1、Designation: D6217 11 (Reapproved 2016)Designation: 415/98Standard Test Method forParticulate Contamination in Middle Distillate Fuels byLaboratory Filtration1This standard is issued under the fixed designation D6217; the number immediately following the designation indicates the year oforiginal ado
2、ption 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.1. Scope1.1 This test method covers the determination of the mass ofparticulate con
3、tamination in a middle distillate fuel by filtra-tion. This test method is suitable for all No. 1 and No. 2 gradesin Specifications D396, D975, D2880 and D3699 and forgrades DMA and DMB in Specification D2069.1.2 This test method is not suitable for fuels whose flashpoint as determined by Test Metho
4、ds D56, D93 or D3828 isless than 38 C.NOTE 1Middle distillate fuels with flash points less than 38 C havebeen ignited by discharges of static electricity when the fuels have beenfiltered through inadequately bonded or grounded membrane filter sys-tems. See Test Methods D2276 and D5452 for means of d
5、eterminingparticulate contamination in Specification D1655 aviation turbine fuelsand other similar aviation fuels. See Guide D4865 for a more detaileddiscussion of static electricity formation and discharge.1.3 This test method has not been validated for testingbiodiesel, such as meeting Specificati
6、on D6751 or blends ofmiddle distillates and biodiesel, such as meeting SpecificationD7467, or both. Test Method D7321 has been determined to besuitable for testing B100 and all blends of middle distillatesand biodiesel.NOTE 2No. 1 and No. 2 grades in Specifications D396 or D975currently allow up to
7、5% biodiesel meeting Specification D6751. Samplescontaining biodiesel can result in partial dissolution or compromise of themembrane filters and give erroneous results.1.4 The precision of this test method is applicable toparticulate contaminant levels between 0 g m3to 25 g m3provided that 1 L sampl
8、es are used and the 1 L is filteredcompletely. Higher levels of particulate contaminant can bemeasured, but are subject to uncertain precision.1.5 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.6 This standard does not purpor
9、t 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.2. Referenced Documents2.1 ASTM Standards:2D56 T
10、est Method for Flash Point by Tag Closed Cup TesterD93 Test Methods for Flash Point by Pensky-MartensClosed Cup TesterD396 Specification for Fuel OilsD975 Specification for Diesel Fuel OilsD1193 Specification for Reagent WaterD1655 Specification for Aviation Turbine FuelsD2069 Specification for Mari
11、ne Fuels (Withdrawn 2003)3D2276 Test Method for Particulate Contaminant in AviationFuel by Line SamplingD2880 Specification for Gas Turbine Fuel OilsD3699 Specification for KerosineD3828 Test Methods for Flash Point by Small Scale ClosedCup TesterD4057 Practice for Manual Sampling of Petroleum andPe
12、troleum ProductsD4865 Guide for Generation and Dissipation of Static Elec-tricity in Petroleum Fuel SystemsD5452 Test Method for Particulate Contamination in Avia-tion Fuels by Laboratory FiltrationD6751 Specification for Biodiesel Fuel Blend Stock (B100)for Middle Distillate FuelsD7321 Test Method
13、for Particulate Contamination of Bio-diesel B100 Blend Stock Biodiesel Esters and BiodieselBlends by Laboratory FiltrationD7467 Specification for Diesel Fuel Oil, Biodiesel Blend(B6 to B20)1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubri
14、cants and is the direct responsibility ofSubcommittee D02.14 on Stability and Cleanliness of Liquid Fuels.Current edition approved Dec. 1, 2016. Published January 2017. Originallyapproved in 1998. Last previous edition approved in 2011 as D6217 11. DOI:10.1520/D6217-11R16.2For referenced ASTM standa
15、rds, 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.3The last approved version of this historical standard is referenced onwww.astm.org.Copy
16、right ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of Internati
17、onal Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.13. Terminology3.1 Definitions:3.1.1 bond, vto connect two parts of a system electricallyby means of a conductive wire to eliminate voltage differences.3.1.2 ground, vto conn
18、ect electrically with earth.3.1.3 membrane filter, na porous article of closely con-trolled pore size through which a liquid is passed to separatematter in suspension.3.2 Definitions of Terms Specific to This Standard:3.2.1 control membrane, nthe lower of the two stackedmembrane filters used in this
