1、Manual of PetroleumMeasurement StandardsChapter 10Sediment and WaterSection 1Standard Test Method for Sediment in Crude Oils and Fuel Oils by the Extration MethodTHIRD EDITION, NOVEMBER 2007REAFFIRMED, OCTOBER 2012Manual of PetroleumMeasurement StandardsChapter 10Sediment and WaterSection 1Standard
2、Test Method for Sediment in Crude Oils and Fuel Oils by the Extration MethodMeasurement CoordinationTHIRD EDITION, NOVEMBER 2007REAFFIRMED, OCTOBER 2012Special NotesAPI publications necessarily address problems of a general nature. With respect to particular circumstances, local,state, and federal l
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6、pressly disclaims any liability or responsibility for loss ordamage resulting from its use or for the violation of any authorities having jurisdiction with which this publication mayconflict.API publications are published to facilitate the broad availability of proven, sound engineering and operatin
7、gpractices. These publications are not intended to obviate the need for applying sound engineering judgmentregarding when and where these publications should be utilized. The formulation and publication of API publicationsis not intended in any way to inhibit anyone from using any other practices.An
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10、20 L Street, N.W., Washington, D.C. 20005.Copyright 2007 American Petroleum InstituteForewordNothing contained in any API publication is to be construed as granting any right, by implication or otherwise, for themanufacture, sale, or use of any method, apparatus, or product covered by letters patent
11、. Neither should anythingcontained in the publication be construed as insuring anyone against liability for infringement of letters patent.This document was produced under API standardization procedures that ensure appropriate notification andparticipation in the developmental process and is designa
12、ted as an API standard. Questions concerning theinterpretation of the content of this publication or comments and questions concerning the procedures under whichthis publication was developed should be directed in writing to the Director of Standards, American PetroleumInstitute, 1220 L Street, N.W.
13、, Washington, D.C. 20005. Requests for permission to reproduce or translate all or anypart of the material published herein should also be addressed to the director.Generally, API standards are reviewed and revised, reaffirmed, or withdrawn at least every five years.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
14、 years may be added to this review cycle. Status of the publication can be ascertained from theAPI Standards Department, telephone (202) 682-8000. A catalog of API publications and materials is publishedannually and updated quarterly by API, 1220 L Street, N.W., Washington, D.C. 20005.Suggested revi
15、sions are invited and should be submitted to the Standards Department, API, 1220 L Street, NW,Washington, D.C. 20005, standardsapi.org.ContentsPage1 Scope . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
16、 . . . . . . . . . 12 Referenced Documents. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13 Summary of Test Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
17、. . . . . . . . . . . . . . . . . . 14 Significance and Use. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15 Apparatus . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
18、. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16 Solvent . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37 Sampling. . . . . . . . . . . . . . . . . . . . . . .
19、. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 48 Procedure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49 Calculation
20、. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 410 Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
21、 . . . . . . . . . . . . . . . 411 Precision and Bias. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 512 Keywords . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
22、. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5Annex A1 Warning Statement. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5Summary of Changes. . . . . . . . . . . . . . . . . . . . . . . . . .
23、. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6Figures1 Extraction Apparatus for Determination of Sediment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22 Basket Thimble Support . . . . . . . . . . . . . . . .
24、 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3Table1 Typical Characteristics for ACS Reagent Grade Toluene . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4Designation: D 473 07Designation: Manual of Petroleu
25、m Measurement Standards (MPMS), Chapter 10.1Designation: 53/82An American National StandardStandard Test Method forSediment in Crude Oils and Fuel Oils by the ExtractionMethod1This standard is issued under the fixed designation D 473; the number immediately following the designation indicates the ye
26、ar 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 (e) indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Depart
27、ment of Defense.1. Scope*1.1 This test method covers the determination of sedimentin crude oils and fuel oils by extraction with toluene. Theprecision applies to a range of sediment levels from 0.01 to0.40 % mass, although higher levels may be determined.NOTE 1Precision on recycled oils and crank ca
28、se oils is unknown andadditional testing is required to determine that precision.1.2 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.3 This standard does not purport to address all of thesafety concerns, if any, associated wi
29、th 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 specificwarning statements, see 5.1.1.6 and 6.1.2. Referenced Documents2.1 ASTM Standards:2D 4057 Practi
