1、Designation: D4870 09 (Reapproved 2014)D4870 18Designation: 375/99Standard Test Method forDetermination of Total Sediment in Residual Fuels1This standard is issued under the fixed designation D4870; the number immediately following the designation indicates the year oforiginal adoption or, in the ca
2、se 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 Scope*1.1 This test method covers the determination of total sediment up to 0.40 % 0.40 % m/m
3、 for distillate fuel oils containingresidual components and to 0.50 % m/m in residual fuel oils having a maximum viscosity of 55 cSt (mm2/s) at 100C.100 C.Some fuels can exceed the maximum filtration time specified in this test method due to factors other than the presence of significantquantities o
4、f insoluble organic or inorganic material. This test method can be used for the assessment of total sediment afterregimes of fuel pretreatment designed to accelerate the aging process.1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this
5、 standard.1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine theapplicability of regulatory lim
6、itations prior to use. For specific warning statements, see 7.2, 7.3, Annex A1, and X1.6.1.1.4 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards
7、, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D4057 Practice for Manual Sampling of Petroleum and Petroleum ProductsD4177 Practice for Automatic Sampling of Petroleum and Petroleum ProductsE1
8、Specification for ASTM Liquid-in-Glass Thermometers3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 total sedimentsediment, nthe sum of the insoluble organic and inorganic material that is separated from the bulk ofthe residual fuel oil by filtration through a Whatman GF/A filt
9、er medium, and that is also insoluble in a predominantly paraffinicsolvent.4. Summary of Test Method4.1 Aweighed quantity (10 g) (10 g) of the oil sample is filtered through the prescribed apparatus at 100C.100 C.After solventwashing and drying the total sediment on the filter medium is weighed. The
10、 test is to be carried out in duplicate.5. Significance and Use5.1 Appreciable amounts of sediment in a residual fuel oil can cause fouling of facilities for handling, and give problems inburner mechanisms. Sediment can accumulate in storage tanks, on filter screens, or on burner parts, resulting in
11、 obstruction of theflow of oil from the tank to the burner.1 This test method is under the jurisdiction ofASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of SubcommitteeD02.14 on Stability Stability, Cleanliness and CleanlinessCompatibility of
12、Liquid Fuels.Current edition approved Dec. 1, 2014April 1, 2018. Published February 2015May 2018. Originally approved in 1988. Last previous edition approved in 20092014 asD4870 09.D4870 09 (2014). DOI: 10.1520/D4870-09R14.10.1520/D4870-18.2 For referencedASTM standards, visit theASTM website, www.a
13、stm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what
14、changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the o
15、fficial document.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States16. Apparatus6.1 Filtration Apparatus, constructed of brass, with copper steam coils attached, suitably s
16、upported above a vacuum flaskappropriately protected against the effects of implosion. See Figs. 1 and 2.6.2 Temperature Measuring Device , Device, capable of measuring the temperature in the range from 9595 C to 105C105 Cwith an accuracy of 0.5C.0.5 C.6.3 Oven, electric, capable of maintaining a te
17、mperature of 110110 C 6 1C.1 C. The oven should be capable of safelyevaporating the solvent without risk of fire.6.4 Stirring Rod, glass or polytetrafluoroethylene (PTFE) approximately 150 mm 150 mm in length and 3 mm 3 mm indiameter.6.5 Beaker, glass, 30 mL 30 mL capacity, either squat form with li
18、p or conical.6.6 Small Dishes, such as watch glasses or Petri dishes.6.7 Hotplate, electric.6.8 Steam Generator, to provide steam at 100100 C 6 1C.1 C.6.9 Vacuum Source, capable of providing the specified vacuum.6.10 Vacuum Gauge, capable of measuring the specified vacuum.6.11 Filter Medium, Whatman
19、 glass fiber filter medium, Grade GF/A, 47 mm 47 mm diameter.6.12 High Speed Mixer, any convenient type, minimum speed 400 400 rrpm.min.6.13 Desiccator.6.14 Cooling Vessel, a desiccator or other type of tightly covered vessel for cooling the filter media before weighing. The useof a drying agent is
