1、Designation: D7321 14Standard Test Method forTest Method for Particulate Contamination of Biodiesel B100Blend Stock Biodiesel Esters and Biodiesel Blends byLaboratory Filtration1This standard is issued under the fixed designation D7321; the number immediately following the designation indicates the
2、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 () indicates an editorial change since the last revision or reapproval.1. Scope*1.1 This test method covers the determination of the ma
3、ss ofparticulate contamination in B100 biodiesel in accordance withSpecification D6751 and BXX blends that are prepared againstall No. 1 and No. 2 grade fuels allowed within SpecificationsD396 and D975.NOTE 1Middle distillate fuels with flash points less than 38 C havebeen ignited by discharges of s
4、tatic electricity when the fuels have beenfiltered through inadequately bonded or grounded glass fiber filtersystems. See Guide D4865 for a more detailed discussion of staticelectricity formation and discharge.1.2 The values stated in SI units are to be regarded asstandard. No other units of measure
5、ment are included in thisstandard.1.3 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 applica-bility of regulatory limita
6、tions prior to use.2. Referenced Documents2.1 ASTM Standards:2D396 Specification for Fuel OilsD975 Specification for Diesel Fuel OilsD1193 Specification for Reagent WaterD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4865 Guide for Generation and Dissipation of Static Elec-tri
7、city in Petroleum Fuel SystemsD6751 Specification for Biodiesel Fuel Blend Stock (B100)for Middle Distillate Fuels3. Terminology3.1 Definitions:3.1.1 biodiesel, nfuel comprised of mono-alkyl esters oflong chain fatty acids derived from vegetable oils or animalfats, designated B100.3.1.2 biodiesel bl
8、end, BXX, nblend of biodiesel fuel withpetroleum based biodiesel fuel.3.1.3 bond, vto connect two parts of a system electricallyby means of a conductive wire to eliminate voltage differences.3.1.4 ground, vto connect electrically with earth.3.2 Definitions of Terms Specific to This Standard:3.2.1 fi
9、ltered flushing fluids, nany of three solvents,methanol, propan-2-ol (isopropanol), or 2,2,4-trimethylpentane, filtered through a nominal 0.45 m filter.3.2.2 glass fiber filter, nglass fiber filter used in this testmethod.4. Summary of Test Method4.1 B100 Biodiesel Blend Stock Filtration:4.1.1 Ameas
10、ured volume of about 400 mLof biodiesel ester(B100) is vacuum filtered through one 0.7 m glass fiber filter.When the contamination is high or of a nature that inducesslow filtration rates, two or more filtrations using a fresh filtereach time may be required to complete filtration in a reasonabletim
11、e.4.1.2 After the filtration has been completed, the filter iswashed with solvent, dried, and weighed. The particulatecontamination level is determined by the mass gained by theglass fiber filter, and is reported in units of grams per cubicmetre or its equivalent in milligrams per litre.4.2 BXX Biod
12、iesel Blend Filtration:4.2.1 A measured volume of about 800 mL of biodieselblend (BXX) is vacuum filtered through one 0.7 m glass fiberfilter. When the contamination is high or of a nature thatinduces slow filtration rates, two or more filtrations using afresh filter each time may be required to com
13、plete filtration ina reasonable time.4.2.2 After the filtration has been completed, the filter iswashed with solvent, dried, and weighed. The particulate1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibili
14、ty ofSubcommittee D02.14 on Stability and Cleanliness of Liquid Fuels.Current edition approved June 1, 2014. Published July 2014. Originally approvedin 2008. Last previous edition approved in 2011 as D7321 111. DOI: 10.1520/D7321-14.2For referenced ASTM standards, visit the ASTM website, www.astm.or
15、g, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C70
16、0, West Conshohocken, PA 19428-2959. United States1contamination level is determined by the mass gained from theglass fiber filter, and is reported in units of grams per cubicmetre or its equivalent in milligrams per litre.5. Significance and Use5.1 The mass of particulates present in a fuel is a si
17、gnificantfactor, 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.5.2 The test method ca
18、n be used in specifications andpurchase documents as a means of controlling particulatecontamination levels in the fuels purchased.6. Apparatus6.1 Filtration SystemArrange the following componentsas shown in Fig. 1.6.1.1 Funnel and Funnel Base, with filter support for a47 mm diameter glass fiber, an
19、d 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, orcopper installed in the flasks and grounded as shown in Fig. 1.NOTE 2The electrical bonding apparatus shown in Fig. 1 or othersuitable means of electrical
20、 grounding that ensure safe operation of thefiltration apparatus and flask can be used. If the filtrate is to besubsequently tested for stability, it is advisable not to use copper sincecopper ions catalyze gum formation during the stability test.6.1.3 Receiving Flask, 1.5 L or larger borosilicate g
21、lassvacuum filter flask, into which the filtration apparatus fits,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 the vacuumsystem. A fuel and solvent resistance rubber hose throughwhi
22、ch 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 may be used if capable of producing avacuum of 1 kPa to 100 kPa below a
23、tmospheric pressure whenmeasured at the receiving flask.6.2 Other Apparatus:6.2.1 Air Ionizer, if used for the balance case.Air ionizers ifused should be replaced annually.NOTE 3When using a solid-pan balance, the air ionizer may beomitted provided that, when weighing a glass fiber filter, it is pla
24、ced on thepan so that no part protrudes over the edge of the pan.6.2.2 Analytical Balance, single- or double-pan, with theprecision standard deviation of 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 cir
25、culation), controlling to 90 C 6 5 C.6.2.5 Flushing Fluid Dispenser, an apparatus for dispensingflushing fluid through a nominal 0.45 m filter.6.2.6 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 marke
