1、Designation: D 6217 98 (Reapproved 2003)e1Designation: 415/98An American National StandardStandard Test Method forParticulate Contamination in Middle Distillate Fuels byLaboratory Filtration1This standard is issued under the fixed designation D 6217; the number immediately following the designation
2、indicates the year oforiginal adoption or, in 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.e1NOTEWarning notes were editorially moved into t
3、he standard text in August 2003.1. Scope1.1 This test method covers the determination of the mass ofparticulate contamination in a middle distillate fuel by filtra-tion. This test method is suitable for all No. 1 and No. 2 gradesin Specifications D 396, D 975, D 2880 and D 3699 and forgrades DMA and
4、 DMB in Specification D 2069.1.2 This test method is not suitable for fuels whose flashpoint as determined by Test Methods D 56, D 93 or D 3828 isless than 38C.NOTE 1Middle distillate fuels with flash points less than 38C havebeen ignited by discharges of static electricity when the fuels have beenf
5、iltered through inadequately bonded or grounded membrane filter sys-tems. See Test Methods D 2276 and D 5452 for means of determiningparticulate contamination in Specification D 1655 aviation turbine fuelsand other similar aviation fuels. See Guide D 4865 for a more detaileddiscussion of static elec
6、tricity formation and discharge.1.3 The precision of this test method is applicable toparticulate contaminant levels between 0 to 25 g/m3providedthat 1 L samples are used and the 1 L is filtered completely.Higher levels of particulate contaminant can be measured, butare subject to uncertain precisio
7、n.1.4 The values stated in SI units are to be regarded as thestandard.1.5 This 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
8、 applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:D 56 Test Method for Flash Point by Tag Closed Tester2D 93 Test Methods for Flash Point by Pensky-MartensClosed Cup Tester2D 396 Specification for Fuel Oils2D 975 Specification for Diesel Fuel Oils2D 119
9、3 Specification for Reagent Water3D 1655 Specification for Aviation Turbine Fuels2D 2069 Specification for Marine Fuels2D 2276 Test Method for Particulate Contaminant in Avia-tion Fuel by Line Sampling2D 2880 Specification for Gas Turbine Fuel Oils2D 3699 Specification for Kerosine4D 3828 Test Metho
10、ds for Flash Point by Small Scale ClosedTester4D 4057 Practice for Manual Sampling of Petroleum andPetroleum Products4D 4865 Guide for Generation and Dissipation of StaticElectricity in Petroleum Fuel Systems4D 5452 Test Method for Particulate Contamination in Avia-tion Fuels by Laboratory Filtratio
11、n53. 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 connect electrically with earth.3.1.3 membrane filter, na thin medium of closely con-trolled pore size through which a liquid is
12、passed and on whichparticulate matter in suspension is retained.3.2 Definitions of Terms Specific to This Standard:3.2.1 control membrane, nthe lower of the two stackedmembrane filters used in this test method.3.2.2 filtered flushing fluids, neither of two solvents,heptane or 2,2,4-trimethylpentane,
13、 filtered through a nominal0.45 m membrane filter.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 edition approved June 10, 2003. Publishe
14、d August 2003. Originallyapproved in 1998. Last previous edition approved in 1998 as D 621798.2Annual Book of ASTM Standards, Vol 05.01.3Annual Book of ASTM Standards, Vol 11.01.4Annual Book of ASTM Standards, Vol 05.02.5Annual Book of ASTM Standards, Vol 05.03.1Copyright ASTM International, 100 Bar
15、r Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.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 1 L of fuel is vacuumfiltered through one or more sets of 0.8 m membranes.
16、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 that induces slow filtrationrates, two or more sets may be required to comple
17、te 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 test membranes relative to the control membranes,and is reported in units of g
18、/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 D 5452 and its predecessor Test Method D 2276were developed for aviation fuels and used 1 gal or 5 L of fuelsample.