19、 test method.3.2.2 filtered flushing fluids, neither of two solvents,heptane or 2,2,4-trimethylpentane, filtered through a nominal0.45 m membrane filter.3.2.3 test membrane, nthe upper of the two stackedmembrane filters used in this test method.4. Summary of Test Method4.1 A measured volume of about
20、 1 L of fuel is vacuumfiltered through one or more sets of 0.8 m membranes. Eachmembrane set consists of a tared nylon test membrane and atared nylon control membrane. When the level of particulatecontamination is low, a single set will usually suffice; when thecontamination is high or of a nature t
21、hat induces slow filtrationrates, two or more sets may be required to complete filtrationin a reasonable time.4.2 After the filtration has been completed, the membranesare washed with solvent, dried, and weighed. The particulatecontamination level is determined from the increase in themass of the te
22、st membranes relative to the control membranes,and is reported in units of g/m3or its equivalent mg/L.5. Significance and Use5.1 This is the first ASTM standard test method for assess-ing the mass quantity of particulates in middle distillate fuels.Test Method D5452 and its predecessor Test Method D
23、2276were developed for aviation fuels and used 1 gal or 5 L of fuelsample. Using 1 gal of a middle distillate fuel, which cancontain greater particulate levels, often required excessive timeto complete the filtration. This test method used about a quarterof the volume used in the aviation fuel metho
24、ds.5.2 The mass of particulates present in a fuel is a significantfactor, along with the size and nature of the individualparticles, in the rapidity with which fuel system filters andother small orifices in fuel systems can become plugged. Thistest method provides a means of assessing the mass ofpar
25、ticulates present in a fuel sample.5.3 The test method can be used in specifications andpurchase documents as a means of controlling particulatecontamination levels in the fuels purchased. Maximum particu-late levels are specified in several military fuel specifications.6. Apparatus6.1 Filtration Sy
26、stemArrange the following componentsas shown in Fig. 1.6.1.1 Funnel and Funnel Base, with filter support for a47 mm diameter membrane, and locking ring or spring actionclip.6.1.2 Ground/Bond Wire, 0.912 mm to 2.59 mm (No. 10through No. 19) bare stranded flexible, stainless steel or copperinstalled i
27、n the flasks and grounded as shown in Fig. 1.NOTE 3The electrical bonding apparatus described in Test MethodD5452 or other suitable means of electrical grounding which ensure safeoperation of the filtration apparatus and flask can be used. If the filtrate isto be subsequently tested for stability it
28、 is advisable not to use copper ascopper ions catalyze gum formation during the stability test.6.1.3 Receiving Flask, 1.5 L or larger borosilicate glassvacuum filter flask, which the filtration apparatus fits into,equipped with a sidearm to connect to the safety flask.6.1.4 Safety Flask, 1.5 L or la
29、rger borosilicate glass vacuumfilter flask equipped with a sidearm to connect the vacuumsystem. A fuel and solvent resistance rubber hose throughwhich the grounding wire passes shall connect the sidearm ofthe receiving flask to the tube passing through the rubberstopper in the top of the safety flas
30、k.6.1.5 Vacuum System, either a water aspirated or a mechani-cal vacuum pump may be used if capable of producing avacuum of 1 kPa to 100 kPa below atmospheric pressure whenmeasured at the receiving flask.FIG. 1 Schematic of Filtration SystemD6217 11 (2016)26.2 Other Apparatus:6.2.1 Air Ionizer, for
31、the balance case. Air ionizers shall bereplaced within one year of manufacture.NOTE 4When using a solid-pan balance, the air ionizer may beomitted provided that, when weighing a membrane filter, it is placed onthe pan so that no part protrudes over the edge of the pan.6.2.2 Analytical Balance, singl
32、e- or double-pan, the preci-sion standard deviation of which must be 0.07 mg or less.6.2.3 Crucible Tongs, for handling clean sample containerlids.6.2.4 Drying Oven, naturally convected (without fan-assisted air circulation), controlling to 90 C 6 5 C.6.2.5 Flushing Fluid Dispenser, an apparatus for
33、 dispensingflushing fluid through a nominal 0.45 m membrane filter.4NOTE 5An apparatus such as pictured in Fig. 2 has been foundsuitable for this task. A standard laboratory wash bottle can also be usedprovided the flushing fluid is pre-filtered through a 0.45 m pore sizemembrane filter and precauti
