1、Designation: D473 07 (Reapproved 2012)1Manual of Petroleum Measurement Standards (MPMS), Chapter 10.1Standard Test Method forSediment in Crude Oils and Fuel Oils by the ExtractionMethod1This standard is issued under the fixed designation D473; the number immediately following the designation indicat
2、es 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 last revision or reapproval.This standard has been approved for use by agencies of th
3、e U.S. Department of Defense.1NOTEIP information was removed editorially in March 2016.1. Scope1.1 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
4、levels may be determined.NOTE 1Precision on recycled oils and crankcase oils is unknown andadditional testing is required to determine that precision.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 This standard does not
5、 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-bility of regulatory limitations prior to use. For specificwarning statements, see 5.1.
6、1.6 and 6.1.2. Referenced Documents2.1 ASTM Standards:2D4057 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 Liquid Samplesof
7、 Petroleum and Petroleum Products (API MPMS Chap-ter 8.3)E29 Practice for Using Significant Digits in Test Data toDetermine Conformance with Specifications2.2 API Standards:3Chapter 8.1 Manual Sampling of Petroleum and PetroleumProducts (ASTM Practice D4057)Chapter 8.2 Automatic Sampling of Petroleu
8、m and Petro-leum Products (ASTM Practice D4177)Chapter 8.3 Mixing and Handling of Liquid Samples ofPetroleum and Petroleum Products (ASTM PracticeD5854)2.3 ISO Standard:45272 Toluene for industrial useSpecifications3. Summary of Test Method3.1 Extract test portion of a representative oil sample,cont
9、ained in a refractory thimble, with hot toluene until theresidue reaches constant mass. The mass of residue, calculatedas a percentage, 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 o
10、f refining and thebuying or selling of these commodities.5. Apparatus5.1 Usual laboratory apparatus and glassware, together withthe following are required for this test method.5.1.1 Extraction ApparatusUse the apparatus illustrated inFigs. 1 and 2 and consisting of the elements described in5.1.1.1 5
11、.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 the procedure.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and the API Committee onPetroleum Me
12、asurement, and is the direct responsibility of Subcommittee D02.02/COMQ on Hydrocarbon Measurement for Custody Transfer (Joint ASTM-API).Current edition approved Nov. 1, 2012. Published December 2012. Originallyapproved in 1938. Last previous edition approved in 2007 as D47307. DOI:10.1520/D0473-07R
13、12E01.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from American Petroleum Institute (API), 122
14、0 L. St., NW,Washington, 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, http:/www.ansi.org.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United State
15、s15.1.1.2 CondenserAcondenser 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 as shown inFig. 1. The coil shall be made from stainless steel, tin,tin-plated cop
16、per, 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 surfaceof the coil for cooling purposes is about 115 cm2.NOTE 2The use of a water
17、 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 use of such a device is recom-mended.5.1.1.3 Extraction Thimble5The extraction thimb
18、le 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 the condenser coil by means of abasket so that it hangs approximately midway betwee
19、n 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 similar material. Fig. 2 showsthe design and dimensions of two typical baskets that
20、 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,conical in shape, approximately 20 mm in diameter and 25 mmdeep, and have a capacity
21、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,Apparatus A by means of the corrosion-resistant wire loopedover the bottom of the con
22、denser 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 of heat, preferably ahot plate operated under a ventilated hood, suitable for vapo
23、r-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 National Institute of Standards and Technology (NIST).5.3 Non-aerating MixerUse a non
24、-aerating mixer, meet-ing the verification of mixing efficiency requirements specifiedin Practice D5854 (API Chapter 8.3). Either insertion mixers or5The sole source of supply of the extraction thimble, AN 485, 25 70-mm,coarse porosity, drawing number QA 005163, known to the committee at this timeis
25、 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 consideration at ameeting of the responsible technical committee,1which you may atten
26、d.NOTE 1Apparatus B shows the water cup in position.FIG. 1 Extraction Apparatus for Determination of SedimentD473 07 (2012)12circulating mixers or circulating external mixers are acceptableprovided they meet the criteria in Practice D5854 (API Chapter8.3).5.4 OvenUse an oven capable of maintaining a
27、 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 athermometer, capable of measuring the temperature of thesample to the nearest 1C (2F).6. Solvent6.1 TolueneReagent grade conforming to the speci
28、fica-tions of the Committee onAnalytical Reagents of theAmericanChemical Society (ACS)6or to Grade 2 of ISO 5272.(WarningFlammable. Keep away from heat, sparks andopen flame. Vapor harmful. Toluene is toxic. Particular careshall be taken to avoid breathing the vapors and to protect theeyes. Keep the
29、 container closed. Use with adequate ventilation.Avoid prolonged or repeated contact with the skin.)6.1.1 The typical characteristics for the ACS reagent areshown in Table 1.6Reagent Chemicals, American Chemical Society Specifications , AmericanChemical Society, Washington, DC. For suggestions on th
30、e testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia andNational Formulary, U.S. Pharmacopeial Convention, Inc., (USPC), Rockville, MD20852.FIG. 2 Basket Thimble SupportD473 0
