1、Manual of PetroleumMeasurement StandardsChapter 10.2Standard Test Method for Water in Crude Oil by DistillationTHIRD EDITION, AUGUST 2013Special NotesAPI publications necessarily address problems of a general nature. With respect to particular circumstances, local,state, and federal laws and regulat
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14、g anyone against liability for infringement of letters patent.Shall: As used in a standard, “shall” denotes a minimum requirement in order to conform to the specification.Should: As used in a standard, “should” denotes a recommendation or that which is advised but not required in orderto conform to
15、the specification.This document was produced under API standardization procedures that ensure appropriate notification andparticipation in the developmental process and is designated as an API standard. Questions concerning theinterpretation of the content of this publication or comments and questio
16、ns concerning the procedures under whichthis publication was developed should be directed in writing to the Director of Standards, American PetroleumInstitute, 1220 L Street, NW, Washington, DC 20005. Requests for permission to reproduce or translate all or any partof the material published herein s
17、hould also be addressed to the director.Generally, API standards are reviewed and revised, reaffirmed, or withdrawn at least every five years. A one-timeextension of up to two years may be added to this review cycle. Status of the publication can be ascertained from theAPI Standards Department, tele
18、phone (202) 682-8000. A catalog of API publications and materials is publishedannually by API, 1220 L Street, NW, Washington, DC 20005.Suggested revisions are invited and should be submitted to the Standards Department, API, 1220 L Street, NW,Washington, DC 20005, standardsapi.org.iiiContentsPage1 S
19、cope . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12 Referenced Documents . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
20、 . . . . . . . . . . . . . 13 Summary of Test Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14 Significance and Use . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
21、 . . . . . . . . . . . . . . . . . . . . . . . 15 Apparatus . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26 Solvent . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
22、 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27 Sampling, Test Samples, and Test Units. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28 Calibration . . . . . . . . . . . . . . . . . . . . . . .
23、 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39 Procedure. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 310 Calculation . .
24、 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 311 Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
25、. . . . . . . . . . . . . . 412 Precision and Bias . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 413 Keywords . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
26、. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4Annex A1 (Mandatory Information) Warning Statement. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5Appendix X1 (Nonmandatory Information) Precision and Bias of Test Methods for Determining
27、Water in Crude Oils . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5Summary of Changes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
28、. . . . . . . . . . . . . 11Figures1 Distilation Apparatus. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22 Pick, Scraper, and Jet Spray Tube for Distillation Apparatus . . . . . . . . . . . . . . . . . . . .
29、. . . . . . . . . . . . . . . 43 Basic Sediment and Water Precision . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5X1.1 Basic Sediment Water Precision for ASTM Test Method D95 (API MPMS Chapter 10.5) Distillation Method (Based on Seven
30、Laboratories) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9X1.2 Basic Sediment and Water Precision for ASTM Test Method D1796 (API MPMS Chapter 10.6) Centrifuge Method (Based on Five Laboratories) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
31、 . . . . . . . . . . . . . 10X1.3 Basic Sediment and Water Precision for ASTM Test Method D1796 (API MPMS Chapter 10.6) Centrifuge Method (Based on Six Laboratories) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10TablesX1.1 Base CaseWater Content of Crude
32、s . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6X1.2 Water Content of Crude Oil Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6X1.3 Determination of Water in Crude O
33、ils, % H2O . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7X1.4 Corrections to be Applied to Measured Values to Obtain “True” Water Content . . . . . . . . . . . . . . . . . . . 7X1.5 Bias of Test Methods Estimated from Spiked Samples . . . . . . . .
34、. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7X1.6 Round-Robin Results of Water in Crude Oils by ASTM D95 (API MPMS Chapter 10.5) and ASTM D1796 (API MPMS Chapter 10.6). . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8X1.7 ASTM Pr
35、ecision Intervals: ASTM D95 (API MPMS Chapter 10.5) (7 Laboratories) . . . . . . . . . . . . . . . . . . 9vDesignation: D4006 11 (Reapproved 2012)1Manual of Petroleum Measurement Standards (MPMS), Chapter 10.2Standard Test Method forWater in Crude Oil by Distillation1This standard is issued under th
36、e fixed designation D4006; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the la
37、st revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1NOTEAPI information was editorially corrected in June 2013.1. Scope*1.1 This test method covers the determination of water incrude oil by distillation.1.2 The values stated in SI units are to
38、be regarded asstandard. No other units of measurement are included in thisstandard.1.3 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
39、determine the applica-bility of regulatory limitations prior to use. For specificwarning statements, see 6.1 and A1.1.2. Referenced Documents2.1 ASTM Standards:2D95 Test Method for Water in Petroleum Products andBituminous Materials by Distillation (API MPMS Chapter10.5)D473 Test Method for Sediment
40、 in Crude Oils and Fuel Oilsby the Extraction Method (API MPMS Chapter 10.1)D665 Test Method for Rust-Preventing Characteristics ofInhibited Mineral Oil in the Presence of WaterD1796 Test Method for Water and Sediment in Fuel Oils bythe Centrifuge Method (Laboratory Procedure) (APIMPMS Chapter 10.6)
41、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)D4928 Test Method for Water in Crude Oils by CoulometricKarl Fischer Titration (API MPMS Chapter 10.9)E123 Specif
42、ication forApparatus for Determination ofWaterby Distillation2.2 API Standards:MPMS Chapter 8.1 Manual Sampling of Petroleum andPetroleum Products (ASTM Practice D4057)MPMS Chapter 8.2 Automatic Sampling of Petroleum andPetroleum Products (ASTM Practice D4177)MPMS Chapter 10.1 Test Method for Sedime
43、nt in CrudeOils and Fuel Oils by the Extraction Method (ASTM TestMethod D473)MPMS Chapter 10.4 Determination of Water and/or Sedi-ment in Crude Oil by the Centrifuge Method (FieldProcedure)MPMS Chapter 10.5 Test Method for Water in PetroleumProducts and Bituminous Materials by Distillation(ASTM Test
44、 Method D95)MPMS Chapter 10.6 Test Method for Water and Sediment inFuel Oils by the Centrifuge Method (Laboratory Proce-dure) (ASTM Test Method D1796)MPMS Chapter 10.9 Test Method for Water in Crude Oils byCoulometric Karl Fischer Titration (ASTM Test MethodD4928)3. Summary of Test Method3.1 The sam
45、ple is heated under reflux conditions with awater immiscible solvent which co-distills with the water in thesample. Condensed solvent and water are continuously sepa-rated in a trapthe water settles in the graduated section of thetrap, and the solvent returns to the distillation flask.4. Significanc
46、e and Use4.1 A knowledge of the water content of crude oil isimportant in the refining, purchase, sale, or transfer of crudeoils.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 res
47、ponsibility of Subcommittee D02.02 /COMQ on Hydro-carbon Measurement for Custody Transfer (Joint ASTM-API).Current edition approved Nov. 1, 2012. Published December 2012. Originallyapproved in 1981. Last previous edition approved in 2011 as D400611. DOI:10.1520/D4006-11R12.2For referenced ASTM stand
48、ards, visit the 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.*A Summary of Changes section appears at the end of this standardCopyright ASTM Interna
49、tional, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States14.2 This test method may not be suitable for crude oils thatcontain alcohols that are soluble in water. In cases where theimpact on the results may be significant, the user is advised toconsider using another test method, such as Test MethodD4928 (API MPMS Chapter 10.9).5. Apparatus5.1 The preferred apparatus, shown in Fig. 1, consists of aglass distillation flask, a condenser, a graduated glass trap,3anda heater. Other types of distillation apparatus are specified inSpecification E123
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