1、Designation: D 4807 05e1Designation: Manual of Petroleum Measurement Standards (MPMS), Chapter 10.8An American National StandardStandard Test Method forSediment in Crude Oil by Membrane Filtration1This standard is issued under the fixed designation D 4807; the number immediately following the design
2、ation 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 (e) indicates an editorial change since the last revision or reapproval.This standard has been approved for use by
3、agencies of the Department of Defense.e1NOTEFootnote 5 was updated editorially in August 2005.1. Scope*1.1 This test method covers the determination of sedimentin crude oils by membrane filtration. This test method has beenvalidated for crude oils with sediments up to approximately0.15 mass %.1.2 Th
4、e accepted unit of measure for this test method ismass %, but an equation to convert to volume % is provided(see Note 6).1.3 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.4 This standard does not purport to address all of t
5、hesafety 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 6.1 and Annex A1.2. Referenced D
6、ocuments2.1 ASTM Standards:2D 473 Test Method for Sediment in Crude Oils and FuelOils by the Extraction Method (API MPMS Chapter 10.1)D 4057 Practice for Manual Sampling of Petroleum andPetroleum Products (API MPMS Chapter 8.1)D 4177 Practice for Automatic Sampling of Petroleum andPetroleum Products
7、 (API MPMS Chapter 8.2)D 4865 Guide for Generation and Dissipation of StaticElectricity in Petroleum Fuel SystemsD 5854 Practice for Mixing and Handling of LiquidSamples of Petroleum and Petroleum Products (APIMPMS Chapter 8.3)2.2 API Standards:3MPMS Chapter 8.1 Manual Sampling of Petroleum andPetro
8、leum Products (ASTM Practice D 4057)MPMS Chapter 8.2 Automatic Sampling of Petroleum andPetroleum Products (ASTM Practice D 4177)MPMS Chapter 8.3 Mixing and Handling of Liquid Samplesof Petroleum and Petroleum Products (ASTM PracticeD 5854)MPMS Chapter 10.1 Test Method for Sediment in CrudeOils and
9、Fuel Oils by the Extraction Method (ASTM TestMethod D 473)2.3 ISO Standard:4ISO 5272:1979 Toluene for Industrial UseSpecifications3. Summary of Test Method3.1 A portion of a representative crude oil sample isdissolved in hot toluene and filtered under vacuum through a0.45-m porosity membrane filter.
10、 The filter with residue iswashed, dried, and weighed to give the final result.4. Significance and Use4.1 A knowledge of the sediment content of crude oil isimportant both in refinery operations and in crude oil com-merce.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum
11、Products and Lubricants and the API Committee on Petroleum Measure-ment, and is the direct responsibility of Subcommittee D02.02/COMQ, the jointASTM-API committee on Static Petroleum Measurement.This test method has beenapproved by the sponsoring committee and accepted by the Cooperating Societiesin
12、 accordance with established procedures.Current edition approved June 1, 2005. Published July 2005. Originally approvedin 1988. Last previous edition approved in 1999 as D 480788(1999).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceast
13、m.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Published as Manual of Petroleum Measurement Standards.Available from theAmerican Petroleum Institute (API), 1220 L St., NW, Washington DC 20005.4Available from American Natio
14、nal Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5. Apparatus5.1 Funnel and Filter Support
15、AssemblyUse an assemblydesigned to hold 47-mm diameter filters as was used in thedevelopment of this test method (see Fig. 1).55.1.1 Filter FunnelUse a filter funnel with a 250 mLminimum capacity. The lower part of the funnel has a 40-mminside diameter and is designed to secure the 47-mm diameterfil
16、ter against the filter support. The funnel can be jacketed tofacilitate heating the solvent funnel and sample during filtering.NOTE 1Use of a glass funnel should minimize the effect of staticelectricity when filtering.5.1.2 Filter SupportUse a support base for the filter thathas a porous scintered g
17、lass center section about 40 to 43 mmin diameter. The support base is designed to fit securely againstthe funnel holding the filter in place over the porous section.The filter supports stem should be long enough to extend downinto the filter flask such that the end is below the vacuumconnection.5.1.