31、7 (2012)137. Sampling7.1 Sampling shall include 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.7.2 Only use representative samples obtained as specified inPractices D4057 (API Chapter 8.1) and D4177
32、(API Chapter8.2) for this test method.7.3 Draw test portions from the laboratory samples imme-diately after thorough mixing. Heat viscous samples to atemperature which renders the sample liquid, and homogenizeusing a mixer as described in 5.3, as necessary. The difficultiesof obtaining a representat
33、ive test portion for this determinationare usually great, hence the need for great attention to themixing and aliquoting steps.7.4 As specified in Practice D5854 (API Chapter 8.3),record the temperature of the sample before mixing. Mix thelaboratory sample in its original container, using the mixing
34、time, mixing power (speed), and position relative to the bottomof the container appropriate to the crude petroleum or fuel oilbeing analyzed, and as established by the verification of mixingefficiency. To avoid the loss of light ends from crude oil orother samples containing volatile material, opera
35、te the mixerthrough a gland in the closure of the sample container. Take thetest portion for analysis immediately after mixing. Record thetemperature of the sample immediately after mixing. If the risein temperature during mixing exceeds 10C (20F), cool thesample, and repeat the mixing at a lower en
36、ergy input.Arise intemperature greater than 10C (20F) may result in a decreasein viscosity that is sufficient for the sediment to settle.8. Procedure8.1 For referee tests, use a new extraction thimble (5.1.1.3)prepared in accordance with 8.2. For routine tests, thimblesmay be reused. When reusing th
37、imbles, the extraction toconstant mass for one determination should be considered asthe preliminary extraction for the succeeding determination.After several determinations (the accumulated sediment maybe sufficient to interfere with further determinations), followthe procedure described in 8.3 to r
38、emove the combustibleportion of the accumulated sediment. Avoid excessive reuse ofthimbles, as over time the pores become clogged with inor-ganic material resulting in falsely high results. When in doubtregarding a higher than normal result, discard the thimble andretest using a new thimble.8.2 Prep
39、aration of a New ThimbleRub the outside surfacewith fine sandpaper and remove all loosened material with astiff brush. Give the thimble a preliminary extraction with thetoluene, allowing the solvent to drip from the thimble for atleast 1 h. Then dry the thimble for1hatatemperature of 115to 120C (240
40、 to 250F); cool in a cooling vessel, for 1 h, andweigh to the nearest 0.1 mg. Repeat the extraction until themasses of the thimble after two successive extractions do notdiffer by more than 0.2 mg.8.3 Preparation of a Used ThimbleRemove the combus-tible portion of the accumulated sediment by heating
41、 thethimble to a dull red heat for 20 min (preferably in an electricfurnace maintained at approximately 750C (1380F). Subjectthe thimble to a preliminary extraction as described in 8.2before using it for another determination.8.4 Place an estimated 10-g test portion of the sample in thethimble immed
42、iately after the sample has been mixed. Do notattempt to adjust this estimated 10-g portion to any exactpredetermined amount. Weigh the thimble plus test portion tothe nearest 0.01 g. Add 150 mL to 200 mL of toluene to theflask. Place the thimble in the extraction apparatus, place on theheat source,
43、 and extract with the hot toluene for 30 min afterthe solvent dripping from the thimble becomes colorless.Ensure that the rate of extraction is such that the surface of themixture of oil and toluene in the thimble does not rise higherthan to within 20 mm of the top.8.5 When testing samples determine
44、d to have a watercontent greater than 10 % volume, use the assembly shown inFig. 1,Apparatus B. In this procedure, remove any water in thetest portion as its toluene azeotrope and is collected in thewater cup, where it separates as a bottom layer. The toluenelayer overflows into the thimble. If the
45、cup becomes full ofwater, allow the apparatus to cool and empty the cup.8.6 After the extraction is completed, dry the thimble for 1h at 115 to 120C (240 to 250F) in the oven; cool in thecooling vessel, for 1 h; and weigh to the nearest 0.1 mg.8.7 Repeat the extraction, allowing the solvent to drip
46、fromthe thimble for at least 1 h but not longer than 1.25 h; dry, cool,and weigh the thimble as described in 8.6. Repeat thisextraction for further 1-h periods, if necessary, until the massesof the dried thimble plus sediment after two successiveextractions do not differ by more than 0.2 mg.TABLE 1
47、Typical Characteristics for ACS Reagent Grade TolueneAssay 99.5+ %Color (APHA) 10Boiling range (initial to dry point)A2.0CResidue after evaporation 0.001 %Substances darkened by H2SO4passes testSulfur compounds (as S) 0.003 %Water (H2O) (by Karl Fischer titration) 0.03 %ARecorded boiling point 110.6
48、C.D473 07 (2012)149. Calculation9.1 Calculate the sediment content of the sample as apercentage by mass of the original sample.S 5m32 m1m22 m13100 (1)where:S = sediment content of the sample as a percentage bymass,m1= mass, of the thimble, g,m2= mass, of the thimble plus test portion, g, andm3= mass
49、 of the thimble plus sediment, g.10. Report10.1 For each sample with a calculated sediment content0.005 % m/m as determined by Eq 1, report the sedimentcontent of the sample, as sediment by extraction, as a percent-age by mass, rounded to the nearest 0.01 % m/m followingPractice E29 rounding conventions. For each sample with acalculated sediment content 0.005 % m/m as determined inEq 1, report as, “0 % m/m.” The test result shall reference TestMethod D473/API MPMS Chapter 10.1 as the procedure used.NOTE 3Since water and sedimen
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