19、 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 methods.5.2 The mass of particulates present in a fuel is a significantfactor,
20、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 ofparticulates present in a fuel sample.5.3 The test method can be used in spec
21、ifications 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 SystemArrange the following componentsas shown in Fig. 1.6.1.1 Funnel and Fu
22、nnel Base, with filter support for a 47mm diameter membrane, and locking ring or spring action clip.6.1.2 Ground/Bond Wire, 0.912-2.59 mm (No. 10 throughNo. 19) bare stranded flexible, stainless steel or copperinstalled in the flasks and grounded as shown in Fig. 1.NOTE 2The electrical bonding appar
23、atus described in Test Method D5452 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 is advisable not to use copper ascopper ions catalyze gum formation during th
24、e 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 larger borosilicate glass vacuumfilter flask equipped with a sidearm to connect
25、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 flask.6.1.5 Vacuum System, either a water aspirated or a mechani-cal vacuum pump m
26、ay be used if capable of producing avacuum of 1 to 100 kPa below atmospheric pressure whenmeasured at the receiving flask.6.2 Other Apparatus:6.2.1 Air Ionizer, for the balance case. Air ionizers shall bereplaced within one year of manufacture.NOTE 3When using a solid-pan balance, the air ionizer ma
27、y 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, single- 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 co
28、ntainerlids.6.2.4 Drying Oven, naturally convected (without fan-assisted air circulation), controlling to 90 6 5C.6.2.5 Flushing Fluid Dispenser, an apparatus for dispensingflushing fluid through a nominal 0.45 m membrane filter.6NOTE 4An apparatus such as pictured in Fig. 2 has been foundsuitable f
29、or this task. A standard laboratory wash bottle can also be used6Supporting data (a membrane approval procedure) have been filed at ASTMInternational Headquarters and may be obtained by requesting Research Report RR:D02-1012.FIG. 1 Schematic of Filtration SystemD 6217 98 (2003)e12provided the flushi
30、ng fluid is pre-filtered through a 0.45-m pore sizemembrane filter and precautions 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
31、L of fluidand marked at 10 mL intervals. 100 mL graduated cylindersmay be required for samples which filter slowly.6.2.8 Petri Dishes, approximately 12.5 cm in diameter, withremovable glass supports for membrane filters.NOTE 5Small watch glasses, approximately 5 to 7 cm in diameter,have also been fo
32、und suitable to support the membrane filters.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 Chem
33、ical Society,where such specifications are available.7Other grades may beused, 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, refer-ences to water mean rea
34、gent water as defined by Type III ofSpecification D 1193.7.3 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.)7Reagent Chemicals, American Chemical Society Specifications, Am
35、ericanChemical Society, 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. (U
36、SPC), Rockville,MD.FIG. 2 Apparatus for Filtering and Dispensing Flushing FluidD 6217 98 (2003)e137.5 Liquid or Powder Detergent, water-soluble, for cleaningglassware.7.6 Nylon Test Membrane Filters, plain, 47-mm diameter,nominal pore size 0.8-m.7.7 Nylon Control Membrane Filters (see Note 6), 47-mm
37、diameter, nominal pore size 0.8-m.NOTE 6Membrane filters with a grid imprinted on their surface, maybe used as control membrane filters for identification.7.8 Protective Cover, polyethylene film or clean aluminumfoil.8. Preparation of Apparatus and Sample Containers8.1 Clean all components of the fi
38、ltration 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 containing detergent.8.1.3 Rinse thoroughly with warm tap water.8.1.4 Rinse thoroughly with reagent water. Container capsshould be
39、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 0.45 m membrane filter.8.1.6 Rinse thoroughly with filtered flushing fluid and dry.8.1.7 Keep a clean protective cover (the cover ma
40、y be rinsedwith filtered flushing fluid), over the top of the samplecontainer until the cap is installed. Similarly protect the funnelopening of the assembled filtration apparatus with a cleanprotective cover until ready for use.9. Sampling9.1 The sample container shall be 1 L (60.15 L) in volumeand
41、 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 allow for visualinspection of the container, after the sample is emptied, toconfirm complete rinsing of the container. Epoxy lined sa
42、mplecans, polytetrafluoroethylene (PTFE) bottles, and high densitylinear polyethylene bottles have also been found suitable assample containers but are less desirable since visual inspectionof the interior of the container is more difficult. (WarningItis important to note that the entire contents of
43、 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 flushing fluid. Because of this,take care to protect the sample from any external contamina-tion.)9.2 All containers and their ca
44、ps, 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 the sample containers in this manner, thecontainers shall be rinsed three times with the fuel to besampled. When it is not practical
45、 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
46、line of a field samplingkit. Ensure that the line to be sampled is flushed with fuelbefore taking the sample.9.3.1 Where it is desirable or only possible to obtainsamples from static storage, follow the procedures given inPractice D 4057 or equivalent, taking precautions for cleanli-ness of all equi
47、pment used. Ensure that the sample has notpassed through intermediate containers prior to placement inthe prepared container. (WarningSamples obtained fromstatic storage may give results which are not representative ofthe bulk contents of the tank because of particulate mattersettling. Where possibl
48、e, the contents of the tank should becirculated or agitated before sampling, or the sampling per-formed shortly after a tank has been filled.)9.4 Visually inspect the sample container before taking thesamples to verify that there are no visible particles presentinside the container. Fill the sample
49、container 95 volume %full, leaving space for vapor expansion. Protect the fuel samplefrom prolonged exposure to light by wrapping the container inaluminum foil or storing it in the dark to reduce the possibilityof particulate formation by light-promoted reactions. Do nottransfer the fuel sample from its original sample container intoan intermediate storage container. If the original samplecontainer is damaged or leaking, then a new sample must beobtained.9.5 Analyze fuel samples as soon as possible after sampling.When a fuel cannot be analyzed within one
