1、Designation: D 4870 09Designation: 375/99An American National StandardStandard Test Method forDetermination of Total Sediment in Residual Fuels1This standard is issued under the fixed designation D 4870; the number immediately following the designation indicates the year oforiginal adoption or, in t
2、he 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.1. Scope*1.1 This test method covers the determination of totalsediment up to 0.40 % m/m for dist
3、illate fuel oils containingresidual components and to 0.50 % m/m in residual fuel oilshaving a maximum viscosity of 55 cSt (mm2/s) at 100C. Somefuels can exceed the maximum filtration time specified in thistest method due to factors other than the presence of significantquantities of insoluble organ
4、ic or inorganic material. This testmethod can be used for the assessment of total sediment afterregimes of fuel pretreatment designed to accelerate the agingprocess.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 st
5、andard does not 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 state
6、ments, see 7.2, 7.3, Annex A1, and X1.6.1.2. Referenced Documents2.1 ASTM Standards:2D 4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD 4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsE1 Specification for ASTM Liquid-in-Glass Thermometers3. Terminology3.1
7、Definitions of Terms Specific to This Standard:3.1.1 total sedimentthe sum of the insoluble organic andinorganic material that is separated from the bulk of theresidual fuel oil by filtration through a Whatman GF/A filtermedium, and that is also insoluble in a predominantly paraf-finic solvent.4. Su
8、mmary of Test Method4.1 A weighed quantity (10 g) of the oil sample is filteredthrough the prescribed apparatus at 100C. After solventwashing and drying the total sediment on the filter medium isweighed. The test is to be carried out in duplicate.5. Significance and Use5.1 Appreciable amounts of sed
9、iment in a residual fuel oilcan cause fouling of facilities for handling, and give problemsin burner mechanisms. Sediment can accumulate in storagetanks, on filter screens, or on burner parts, resulting inobstruction of the flow of oil from the tank to the burner.6. Apparatus6.1 Filtration Apparatus
10、, constructed of brass, with coppersteam coils attached, suitably supported above a vacuum flaskappropriately protected against the effects of implosion. SeeFigs. 1 and 2.6.2 Temperature Measuring Device, capable of measuringthe temperature in the range from 95 to 105C with an accuracyof 0.5C.6.3 Ov
11、en, electric, capable of maintaining a temperature of110 6 1C. The oven should be capable of safely evaporatingthe solvent without risk of fire.6.4 Stirring Rod, glass or polytetrafluoroethylene (PTFE)approximately 150 mm in length and 3 mm in diameter.6.5 Beaker, glass, 30 mL capacity, either squat
12、 form with lipor conical.6.6 Small Dishes, such as watch glasses or Petri dishes.6.7 Hotplate, electric.6.8 Steam Generator, to provide steam at 100 6 1C.6.9 Vacuum Source, capable of providing the specifiedvacuum.6.10 Vacuum Gauge, capable of measuring the specifiedvacuum.1This test method is under
13、 the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.14 on Stability and Cleanliness of Liquid Fuels.Current edition approved April 15, 2009. Published May 2009. Originallyapproved in 1988. Last previous edition approved in 2
14、007 as D 487007a.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.1*A Summary of Changes section appears at th
15、e end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6.11 Filter Medium, Whatman glass fiber filter medium,Grade GF/A, 47 mm diameter.6.12 High Speed Mixer, any convenient type, minimumspeed 400 rpm.6.13 Desiccator.6
16、.14 Cooling Vessel, a desiccator or other type of tightlycovered vessel for cooling the filter media before weighing.The use of a drying agent is not recommended.6.15 Syringe or Graduated Wash Bottle, minimum capacity25 mL, graduated in 0.5 mL increments.6.16 Forceps, spade-ended.7. Reagents and Mat
17、erials7.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.3Other grad
18、es may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.7.2 Normal Heptane, minimum 99.75 % purity.(WarningFlammable, vapor harmful if inhaled. See A1.1.)7.3 Toluene, at least reagent grade pu
19、rity. (WarningFlammable, vapor harmful. See A1.2.)7.4 Wash Solvent, consisting of 85 volume % n-heptane(7.2) and 15 volume % toluene (see 7.3).8. Sampling8.1 Sample in accordance with Practice D 4057 or PracticeD 4177.3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Soc
20、iety, Washington, DC. For Suggestions on the testing of reagents notlisted by the American Chemical Society, see Annual Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD
21、.FIG. 1 Detail of Filtration CellFIG. 2 Arrangement of Filtration ApparatusD48700929. Procedure9.1 Sample PreparationMix the whole sample, as re-ceived, thoroughly using a high speed mixer when practicable,for 30 s. In all cases a sample taken on a glass or PTFE roddipped to the bottom of the contai
22、ner must show a homoge-neous appearance. For fuels with a high wax content (high pourpoint), or of very high viscosity, the sample must be heatedbefore stirring. The temperature must be either 15C above thepour point in the case of low viscosity fuels, or that equivalentto 150 to 250 cSt in the case
23、 of high viscosity fuels. In no caseshould the temperature exceed 80C.9.2 Filter PreparationFor each test, dry two filter mediafor 20 min in the oven at 110C. Transfer each filter medium,separately, rapidly to a cooling vessel and allow to cool toroom temperature for 20 min. Weigh each filter medium
24、 to thenearest 0.0001 g.NOTE 1The Whatman GF/A filter media are fragile and are to behandled with care. Before use, check each medium for consistency, andthe possible presence of small defects (holes).NOTE 2For convenience, place the filters on numbered small dishes(6.6) during drying and cooling.9.