20、not recommended.6.15 Syringe or Graduated Wash Bottle , Bottle, minimum capacity 25 mL, 25 mL, graduated in 0.5 mL 0.5 mL increments.FIG. 1 Detail of Filtration CellD4870 1826.16 Forceps, spade-ended.7. Reagents and Materials7.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. U
21、nless otherwise indicated, it is intended that allreagents shall conform to the specifications of the committee on Analytical Reagents of the American Chemical Society, wheresuch specifications are available.3 Other grades may be used, provided it is first ascertained that the reagent is of sufficie
22、ntly highpurity to permit its use without lessening the accuracy 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 purity. (WarningFlammable, vapor harmful. See A1.2. )7.4 Wash Solvent, consisti
23、ng of 85 volume % 85 % by volume n-heptane (7.2) and 15 volume % toluene15 % byvolume toluene (see 7.3).8. Sampling8.1 Sample in accordance with Practice D4057 or Practice D4177.9. Procedure9.1 Sample PreparationMix the whole sample, as received, thoroughly using a high speed mixer when practicable,
24、 for 30 s.30 s. In all cases a sample taken on a glass or PTFE rod dipped to the bottom of the container must show a homogeneousappearance. For fuels with a high wax content (high pour point), or of very high viscosity, the sample must be heated beforestirring. The temperature must be either 15C15 C
25、 above the pour point in the case of low viscosity fuels, or that equivalent to150150 cSt to 250 cSt 250 cSt in the case of high viscosity fuels. In no case should the temperature exceed 80C.80 C.9.2 Filter PreparationFor each test, dry two filter media for 20 min 20 min in the oven at 110C.110 C. T
26、ransfer each filtermedium, separately, rapidly to a cooling vessel and allow to cool to room temperature for 20 min. 20 min. Weigh each filtermedium to the nearest 0.0001 g. 0.0001 g.NOTE 1The Whatman GF/Afilter media are fragile and are to be handled with care. Before use, check each medium for con
27、sistency, and the possiblepresence of small defects (holes).NOTE 2For convenience, place the filters on numbered small dishes (6.6) during drying and cooling.9.3 Apparatus AssemblyBefore use, check that the filter support screen is clean. If necessary, the screen must be cleaned byboiling in a high
28、boiling point aromatic solvent. When more than 2 % of the sinter area remains blocked by particulate matter aftersuch cleaning, discard the screen and install a new one.9.3.1 The filtration unit must be clean and dry before assembly. Stack the two previously dried and weighed filter media on topof t
29、he sinter support with the mesh imprint side down, using forceps. Apply slight vacuum to aid in centering the filter media, andplace the top portion of the filtration apparatus carefully on to the media before clamping. Shut off the vacuum and pass steam at100100 C 6 1C1 C through the heating/coolin
30、g coils for 10 min 10 min prior to sample addition.9.4 Sample AdditionInto a 30 mL 30 mL beaker, pour approximately 11 g 11 g of the fuel sample prepared as described in9.1 and weigh to the nearest 0.01 g. 0.01 g. Connect the vacuum source and apply vacuum to an absolute pressure of 4040 kPa6 2 kPa
31、minimum (61.3 kPa 2 kPa minimum (61.3 kPa vacuum). Heat the contents of the beaker to 100100 C 6 2C.2 C. Thentransfer the contents at 100100 C 6 2C2 C (Note 3) to the center of the filter medium, taking care that no sample touches the3 Reagent Chemicals, American Chemical Society Specifications, Ame
32、rican Chemical Society, Washington, DC. For Suggestions on the testing of reagents not listed bythe American Chemical Society, see Annual Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (
33、USPC), Rockville, MD.FIG. 2 Arrangement of Filtration ApparatusD4870 183walls during transfer (Note 4). Reweigh the beaker to the nearest 0.01 g. 0.01 g. The quantity transferred should be 106 0.5 g.10 g6 0.5 g. When filtration is not complete in 25 min, 25 min, discontinue the test and repeat using
34、 55 g 6 0.3 g 0.3 g of sample.If filtration is still not complete in 25 min, 25 min, report the result as filtration exceeds 25 min.25 min.NOTE 3It is expedient to weigh the beaker plus stirrer plus temperature measurement device before and after transfer to avoid errors incurred byattempting to obt
