1、Designation: D473 07 (Reapproved 2012)Manual of Petroleum Measurement Standards (MPMS), Chapter 10.1Designation: 53/82Standard 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 de
2、signation 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 last revision or reapproval.This standard has been approved for use
3、by agencies of the Department of Defense.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 levels may be determined.NOTE 1Precision on re
4、cycled 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 purport to address all of thesafety concerns,
5、 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 5.1.1.6 and 6.1.2. Referenced Documents2.1 ASTM St
6、andards: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 Petroleum and Petroleum Products (API MPMS Ch
7、ap-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 Petroleum and Petro-leum Products (ASTM Practice D4177
8、)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,contained in a refractory thimble, with hot toluen
9、e 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 of refining and thebuying or selling of these c
10、ommodities.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 in5.1.1.1-5.1.1.3.1This test method is under the jurisdic
11、tion of ASTM Committee D02 onPetroleum Products and Lubricants and the API Committee on PetroleumMeasurement, and is the direct responsibility of Subcommittee D02.02 /COMQ onHydrocarbon Measurement for Custody Transfer (Joint ASTM-API).Current edition approved Nov. 1, 2012. Published December 2012.
12、Originallyapproved in 1938. Last previous edition approved in 2007 as D47307. DOI:10.1520/D0473-07R12.2For 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
13、Document Summary page onthe ASTM website.3Available from American Petroleum Institute (API), 1220 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 I
14、nternational, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15.1.1.1 Extraction FlaskUse a wide-neck (Erlenmeyer)flask of 1-L capacity, with a minimum external neck diameterof 50 mm, for the procedure.5.1.1.2 CondenserAcondenser in the form of a metal coilapproxi
15、mately 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 copper, or tin-plated brass tubing having an outsidediameter of 5 t
16、o 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 flowmeter/controller unit that monitorswater flow to the conden
17、ser 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 thimble shallbe of a refractory porous material, pore size 20.0 to 30
18、.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 between thesurface of the extracting solvent and the bottom of thecond
19、enser 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 havebeen used successfully in the industry.5.1.1.5 Water CupUse
20、 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 of approximately 3 mL.Aglass hookfused on the rim at one side is
21、 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 condenser coil and attached to the basketsupports, or as in Fig. 1,
22、 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 vapor-izing toluene (WarningFlammable.)5.2 Analytical BalanceUse an
23、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).5The sole source of supply of the extraction thimble, AN 485, 25 70-mm,coarse porosity, drawing
24、 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 consideration at ameeting of
25、the responsible technical committee,1which you may attend.NOTE 1Apparatus B shows the water cup in position.FIG. 1 Extraction Apparatus for Determination of SedimentD473 07 (2012)25.3 Non-aerating MixerUse a non-aerating mixer, meet-ing the verification of mixing efficiency requirements specifiedin
26、Practice D5854 (API Chapter 8.3). Either insertion mixers orcirculating 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 tempera-ture of 115 to 120C (240 to 250F).5.5 Cooling VesselUse
27、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 specifica-tions of the Committee onAnalytical Reagents of theAmericanC
28、hemical 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 the6Reagent Chemicals, American Chemical Society Specifications , AmericanChemical
29、 Society, Washington, DC. For suggestions on the 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), Rockvil
30、le, MD20852.FIG. 2 Basket Thimble SupportD473 07 (2012)3eyes. Keep the 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 1.7. Sampling7.1 Sampling shall include all steps required
31、 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 (API Chapter8.2) for this test method.7.3 Draw test portions from
32、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 representative test portion for this determinationare usually great, hence th
33、e 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 mixingtime, mixing power (speed), and position relative to the bottomof
34、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, operate the mixerthrough a gland in the closure of the sample container
35、. 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 energy input.Arise intemperature greater than 10C (20F) may result i
36、n 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 thimbles, the extraction toconstant mass for one determination shoul
37、d 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 remove the combustibleportion of the accumulated sediment. Avoid ex
38、cessive 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 Preparation of a New ThimbleRub the outside surfacewith fine sandpaper
39、 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 to 250F); cool in a cooling vessel, for 1 h, andweigh to the near
40、est 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 thethimble to a dull red heat for 20 min (preferably in an electr
41、icfurnace 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 immediately after the sample has been mixed. Do notattempt to adjust th
42、is 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, and extract with the hot toluene for 30 min afterthe solvent drip
43、ping 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 determined to have a watercontent greater than 10 % volume, use the assembl
44、y 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 cup becomes full ofwater, allow the apparatus to cool and empty th
45、e 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 fromthe thimble for at least 1 h but not longer than 1.25 h; dry,
46、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 Typical Characteristics for ACS Reagent Grade TolueneAssay 99.5+ %
47、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 110.6C.D473 07 (2012)49. Calculation9.1 Calculate the sediment content
48、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 of the thimble plus sediment, g.10. Report10.1 For each sample wit
49、h 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 sediment values are commonly reported asvolume percent, calculate the volume of th