18、3 Clamp AssemblyUse a spring or screw type clampto secure the funnel to the filter support. The clamp should betight enough to prevent the solvent from leaking through at thejunction between the glass and filter membrane. The exteriordimensions of the funnel and support are designed to facilitatecla
19、mping the two pieces together.5.1.4 Rubber StopperUse a single-hole, capable of hold-ing the lower stem of the filter support securely onto thefiltering flask.5.1.5 Vacuum Filtering FlaskUse a 500 mL or largervacuum filtering flask.5.2 Membrane FilterUse a nylon membrane filter, 47 mmin diameter wit
20、h 0.45-m pore size.65.3 OvenUse an oven capable of maintaining a tempera-ture of 105 6 2C (220 6 4F).5.4 Vacuum PumpUse a vacuum pump capable of reduc-ing and maintaining the pressure at 80 kPa (24 in. Hg)during the filtering.5.5 Analytical BalanceUse an analytical balance capableof measuring to the
21、 nearest 0.0001 g. Verify the balance, atleast annually, against weights traceable to a national metrol-ogy institute such as the National Institute of Standards andTechnology (NIST).5.6 Heating Coil for Filter AssemblyUse copper tubing(3.175 mm or18-in. diameter) wound around the funnel on thefilte
22、r apparatus and connected to a circulating bath to maintainthe oil in the funnel at 90 6 2C (see Fig. 1). Alternativemethods of heating the funnel such as heating tape or glassthermal jacket could also be used.5.7 MixerUse a nonaerating, high-speed mixer meetingthe verification efficiency requiremen
23、ts specified in PracticeD 5854 (API MPMS Chapter 8.3). Either insertion mixers orcirculating mixers are acceptable provided they meet thecriteria in Practice D 5854 (API MPMS Chapter 8.3).5.8 Cooling VesselUse a desiccator or other type oftightly covered vessel for cooling the membrane filter before
24、weighing. The use of a desiccant/drying agent is not recom-mended.5.9 Ground/Bond WireUse a 0.9122.59 mm (No. 10through No. 19) bare stranded flexible, stainless steel or copperwire installed in the flask through the vacuum connection andconnected to ground.6. Reagents6.1 TolueneReagent grade chemic
25、als shall be used in alltests. Unless otherwise indicated, it is intended that all reagentsshall conform to the specifications of the Committee onAnalytical Reagents of the American Chemical Society, wheresuch specifications are available,7or to Grade 2 of ISO 5272.Other grades may be used, provided
26、 it is first ascertained thatthe reagents lot or batch is of sufficiently high purity to permitits use without lessening the accuracy of the determination.(WarningFlammable. Keep away from heat, sparks andopen flame. Vapor harmful. Toluene is toxic. Particular careshall be taken to avoid breathing t
27、he vapors and to protect theeyes. Keep the container closed. Use with adequate ventilation.Avoid prolonged or repeated contact with the skin.)7. Sampling, Test Specimens7.1 Sampling, shall include all the steps required to obtain arepresentative portion of the contents of any pipe, tank, or othersys
28、tem, and to transfer the sample into the laboratory testcontainer. The laboratory test container and sample volumeshall be of sufficient dimensions and volume to allow mixing asdescribed in 7.3.1. Mixing is required to properly dispersesediment as well as any water present in the sample.7.2 Laborato
29、ry SampleUse only representative samplesobtained as specified in Practice D 4057 (API MPMS Chapter8.1) or Practice D 4177 (API MPMS Chapter 8.2) for this testmethod. Analyze samples within two weeks after taking thesample. Retaining samples longer may affect the results.7.3 Sample PreparationThe fol
30、lowing sample prepara-tion and handling procedure shall apply.7.3.1 Mix the test sample of crude oil at room temperaturein the original container immediately (within 15 min) before5The following filtration assembly was used in generating the precision:Millipore Corp., Ashly Rd., Bedford, MA 01730. O
31、ther filtration assemblies alsomay be acceptable.6The following filter was used in generating the precision: MSI Nylon 60Membrane Filter from Fisher Scientific, Catalog Number NO-4-SP047-00. Othernylon filters of 0.45-m porosity also may be acceptable.7Reagent Chemicals, American Chemical Society Sp
32、ecifications, AmericanChemical 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 Pharmacopeiaand National Formulary, U.S. Pharmacopeial Con
33、vention, Inc. (USPC), Rockville,MD.FIG. 1 Membrane Filtration AssemblyD480705e12analysis to ensure complete homogeneity. A test sample drawndirectly from a large volume dynamic mixing system shall beanalyzed within 15 min or else remix as follows:NOTE 2Analysis should follow mixing as soon as possib
34、le. The15-min interval mentioned above is a general guideline which may notapply to all crudes, especially some light crudes which do not hold waterand sediment in suspension for even this short a time.7.3.2 Mixing of the sample should not increase the tempera-ture of the sample more than 10C (20F),
