1、Designation: D473 07 (Reapproved 2017)Manual 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 indicate
2、s 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 the
3、 U.S. 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 recycled oils
4、 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, if any, as
5、sociated 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 6.1.1.4 This international standard was developed
6、 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 Document
7、s2.1 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 Petroleum and Petroleum Products
8、(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 Petroleum and Petro-leum Products (ASTM Pr
9、actice 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,contained in a refractory thimble, wit
10、h 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 of refining and thebuying or sellin
11、g 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 5.1.1.3.1This test method is under
12、the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and the API Committee onPetroleum Measurement, and is the direct responsibility of Subcommittee D02.02/COMQ on Hydrocarbon Measurement for Custody Transfer (Joint ASTM-API).Current edition approved June 1, 2017
13、. Published July 2017. Originally approvedin 1938. Last previous edition approved in 2012 as D473 07 (2012)1. DOI:10.1520/D0473-07R17.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume info
14、rmation, refer to the standards 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, htt
15、p:/www.ansi.org. Jointly copyrighted by ASTM International, 100 Barr Harbor Drive, PO 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 rec
16、ognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.15.1.1.1 Extraction FlaskUse a wide-neck (Erlenmeyer)flask of 1
17、 L capacity, with a minimum external neck diameterof 50 mm, for the procedure.5.1.1.2 CondenserAcondenser in the form of a metal coilapproximately 25 mm in diameter and 50 mm in length at-tached to, and with the ends projecting through, a lid ofsufficient diameter to cover the neck of the flask as s
18、hown inFig. 1. The coil shall be made from stainless steel, tin,tin-plated copper, or tin-plated brass tubing having an outsidediameter of 5 mm 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
19、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 use
20、 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 m to30.0 m (as certified by the manufacturer), 25 mm in diameterby 70 mm in height, weighing not less than 15 g and not morethan 17 g. Suspend the thimble from
21、the condenser coil bymeans of a basket so that it hangs approximately midwaybetween the surface of the extracting solvent and the bottom ofthe condenser coil.5.1.1.4 Thimble BasketThe thimble basket shall becorrosion-resistant and shall be made of platinum, stainlesssteel, nickel-chromium alloy, or
22、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 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,co
23、nical 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,Ap
24、paratus 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
25、 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 Na
26、tional Institute of Standards and Technology (NIST).5The sole source of supply of the extraction thimble, AN 485, 25 mm 70 mm,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 alte
27、rnative suppliers, please provide this information to ASTMInternational Headquarters. Your comments will receive careful consideration at ameeting of the responsible technical committee,1which you may attend.NOTE 1Apparatus B shows the water cup in position.FIG. 1 Extraction Apparatus for Determinat
28、ion of SedimentD473 07 (2017)25.3 Non-aerating MixerUse a non-aerating mixer, meet-ing the verification of mixing efficiency requirements specifiedin Practice D5854 (API Chapter 8.3). Either insertion mixers orcirculating mixers or circulating external mixers are acceptableprovided they meet the cri
29、teria in Practice D5854 (API Chapter8.3).5.4 OvenUse an oven capable of maintaining a tempera-ture of 115 C to 120 C (240 F to 250 F).5.5 Cooling VesselUse a desiccator without desiccant as acooling vessel.5.6 Temperature Measuring DeviceSuch as athermometer, capable of measuring the temperature of
30、thesample to the nearest 1 C (2 F).6. Solvent6.1 TolueneReagent grade conforming to the specifica-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.
31、 Particular careshall be taken to avoid breathing the vapors and to protect the6Reagent Chemicals, American Chemical Society Specifications , AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for Labo
32、ratoryChemicals, 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 07 (2017)3eyes. Keep the container closed. Use with adequate ventilation.Avoid prolonged or repe
33、ated 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 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
34、 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 the laboratory samples imme-diately after thorough mixing. Heat viscous samples to atemperature which renders the sample liquid, and homogeniz
35、eusing a mixer as described in 5.3, as necessary. The difficultiesof obtaining a representative 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 th
36、e sample before mixing. Mix thelaboratory sample in its original container, using the mixingtime, 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 avo
37、id 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. Take thetest portion for analysis immediately after mixing. Record thetemperature of the sample immediately after mixing. If the risein temp
38、erature during mixing exceeds 10C (20F), cool thesample, and repeat the mixing at a lower energy 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.
39、3)prepared in accordance with 8.2. For routine tests, thimblesmay be reused. When reusing thimbles, the extraction toconstant mass for one determination should be considered asthe preliminary extraction for the succeeding determination.After several determinations (the accumulated sediment maybe suf
40、ficient to interfere with further determinations), followthe procedure described in 8.3 to remove 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 doubtregar
41、ding 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 and remove all loosened material with astiff brush. Give the thimble a preliminary extraction with thetoluene, allowing the solvent to drip f
42、rom the thimble for atleast 1 h. Then dry the thimble for 1 h at a temperature of115 C to 120 C (240 F to 250 F); cool in a cooling vessel,for 1 h, and weigh to the nearest 0.1 mg. Repeat the extractionuntil the masses of the thimble after two successive extractionsdo not differ by more than 0.2 mg.
43、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 electricfurnace maintained at approximately 750 C (1380 F). Sub-ject the thimble to a preliminary extraction as described in 8.2before us
44、ing 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 this estimated 10 g portion to any exactpredetermined amount. Weigh the thimble plus test portion tothe nearest 0.01 g. Add 150 m
45、L 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 dripping from the thimble becomes colorless.Ensure that the rate of extraction is such that the surface of themixture of oil and to
46、luene 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 assembly shown inFig. 1,Apparatus B. In this procedure, remove any water in thetest portion as its toluene azeotrope and is collected
47、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 the cup.8.6 After the extraction is completed, dry the thimble for 1 hat 115 C to 120 C (240 F to 250 F) in the oven; cool in the
48、cooling 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, cool,and weigh the thimble as described in 8.6. Repeat thisextraction for further 1 h periods, if necessary, until the ma
49、ssesof 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+ %Color (APHA) 10Boiling range (initial to dry point)A2.0 CResidue 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 C.D473 07 (2017)49. Calculation9.1 Calculate the sediment content of the sample as apercentage by mass of the original
