1、Designation: D4807 05 (Reapproved 2015)Manual of Petroleum Measurement Standards (MPMS), Chapter 10.8Standard Test Method forSediment in Crude Oil by Membrane Filtration1This standard is issued under the fixed designation D4807; the number immediately following the designation indicates the year ofo
2、riginal 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 U.S. Departme
3、nt of Defense.1. Scope1.1 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 The accepted unit of measure for this test method ismass %, but an equation to conv
4、ert 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 thesafety concerns, if any, associated with its use. It is theresponsibility of th
5、e 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 Documents2.1 ASTM Standards:2D473 Test Method for Sediment in Crude Oils and Fuel
6、Oilsby the Extraction MethodD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD4865 Guide for Generation and Dissipation of Static Elec-tricity in Petroleum Fuel SystemsD5854 Practice for Mixing and Handling o
7、f Liquid Samplesof Petroleum and Petroleum Products2.2 API Standards:3MPMS Chapter 8.1 Manual Sampling of Petroleum andPetroleum Products (ASTM Practice D4057)MPMS Chapter 8.2 Automatic Sampling of Petroleum andPetroleum Products (ASTM Practice D4177)MPMS Chapter 8.3 Mixing and Handling of Liquid Sa
8、mplesof Petroleum and Petroleum Products (ASTM PracticeD5854)MPMS Chapter 10.1 Test Method for Sediment in CrudeOils and Fuel Oils by the Extraction Method (ASTM TestMethod D473)2.3 ISO Standard:4ISO 5272:1979 Toluene for Industrial UseSpecifications3. Summary of Test Method3.1 A portion of a repres
9、entative crude oil sample isdissolved in hot toluene and filtered under vacuum through a0.45 m porosity membrane filter. 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 refin
10、ery operations and in crude oil com-merce.5. Apparatus5.1 Funnel and Filter Support 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 t
11、he funnel has a 40 mminside diameter and is designed to secure the 47 mm diameter1This test method is under 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
12、/COMQ on Hydrocarbon Measurement for Custody Transfer (Joint ASTM-API).Current edition approved April 1, 2015. Published May 2015. Originallyapproved in 1988. Last previous edition approved in 2010 as D4807 05 (2010).DOI: 10.1520/D4807-05R15.2For referenced ASTM standards, visit the ASTM website, ww
13、w.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.3Published as Manual of Petroleum Measurement Standards. Available fromAmerican Petroleum Institute (API), 1220 L. St.,
14、 NW,Washington, DC 20005-4070,http:/www.api.org.4Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.5The following filtration assembly was used in generating the precision:Millipore Corp., Ashly Rd., Bedford, MA 01730. Other
15、filtration assemblies alsomay be acceptable.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1filter against the filter support. The funnel can be jacketed tofacilitate heating the solvent funnel and sample during filtering.NOTE 1Use of
16、 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 glass center section about 40 mm to43 mm in diameter. The support base is designed to fit securelyagainst the funnel holding the filter in p
17、lace over the poroussection. The filter supports stem should be long enough toextend down into the filter flask such that the end is below thevacuum connection.5.1.3 Clamp AssemblyUse a spring or screw type clamp tosecure the funnel to the filter support. The clamp should betight enough to prevent t
18、he solvent from leaking through at thejunction between the glass and filter membrane. The exteriordimensions of the funnel and support are designed to facilitateclamping the two pieces together.5.1.4 Rubber StopperUse a single-hole, capable of hold-ing the lower stem of the filter support securely o
19、nto 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 with 0.45 m pore size.65.3 OvenUse an oven capable of maintaining a tempera-ture of 105 C 6 2 C (220 F 6 4 F).5.4 Vacuum PumpUse a vacuum p
20、ump 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 nearest 0.0001 g. Verify the balance, atleast annually, against weights traceable to a national metrol-ogy institute such as the
21、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 thefilter apparatus and connected to a circulating bath to maintainthe oil in the funnel at 90 C 6 2 C (see Fig. 1). Alternativemethods of
22、 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 requirements specified in PracticeD5854 (API MPMS Chapter 8.3). Either insertion mixers orcirculating mixers are acceptable provided they
23、 meet thecriteria in Practice D5854 (API MPMS Chapter 8.3).5.8 Cooling VesselUse a desiccator or other type of tightlycovered vessel for cooling the membrane filter before weigh-ing. The use of a desiccant/drying agent is not recommended.5.9 Ground/Bond WireUse a 0.912 mm to 2.59 mm (No.10 through N
