyrepresentative samples obtained as specified in PracticesD4057 (API MPMS Chapter 8.1) and D4177 (API MPMSChapter 8.2) shall be used for this test 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 t
35、he 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 Chapter 8.3) containsinformation on sampling and homogenization efficiency ofunknown mixers. This test method should not be followedwithout str
36、ict adherence to Practice D5854 (API MPMSChapter 8.3).9. Verification9.1 The accuracy of the graduation marks on the trap shallbe certified or verified, using only national or internationalstandards, such as National Institute of Standards and Technol-ogy (NIST)4traceable equipment. Verification sha
37、ll 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 E123), each subdivision (that is,0.1 mL through 1.0 mL) in the conical portion of the tube shallbe verified. Thereafter, each maj
38、or 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 (0.1 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, and2.0 mL in the case o
39、f 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 % water maximum) xylene orthe solvent to be utilized in the analysis of unknown samplesinto the apparatus and test in acco
40、rdance 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 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 direc
41、tly 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 suggests amalfunction resulting from vapor leaks, too rapid boiling,inaccuracies in calibration of the trap, or ingress
42、of extraneousmoisture. Eliminate these factors before repeating the verifica-tion.10. ProcedureNOTE 6The precision of this test method will be affected by waterdroplets adhering to surfaces in the apparatus and therefore not settlinginto the water trap to be measured. To minimize the problem, all ap
43、paratusmust 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 if the nature of samples being runcauses persistent contamination.10.1 Measure a suitable amount of sample to an accurac
44、y of61 % 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 mL and two 25 mL portions of thesolvent-carrier liquid (see Section 6 and Table 1). Drain thecylinder thoroughly after th
45、e 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 low-water content when large samples mustbe used, a solvent-carrier liquid volume in excess of 100 mLmay be necessary.10.4
46、 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, choosing the trap in4National Institute of Standards and Technology (NIST), 100 Bureau Dr., Stop1070, Gaithersburg, MD 20899-1
47、070, http:/www.nist.gov.FIG. 2 Two-millilitre Receiver Showing Alternative Connections toGlass StillD95 13 (2018)3NOTE 1Trap shall be 15 to 16 mm in inside diameter.FIG. 3 Typical Assemblies with Metal StillD95 13 (2018)4accordance with the expected water content of the sample andmaking all connecti
48、ons 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 chemically clean toensure free drainage of water into the bottom of the trap. Inserta loose cott
49、on 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 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. Continue distillation until no water isvisible in any part
