1、Designation: D 4870 07aDesignation: 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
2、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.1. Scope*1.1 This test method covers the determination of totalsediment up to 0.40 % m/m for di
3、stillate 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 org
4、anic 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
5、standard 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 sta
6、tements, 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.
7、1 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.
8、Summary 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 s
9、ediment 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 Apparat
10、us, 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
11、Oven, 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 squ
12、at form with lipor conical.6.6 Weighing Bottles, with ground glass stoppers, num-bered, 80 mm diameter by 40 mm.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 specifiedva
13、cuum.6.11 Filter Medium, Whatman glass fiber filter medium,Grade GF/A, 47 mm diameter.1This test method is under 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 edit
14、ion approved July 1, 2007. Published July 2007. Originally approvedin 1988. Last previous edition approved in 2007 as D 487007.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information
15、, refer to the standards Document Summary page onthe ASTM website.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.6.12 High Speed Mixer, any convenient type, minimumsp
16、eed 400 rpm.6.13 Desiccator.6.14 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, sp
17、ade-ended.7. Reagents and Materials7.1 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 specificati
18、ons are available.3Other grades 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 Tolue
19、ne, at least reagent grade purity. (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 4177.9. Procedure9.1 Sample PreparationMix the whole sampl
20、e, 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 rod3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the Americ
21、an Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.FIG. 1 Detail of Filtration CellFIG. 2 Arrangement of Filtration ApparatusD 4870 07a2di
22、pped to the bottom of the container 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 equival
23、entto 150 to 250 cSt in the case 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 paper,separately, rapidly to a numbered weighing bottle and allow tocool in the cooling vessel
24、to room temperature (5 to 10 min).Weigh each weighing bottle plus filter medium to the nearest0.0001 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 convenienc
25、e, it is useful to have a number of weighingbottles dedicated to the procedure, the lightest of which is chosen as thetare. All weighing bottles should be stored in a desiccator in the vicinityof the balance. Do not place these weighing bottles in the oven since theirweights are in equilibrium with
26、the desiccant.9.3 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
27、 andinstall a new 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, placing the one from the lower numberedweighing bottle on the bottom. Apply slight
28、vacuum to aid incentering the filter media, and place the top portion of thefiltration apparatus carefully on to the media before clamping.Shut off the 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
29、approxi-mately 11 g of the fuel sample prepared as described in 9.1 andweigh to the nearest 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)tot
30、hecenter of the filter medium, taking care that no sample touchesthe walls during transfer (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 filtratio
31、n is still notcomplete in 25 min, report the result as filtration exceeds 25min.NOTE 3It 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 s
32、ample to 1006 2C may be used, such as hot plate, water or oil bath,or an oven when equipped 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 ad
33、dition. It is preferable toavoid complete coverage of the filter medium with unfiltered 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, continu
34、e the steam andvacuum for a further 5 min. Discontinue the steam supply andcool the apparatus 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
35、 adhered sample fromthe wall of the upper part of the apparatus. Carefully removethe top 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
36、5If the sample filters very rapidly, the vacuum should bereleased before the first solvent 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,
37、discontinue the vacuum supply. Using the forceps,carefully remove each filter medium separately and transferthem to the oven at 110C. Dry for 20 min and quickly transferthem to the same numbered weighing bottles as used in 9.2.Allow them to cool in the cooling vessel (6.14) to roomtemperature (5 to
38、10 min) and reweigh them to the nearest0.0001 g.10. Calculation10.1 Calculate M2, M3, M4, and M5by subtracting themasses recorded in 9.2 and 9.6 with the mass of the corre-sponding weighing bottle. For each test specimen with acalculated total sediment concentration 0.005 % m/m asdetermined by Eq 1,
39、 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 M32 M2!10 M1(1)where:S = total sediment, % m/m,M1= mass of sample, g,M2= mass of lower filter medium before filt
40、ration, 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 Report the total sediment by hot filtration as theaverage of duplicate determinations, to the nearest 0.01 %m/
41、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 filtration is not complete within the specified 25 min, reportthe results as filtration time exceeds 25 min.11.2 Te
42、st 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 the test (see 11.1),D 4870 07a311.2.4 Any deviation, by agreement or otherwise, from thestandard procedures sp
43、ecified (see 11.1), and11.2.5 The date of the test.12. Precision and Bias412.1 PrecisionThe precision of this test method as deter-mined by the statistical examination of interlaboratory testresults is as follows. The results ranged from 0.01 to 0.40 %m/m for distillate fuel oils containing residual
44、 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 by the same operator with the same apparatusunder constant operating conditions on identical test material,
45、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 distillate fuels containingresidual components (3)where x = the average of the test results, % m/m.12.1.2 Repr
46、oducibilityThe difference between two testresults, expressed as the average of duplicate determinationsindependently obtained by different operators operating indifferent laboratories on nominally identical test materialwould, in the long run, in the normal and correct operation ofthe test method, e
47、xceed 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 results, % m/m.12.2 BiasSince there is no accepted reference materialsuitable for determining the bias for the
48、 procedure in this testmethod, bias cannot be determined.13. Keywords13.1 ageing; fuel oils; hot filtration; residual fuel; sediment;storage stability; total sedimentANNEX(Mandatory Information)A1. HAZARD STATEMENTSA1.1 n-HeptaneKeep away from heat, sparks, and open flame.Keep container closed.Use w
49、ith 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.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-ating the sediment forming tendency of residual fuel oilsdur
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