30、ce for Manual Sampling of Petroleum andPetroleum ProductsD 4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD 5854 Practice for Mixing and Handling of LiquidSamples of Petroleum and Petroleum ProductsE29 Practice for Using Significant Digits in Test Data toDetermine Conformance
31、 with Specifications2.2 API Standards:3Chapter 8.1 Manual Sampling of Petroleum and PetroleumProducts (ASTM Practice D 4057)Chapter 8.2 Automatic Sampling of Petroleum and Petro-leum Products (ASTM Practice D 4177)Chapter 8.3 Mixing and Handling of Liquid Samples ofPetroleum and Petroleum Products (
32、ASTM PracticeD 5854)2.3 ISO Standard:45272 Toluene for industrial useSpecifications3. Summary of Test Method3.1 Extract test portion of a representative oil sample,contained in a refractory thimble, with hot toluene until theresidue reaches constant mass. The mass of residue, calculatedas a percenta
33、ge, is reported as sediment by extraction.4. Significance and Use4.1 A knowledge of the sediment content of crude oils andfuel oils is important both to the operation of refining and thebuying or selling of these commodities.5. Apparatus5.1 Usual laboratory apparatus and glassware, together withthe
34、following are required for this test method.5.1.1 Extraction ApparatusUse the apparatus illustratedin Figs. 1 and 2 and consisting of the elements described in5.1.1.1-5.1.1.3.5.1.1.1 Extraction FlaskUse a wide-neck (Erlenmeyer)flask of 1-L capacity, with a minimum external neck diameterof 50 mm, for
35、 the procedure.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 Subcommittee D02.02.0B /COMQ, the jointASTM-API Committee on Sampling, Sediment, Water.Current edi
36、tion approved May 1, 2007. Published June 2007. Originallyapproved in 1938. Last previous edition approved in 2006 as D 47302(2006).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume inform
37、ation, refer to the standards Document Summary page onthe ASTM website.3Available from American Petroleum Institute (API), 1220 L. St., NW, Wash-ington, DC 20005-4070, http:/api-ec.api.org.4Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, htt
38、p:/www.ansi.org.1*A Summary of Changes section appears at the end of this standard.5.1.1.2 CondenserA condenser in the form of a metal coilapproximately 25 mm in diameter and 50 mm in lengthattached to, and with the ends projecting through, a lid ofsufficient diameter to cover the neck of the flask
39、as shown inFig. 1. The coil shall be made from stainless steel, tin,tin-plated copper, or tin-plated brass tubing having an outsidediameter of 5 to 8 mm and a wall thickness of 1.5 mm. Ifconstructed of tin-plated copper or brass, the tin coating shallhave a minimum thickness of 0.075 mm. The exposed
40、 surfaceof the coil for cooling purposes is about 115 cm2.NOTE 2The use of a water flowmeter/controller unit that monitorswater flow to the condenser that shuts off the heat source when the flowrate drops below a pre-set limit has been found suitable to preventvaporized toluene from igniting. The us
41、e of such a device is recom-mended.5.1.1.3 Extraction Thimble5The extraction thimble shallbe of a refractory porous material, pore size 20.0 to 30.0 m (ascertified by the manufacturer), 25 mm in diameter by 70 mm inheight, weighing not less than 15 g and not more than 17 g.Suspend the thimble from t
42、he condenser coil by means of abasket so that it hangs approximately midway between thesurface of the extracting solvent and the bottom of thecondenser coil.5.1.1.4 Thimble BasketThe thimble basket shall becorrosion-resistant and shall be made of platinum, stainlesssteel, nickel-chromium alloy, or s
43、imilar material. Fig. 2 showsthe design and dimensions of two typical baskets that havebeen used successfully in the industry.5.1.1.5 Water CupUse a water cup when testing a sampledetermined to have a water content greater than 10 % volume(see Fig. 1, Apparatus B). The cup shall be made of glass,con
44、ical in shape, approximately 20 mm in diameter and 25 mmdeep, and have a capacity of approximately 3 mL.Aglass hookfused on the rim at one side is so shaped that when hung on thecondenser the cup hangs with its rim reasonably level. In thisprocedure, suspend the thimble basket as shown in Fig. 1,App
45、aratus A by means of the corrosion-resistant wire loopedover the bottom of the condenser coil and attached to the basketsupports, or as in Fig. 1, Apparatus B, where the wire supportsof the basket are attached to hooks soldered to the underside ofthe condenser lid.5.1.1.6 Source of HeatUse a source
46、of heat, preferably ahot plate operated under a ventilated hood, suitable for vapor-izing toluene (WarningFlammable.)5.2 Analytical BalanceUse an analytical balance, with anaccuracy of 0.1 mg. Verify the balance, at least annually,against weights traceable to a national standards body such asthe Nat
47、ional Institute of Standards and Technology (NIST).5.3 Non-aerating MixerUse a non-aerating mixer, meet-ing the verification of mixing efficiency requirements specifiedin Practice D 5854 (API Chapter 8.3). Either insertion mixers5The sole source of supply of the extraction thimble, AN 485, 25 3 70-m
48、m,coarse porosity, drawing number QA 005163, known to the committee at this timeis Saint-Gobain/Norton Industrial Ceramics Corporation of Worcester, MA. If youare aware of alternative suppliers, please provide this information to ASTMInternational Headquarters. Your comments will receive careful con
49、sideration at ameeting of the responsible technical committee,1which you may attend.NOTEApparatus B shows the water cup in position.FIG. 1 Extraction Apparatus for Determination of SedimentD473072or circulating mixers or circulating external mixers are accept-able provided they meet the criteria in Practice D 5854 (APIChapter 8.3).5.4 OvenUse an oven capable of maintaining a tempera-ture of 115 to 120C (240 to 250F).5.5 Cooling VesselUse a desiccator without desiccant as acooling vessel.5.6 Temperature Measuring DeviceSuch as a thermom-eter, capable of meas
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