25、3 Apparatus AssemblyBefore use, check that the filtersupport screen is clean. If necessary, the screen must becleaned by boiling in a high boiling point aromatic solvent.When more than 2 % of the sinter area remains blocked byparticulate matter after such cleaning, discard the screen andinstall a ne
26、w one.9.3.1 The filtration unit must be clean and dry beforeassembly. Stack the two previously dried and weighed filtermedia on top of the sinter support with the mesh imprint sidedown, using forceps. Apply slight vacuum to aid in centeringthe filter media, and place the top portion of the filtratio
27、napparatus carefully on to the media before clamping. Shut offthe vacuum and pass steam at 100 6 1C through theheating/cooling coils for 10 min prior to sample addition.9.4 Sample AdditionInto a 30 mL beaker, pour approxi-mately 11 g of the fuel sample prepared as described in 9.1 andweigh to the ne
28、arest 0.01 g. Connect the vacuum source andapply vacuum to an absolute pressure of 40 6 2 kPa minimum(61.3 kPa vacuum). Heat the contents of the beaker to 100 62C. Then transfer the contents at 100 6 2C (Note 3)tothecenter of the filter medium, taking care that no sample touchesthe walls during tran
29、sfer (Note 4). Reweigh the beaker to thenearest 0.01 g. The quantity transferred should be 106 0.5 g.When filtration is not complete in 25 min, discontinue the testand repeat using 5 6 0.3 g of sample. If filtration is still notcomplete in 25 min, report the result as filtration exceeds 25min.NOTE 3
30、It is expedient to weigh the beaker plus stirrer plus tempera-ture measurement device before and after transfer to avoid errors incurredby attempting to obtain a net weight.Any convenient means of heating thefuel sample to 1006 2C may be used, such as hot plate, water or oil bath,or an oven when equ
31、ipped with a suitable stirrer. Samples that overheatabove 105C must be discarded and not reused.NOTE 4For samples of high viscosity or high sediment, level filtrationwill be aided by small stage or even dropwise addition. It is preferable toavoid complete coverage of the filter medium with unfiltere
32、d oil sample.For samples of low filtration rate the pressure of 40 6 2 kPa should bemaintained for the 25-min period.9.5 Filter WashingWhen the filtration is complete and theupper filter medium appears dry, continue the steam andvacuum for a further 5 min. Discontinue the steam supply andcool the ap
33、paratus by passing tap water through the coils. Washthe filtration unit carefully with two portions of 25 6 1mLofthe wash solvent from a syringe or graduated wash bottle witha fine nozzle, taking care to remove any adhered sample fromthe wall of the upper part of the apparatus. Carefully removethe t
34、op portion of the filtration unit and wash the rim of thefilter with a further 10 6 0.5 mL of the wash solvent in asimilar manner. Finally wash the whole of the filter mediumarea with 10 6 0.5 mL of n-heptane.NOTE 5If the sample filters very rapidly, the vacuum should bereleased before the first sol
35、vent washing, to ensure complete coverage ofthe filter medium area by solvent. The vacuum should then be gentlyreapplied for the subsequent operations.9.6 Apparatus DisassemblyAfter the filter medium ap-pears dry, discontinue the vacuum supply. Using the forceps,carefully remove each filter medium s
36、eparately and transferthem to the oven at 110C. Dry for 20 min and quickly transferthem to the cooling vessel (6.14). Allow them to cool to roomtemperature for 20 min and reweigh them to the nearest 0.0001g.10. Calculation10.1 Calculate the mass percentage of total sediment foreach test specimen usi
37、ng Eq 1. For each test specimen with acalculated total sediment concentration 0.005 % m/m asdetermined by Eq 1, record the mass percentage of totalsediment to the nearest 0.01 % m/m. For each test specimenwith a total sediment concentration #0.005 % m/m, record theresult as 0.00 % m/m.S 5M52 M4! 2 M