24、o. 19) bare stranded flexible, stainless steel orcopper wire installed in the flask through the vacuum connec-tion and connected to ground.6. Reagents6.1 TolueneReagent grade chemicals shall be used in alltests. Unless otherwise indicated, it is intended that all reagentsshall conform to the specifi
25、cations 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 it is first ascertained thatthe reagents lot or batch is of sufficiently high purity to permitits use without lessenin
26、g 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 the vapors and to protect theeyes. Keep the container closed. Use with adequate ventilation.Avoid prolonged or repeated
27、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 othersystem, and to transfer the sample into the laboratory testcontainer. The laboratory test container and sample volumeshall
28、 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 Laboratory SampleUse only representative samplesobtained as specified in Practice D4057 (API MPMS Chapter8.1) or Practice D4177
29、 (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 following sample preparationand handling procedure shall apply.7.3.1 Mix the test sample of crude oil at room temperaturein
30、the original container immediately (within 15 min) beforeanalysis 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 possible. The15 min interval
31、mentioned above is a general guideline which may notapply to all crudes, especially some light crudes which do not hold water6The 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 poro
32、sity also may be acceptable.7Reagent 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 LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and
33、the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.FIG. 1 Membrane Filtration AssemblyD4807 05 (2015)2and 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 t
34、han 10 C (20 F), 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 D5854 (API MPMS Chapter 8.3), must be met. Themixer must be re-evaluated followi
35、ng any changes in the typeof crude, quantity of crude, or shape of the sample container.7.3.3 For small test sample volumes, 50 mL 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 P
36、ractice D5854 (APIMPMS Chapter 8.3). Clean and dry the mixer betweensamples.8. Procedure8.1 Filter PreparationPrepare nylon filters by heating inan oven at 105 C 6 2 C (220 F 6 4 F) for 15 min. Cooland store the dried filters in a cooling vessel (desiccatorwithout desiccant) until needed. Use only n
37、ew filters.8.2 Weigh 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 he
38、ating coil to the circulating 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 C 6 2 C (195 F 6 4 F).NOTE 3Care should be taken not to overheat the funnel so as to causeevaporation of the toluene and g
39、lazing of the filter.8.5 Sample 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 C 6 2 C (195 F 6 4 F).Maintain the temperature at 90 C 6 2 C (195 F 6 4 F) forabout
40、 15 min to dissolve any wax in the crude.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 min to 15 min. If the nature of the crude (forexample, heavy versus light
41、gravity or high versus lowviscosity) or the amount of sediment causes the filtration toproceed extremely slowly (for example, filtering times greaterthan 30 min), reduce the sample size to 5 g or less and repeatthe test. Keep the volume of toluene at 100 mL.NOTE 4If the filtration of a given crude t
42、ypically takes less than10 min and the sample stays at 90 C 6 2 C (195 F 6 4 F) during thistime, 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 (90 C, 195
43、F) until no oil is visible on the filter.With the vacuum 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
44、 wash the edges after disassembly. However, ifupon removing 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(90 C, 195 F).8.9 If the filter is completely or partially covered with
45、blackor dark brown crude oil residue after the washing step 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
46、.10 If the appearance of the filter is acceptable (as in 8.9)then carefully remove it and place it in an oven at 105 C(220 F) 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 follow
47、s:S 5m22 m1ms3100 (1)where:S = sediment content of the sample 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 tes
48、t reportshall reference this Test Method D4807 (API MPMS 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 besan
49、d (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 sediment by2.0 and multiply by the relative density of the crude oil. (Note that thiscalculation is provided for convenience only, and the precision and biasfor this standard are based on mass percent sediment and not on volumeperce