35、ain a net weight. Any convenient means of heating the fuel sample to 1006 2C 100 C 6 2 C may be used, such as hot plate, wateror oil bath, or an oven when equipped with a suitable stirrer. Samples that overheat above 105C105 C must be discarded and not reused.NOTE 4For samples of high viscosity or h
36、igh sediment, level filtration will be aided by small stage or even dropwise addition. It is preferable to avoidcomplete coverage of the filter medium with unfiltered oil sample. For samples of low filtration rate the pressure of 4040 kPa 6 2 kPa 2 kPa should bemaintained for the 25-min25 min period
37、.9.5 Filter WashingWhen the filtration is complete and the upper filter medium appears dry, continue the steam and vacuumfor a further 5 min. Discontinue the steam supply and cool the apparatus by passing tap water through the coils. Wash the filtrationunit carefully with two portions of 2525 mL 6 1
38、 mL 1 mL of the wash solvent from a syringe or graduated wash bottle with afine nozzle, taking care to remove any adhered sample from the wall of the upper part of the apparatus. Carefully remove the topportion of the filtration unit and wash the rim of the filter with a further 1010 mL6 0.5 mL0.5 m
39、Lof the wash solvent in a similarmanner. Finally wash the whole of the filter medium area with 1010 mL 6 0.5 mL 0.5 mL of n-heptane.NOTE 5If the sample filters very rapidly, the vacuum should be released before the first solvent washing, to ensure complete coverage of the filtermedium area by solven
40、t. The vacuum should then be gently reapplied for the subsequent operations.9.6 Apparatus DisassemblyAfter the filter medium appears dry, discontinue the vacuum supply. Using the forceps, carefullyremove each filter medium separately and transfer them to the oven at 110C.110 C. Dry for 20 min 20 min
41、 and quickly transferthem to the cooling vessel (6.14). Allow them to cool to room temperature for 20 min 20 min and reweigh them to the nearest0.0001 g.0.0001 g.10. Calculation10.1 Calculate the mass percentage of total sediment for each test specimen using Eq 1. For each test specimen with a calcu
42、latedtotal sediment concentration 0.005 % 0.005 % m/m as determined by Eq 1, record the mass percentage of total sediment to thenearest 0.01 % m/m.mm. For each test specimen with a total sediment concentration 0.005 %0.005 % m m/m, m, record theresult as 0.00 % m/m.S 5M 52M4!2M 32M2!10 M1 (1)where:S
43、 = total sediment, % m/m,S = total sediment, percent 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, m
44、g.11. Report11.1 Report the total sediment by hot filtration as the average of duplicate determinations, to the nearest 0.01 % mm. If theaverage of the duplicate determinations is 0.01 %0.01 % m m/m, m, report it as “0.01 % “0.01 % m/m.” If a 5-g5 g samplehas been used, report the results as total s
45、ediment (5 g) (5 g) by hot filtration. If filtration is not complete within the specified 25min, 25 min, report the results as filtration time exceeds 25 min.25 min.11.2 Test ReportThe test report shall contain at least the following information:11.2.1 The type and identification of the product test
46、ed,11.2.2 A reference to this test method,11.2.3 The result of the test (see 11.1),11.2.4 Any deviation, by agreement or otherwise, from the standard procedures specified (see 11.1), and11.2.5 The date of the test.12. Precision and Bias412.1 PrecisionThe precision of this test method as determined b
47、y the statistical examination of interlaboratory test results isas follows. The results ranged from 0.010.01 % to 0.40 % m/m for distillate fuel oils containing residual components and from0.010.01 % to 0.50 % m/m0.50 % mm for residual fuel oils.4 Supporting data have been filed at ASTM Internationa
48、l Headquarters and may be obtained by requesting Research Report RR:D02-1238. Contact ASTM CustomerService at serviceastm.org.D4870 18412.1.1 RepeatabilityThe difference between successive test results, expressed as the average of duplicate determinations,obtained by the same operator with the same
49、apparatus under constant operating conditions on identical test material, would, inthe long run, in the normal and correct operation of the test method, exceed the following values only in one case in twenty:r 50.089=x for residual fuels,and (2)r 50.048=x for distillate fuels containing (3)residual componentswhere x = the average of the test results, % m/m.12.1.2 ReproducibilityThe difference between two test results, expressed as the average of duplicate determinationsindependently obtained by different ope