38、32 M2!10 M1(1)where:S = total sediment, % m/m,M1= mass of sample, g,M2= mass of lower filter medium before filtration, mg,M3= mass of lower filter medium after filtration, mg,M4= mass of upper filter medium before filtration, mg, andM5= mass of upper filter medium after filtration, mg.11. Report11.1
39、 Report the total sediment by hot filtration as theaverage of duplicate determinations, to the nearest 0.01 %m/m. If the average of the duplicate determinations is 0.01 %m/m, report it as “0.01 % m/m.” If a 5-g sample has beenused, report the results as total sediment (5 g) by hot filtration.If filt
40、ration is not complete within the specified 25 min, reportthe results as filtration time exceeds 25 min.11.2 Test ReportThe test report shall contain at least thefollowing information:11.2.1 The type and identification of the product tested,11.2.2 A reference to this test method,11.2.3 The result of
41、 the test (see 11.1),11.2.4 Any deviation, by agreement or otherwise, from thestandard procedures specified (see 11.1), and11.2.5 The date of the test.D487009312. Precision and Bias412.1 PrecisionThe precision of this test method as deter-mined by the statistical examination of interlaboratory testr
42、esults is as follows. The results ranged from 0.01 to 0.40 %m/m for distillate fuel oils containing residual components andfrom 0.01 to 0.50 % m/m for residual fuel oils.12.1.1 RepeatabilityThe difference between successivetest results, expressed as the average of duplicate determina-tions, obtained
43、 by the same operator with the same apparatusunder constant operating conditions on identical test material,would, in the long run, in the normal and correct operation ofthe test method, exceed the following values only in one casein twenty:r 5 0.089 =x for residual fuels, and (2)r 5 0.048 =x for di
44、stillate fuels containingresidual components (3)where x = the average of the test results, % m/m.12.1.2 ReproducibilityThe difference between two testresults, expressed as the average of duplicate determinationsindependently obtained by different operators operating indifferent laboratories on nomin
45、ally identical test materialwould, in the long run, in the normal and correct operation ofthe test method, exceed the following values only one case intwenty:R 5 0.294=x for residual fuels, and (4)R 5 0.174 =x for distillate fuels containingresidual components (5)where x = the average of the test re
46、sults, % m/m.12.2 BiasSince there is no accepted reference materialsuitable for determining the bias for the procedure in this testmethod, bias cannot be determined.13. Keywords13.1 ageing; fuel oils; hot filtration; residual fuel; sediment;storage stability; total sedimentANNEX(Mandatory Informatio
47、n)A1. HAZARD STATEMENTSA1.1 n-HeptaneKeep away from heat, sparks, and open flame.Keep container closed.Use with adequate ventilation.Avoid prolonged breathing of vapor or spray mist.Avoid prolonged or repeated skin contact.A1.2 TolueneKeep away from heat, sparks, and open flame.Keep container closed
48、.Use with adequate ventilation.Avoid breathing of vapor or spray mist.Avoid prolonged or repeated skin contact.APPENDIX(Nonmandatory Information)X1. PREDICTION OF TOTAL SEDIMENT IN RESIDUAL FUEL OILS(STANDARD PROCEDURES FOR AGEING)X1.1 ScopeX1.1.1 This test method describes two procedures for evalu-
49、ating the sediment forming tendency of residual fuel oilsduring storage.NOTE X1.1Experience has shown that this test method can beapplicable to other fuel oils as well, but precision is unknown andadditional testing is required to determine that precision.X1.1.2 Procedure A covers thermal ageing.X1.1.3 Procedure B covers chemical ageing.X1.2 TerminologyX1.2.1 Definitions of Terms Specific to This Standard:X1.2.1.1 accelerated total sedimentthe total sedimentformed in a fuel when it is diluted with hexadecane andstressed at an elevated temperatur
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