35、 or a loss of watermay occur affecting the samples composition. The type ofmixer depends on the quantity of crude. Before any unknownmixer is used, the specifications for the homogenization test,Practice D 5854 (API MPMS Chapter 8.3), must be met. Themixer must be re-evaluated following any changes
36、in the typeof crude, quantity of crude, or shape of the sample container.7.3.3 For small test sample volumes, 50 to 300 mL, anonaerating, high-speed, shear mixer is required. Use themixing time, mixing speed, and height above the bottom of thecontainer found to be satisfactory in Practice D 5854 (AP
37、IMPMS Chapter 8.3). Clean and dry the mixer betweensamples.8. Procedure8.1 Filter PreparationPrepare nylon filters by heating inan oven at 105 6 2C (220 6 4F) for 15 min. Cool and storethe dried filters in a cooling vessel (desiccator without desic-cant) until needed. Use only new filters.8.2 Weigh
38、the filter immediately before use to the nearest0.0001 g.8.3 Using tweezers, place the membrane filter on the centerof the filter support, which is mounted on the filtering flaskwith a rubber stopper.Attach the funnel to the filter support andclamp it securely.8.4 Connect the heating coil to the cir
39、culating bath andplace the coil around the lower part of the funnel. Set thetemperature of the circulating bath so as to maintain the oil inthe funnel at 90 6 2C (195 6 4F).NOTE 3Care should be taken not to overheat the funnel so as to causeevaporation of the toluene and glazing of the filter.8.5 Sa
40、mple AdditionInto a 200-mL beaker, weigh 10 g ofa thoroughly mixed sample (see Section 7) to the nearest0.0001 g. Add 100 mL of toluene to the beaker and heat themixture with stirring to 90 6 2C (195 6 4F). Maintain thetemperature at 90 6 2C (195 6 4F) for about 15 min todissolve any wax in the crud
41、e.8.6 Start the vacuum pump and adjust the vacuum to80 kPa (24 in. Hg). Carefully pour the sample mixture intothe filter funnel in three portions. Generally the sample shouldfilter in 10 to 15 min. If the nature of the crude (for example,heavy versus light gravity or high versus low viscosity) or th
42、eamount of sediment causes the filtration to proceed extremelyslowly (for example, filtering times greater than 30 min),reduce the sample size to5gorless and repeat the test. Keepthe volume of toluene at 100 mL.NOTE 4If the filtration of a given crude typically takes less than10 min and the sample s
43、tays at 90 6 2C (195 6 4F) during this time,then external heating of the filter funnel may not be necessary.8.7 Filter WashingBefore the last portion of sample hascompletely filtered, wash the funnel and filter with 50 mL ofhot toluene (90C, 195F) until no oil is visible on the filter.With the vacuu
44、m on, leave the filter on the apparatus for 2 min.8.8 Apparatus DisassemblyDisassemble the filter appara-tus by removing the clamp and funnel. Inspect the condition ofthe filter. If the filter has been properly mounted, it may not benecessary to wash the edges after disassembly. However, ifupon remo
45、ving the funnel dark spots are observed around theedge of the filter further washing is necessary.With the vacuumon, use a dropper to wash the filters edges with hot toluene(90C, 195F).8.9 If the filter is completely or partially covered with blackor dark brown crude oil residue after the washing st
46、ep above,then discard the filter and repeat the test with a smaller samplesize.NOTE 5Normally the color of the sediment on the filter is gray or lighttan. A black or deep brown colored deposit on the filter is indicative ofincomplete washing.8.10 If the appearance of the filter is acceptable (as in
47、8.9)then carefully remove it and place it in an oven at 105C(220F) for 15 min. Cool in the cooling vessel to roomtemperature (5 to 10 min) and reweigh to the nearest 0.0001 g.9. Calculation9.1 Calculate the mass percent of sediment as follows:S 5m22 m1ms3 100 (1)where:S = sediment content of the sam
48、ple as a percentage bymass,m1= mass of the filter, g,m2= mass of the filter with the sediment, g, andms= mass of the sample, g.10. Report10.1 Report results to the nearest 0.001 % as the masspercent of sediment by membrane filtration. The test reportshall reference this Test Method D 4807 (API MPMS
49、Chapter10.8) as the procedure used.NOTE 6Since water and sediment values are commonly reported asvolume percent, calculate the volume of the sediment as a percentage ofthe original sample.As a major portion of the sediment probably would besand (silicon dioxide, which has a density of 2.32) and a small amount ofother naturally occurring materials (with a relative density lower than thatof sand), use an arbitrary density of 2.0 for the resulting sediment. Then,to obtain volume percent sediment, divide the mass percent sedim
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