34、ons are taken to maintain appropriatecleanliness of the interior of the wash bottle6.2.6 Forceps, approximately 12 cm long, flat-bladed, withnon-serrated, non-pointed tips.6.2.7 Graduated Cylinders, to contain at least 1 L of fluidand marked at 10 mL intervals. 100 mL graduated cylindersmay be requi
35、red for samples which filter slowly.6.2.8 Petri Dishes, approximately 12.5 cm in diameter, withremovable glass supports for membrane filters.NOTE 6Small watch glasses, approximately 5 cm to 7 cm in diameter,have also been found suitable to support the membrane filters.7. Reagents and Materials7.1 Pu
36、rity 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.5Other grades may be4Su
37、pporting data (a membrane approval procedure) have been filed at ASTMInternational Headquarters and may be obtained by requesting Research ReportRR:D02-1012. Contact ASTM Customer Service at serviceastm.org.5Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washi
38、ngton, 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.FIG. 2 App
39、aratus for Filtering and Dispensing Flushing FluidD6217 11 (2016)3used, provided it is first ascertained that the reagent is ofsufficient purity to permit its use without lessening the accu-racy of the determination.7.2 Purity of Water Unless otherwise indicated, referencesto water mean reagent wate
40、r as defined by Type III ofSpecification D1193.7.3 Flushing Fluids:7.3.1 Heptane, (WarningFlammable.)7.3.2 2,2,4-trimethylpentane (isoctane), (WarningFlammable.)7.4 Propan-2-ol (2-propanol; isopropyl alcohol),(WarningFlammable.)7.5 Liquid or Powder Detergent, water-soluble, for cleaningglassware.7.6
41、 Nylon Test Membrane Filters, plain, 47 mm diameter,nominal pore size 0.8 m.7.7 Nylon Control Membrane Filters (see Note 7), 47 mmdiameter, nominal pore size 0.8 m.NOTE 7Membrane filters with a grid imprinted on their surface, maybe used as control membrane filters for identification.7.8 Protective
42、Cover, polyethylene film or clean aluminumfoil.8. Preparation of Apparatus and Sample Containers8.1 Clean all components of the filtration apparatus, samplecontainers, their caps and petri dishes as described in 8.1.1 8.1.7.8.1.1 Remove any labels, tags, and so forth.8.1.2 Wash with warm tap water c
43、ontaining detergent.8.1.3 Rinse thoroughly with warm tap water.8.1.4 Rinse thoroughly with reagent water. Container capsshould be handled only externally with clean laboratorycrucible tongs during this and subsequent washings.8.1.5 Rinse thoroughly with propan-2-ol that has beenfiltered through a 0.
44、45 m membrane filter.8.1.6 Rinse thoroughly with filtered flushing fluid and dry.8.1.7 Keep a clean protective cover (the cover may be rinsedwith filtered flushing fluid), over the top of the samplecontainer until the cap is installed. Similarly protect the funnelopening of the assembled filtration
45、apparatus with a cleanprotective cover until ready for use.9. Sampling9.1 The sample container shall be 1 L (60.15 L) in volumeand have a screw on cap. Glass containers are preferred tofacilitate a visual inspection of the contents and the containerbefore and after filling. Glass containers also all
46、ow for visualinspection of the container, after the sample is emptied, toconfirm complete rinsing of the container. Epoxy lined samplecans, polytetrafluoroethylene (PTFE) bottles, and high densitylinear polyethylene bottles have also been found suitable assample containers but are less desirable sin
47、ce visual inspectionof the interior of the container is more difficult. (WarningItis important to note that the entire contents of the samplecontainer are filtered during the conduct of this test method.This includes not only all of the fuel but also all rinsings of theinterior of the container with
48、 flushing fluid. Because of this,take care to protect the sample from any external contamina-tion.)9.2 All containers and their caps, sampling lines, and otherequipment used in obtaining the sample for analysis shall bethoroughly cleaned as described in Section 8. When it is notpractical to clean th
49、e sample containers in this manner, thecontainers shall be rinsed three times with the fuel to besampled. When it is not practical to clean the sampling lines,rinse them thoroughly with the fuel to be sampled.9.3 Precautions to avoid sample contamination shall includeselection of an appropriate sampling point. Samples shouldpreferentially be obtained dynamically from a sampling loop ina distribution line, or from the flushing line of a field samplingkit. Ensure that the line to be sampled is flushed with fuelbefore taking the sample.9.3.1 Where i
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