26、d at 10 mL intervals. For samples that filter slowly,100 mL graduated cylinders may be required.6.2.8 Petri Dishes, approximately 12.5 cm in diameter, withremovable glass supports for glass fiber filters.NOTE 4Small watch glasses, approximately 5 cm to 7 cm in diameter,have also been found suitable
27、to support the glass fiber filter.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 Societ
28、y,where such specifications are available.3Other 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 WaterUnless otherwise indicated, referencesto water mean reagent water as
29、defined by Types I, II and III ofSpecification D1193.7.3 Flushing Fluids:7.3.1 Methanol, (Warning Flammable).7.3.2 2,2,4-trimethylpentane (isooctane), (WarningFlammable).7.4 propan-2-ol (2-propanol; isopropyl alcohol),(WarningFlammable).7.5 Liquid or Powder Detergent, water-soluble, for cleaningglas
30、sware.7.6 Glass Fiber Filter, plain, with a diameter of 47 mm anda nominal pore size of 0.7 m.7.7 Protective Cover, polyethylene film or clean aluminumfoil.3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagen
31、ts notlisted by the American 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 Schematic of Filtration SystemD7321 1428. Sampling8.1
32、Sampling for Procedure for Biodiesel Blend Stock(B100):8.1.1 The sample container should be 500 mL(60.015 L) involume and have a screw-on cap with an inert liner. Glasscontainers are preferred to facilitate a visual inspection of thecontents and the container before and after filling. Glasscontainer
33、s also allow for visual inspection of the container,after the sample is emptied, to confirm complete rinsing of thecontainer. Epoxy-lined sample cans, polytetrafluoroethylene(PTFE) bottles, and high density linear polyethylene bottleshave also been found suitable as sample containers, but theyare le
34、ss desirable since visual inspection of the interior of thecontainer is more difficult.8.1.1.1 It is imperative that the entire contents of the samplecontainer are filtered during the B100 filtration. This includesnot only all of the fuel but also all rinsings of the interior of thecontainer with fl
35、ushing fluid. Because of this, take care toprotect the sample from any external contamination.8.1.2 If it is not possible to sample in a 500 mLbottle, or thesample has already been received ina1Lbottle, follow8.1.2.1.8.1.2.1 Vigorously shake the sample for 1 min, and transfer400 mL to a clean fresh
36、500 mL (60.015 L) bottle. If a cleanfresh 500 mL (60.015 L) bottle is not available, use a cleanfresh 1 L (60.015 L) bottle.8.1.3 Precautions to avoid sample contamination shall in-clude selection of an appropriate sampling point. Samplesshould preferentially be obtained dynamically from a samplingl
37、oop in a distribution line, or from the flushing line of a fieldsampling kit. Ensure that the line to be sampled is flushed withfuel before taking the sample.8.1.3.1 Where it is desirable or only possible to obtainsamples from static storage, follow the procedures given inPractice D4057 or equivalen
38、t, taking precautions for cleanli-ness of all equipment used. Ensure that the sample has notpassed through intermediate containers prior to placement inthe prepared container.NOTE 5Samples obtained from static storage may give results that arenot representative of the bulk contents of the tank becau
39、se of particulatematter settling. Where possible, the contents of the tank should becirculated or agitated before sampling, or the sampling should beperformed shortly after a tank has been filled.8.1.4 Visually inspect the sample container before taking thesamples to verify that there are no visible
40、 particles presentinside the container. Fill the sample container 90 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
41、-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.8.1.5 Analyze fuel samples as soon as possible after sam-pling. When a fuel cannot be
42、 analyzed within one day, it shouldbe blanketed with an inert gas such as oxygen-free nitrogen,argon, or helium. Store at a temperature no higher than 10 C;samples with cloud points above 10 C may be stored at roomtemperature.8.2 Sampling for Procedure for Biodiesel Blends (BXX):8.2.1 The sample con
43、tainer for BXX shall be 1 L(60.015 L) in volume and have a screw-on cap with an inertliner. Glass containers are preferred to facilitate a visualinspection of the contents and the container before and afterfilling. Glass containers also allow for visual inspection of thecontainer, after the sample i
44、s emptied, to confirm completerinsing of the container. Epoxy-lined sample cans, polytetra-fluoroethylene (PTFE) bottles, and high density linear polyeth-ylene bottles have also been found suitable as samplecontainers, but these are less desirable since visual inspectionof the interior of the contai
45、ner is more difficult.8.2.1.1 It is important to note that the entire contents of thesample container are filtered during the BXX filtration. Thisincludes 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 samp
46、le from any external contamina-tion. The expectation is, allowing for ullage, that the volume inthe 1 L sample bottle will be 800 mL (60.015 L).8.2.2 Follow 8.1.3 8.1.5.9. Preparation of Apparatus and Sample Containers9.1 Clean all components of the filtration apparatus asdescribed in 9.1.1 9.1.4.9.
47、1.1 Remove any labels, tags, and so forth.9.1.2 Rinse apparatus thoroughly with propan-2-ol that hasbeen filtered through a 0.45 m glass fiber filter.9.1.3 Rinse thoroughly with filtered flushing fluid and dry.9.1.4 Keep a clean protective cover (the cover may be rinsedwith filtered flushing fluid)
48、over the top of the sample containeruntil the cap is installed. Similarly protect the funnel openingof the assembled filtration apparatus with a clean protectivecover until ready for use.9.1.5 Use clean sample containers.10. Preparation of Glass Fiber Filter10.1 For fuels containing little particula
49、te materials, onlyone filter is required (as a control filter is not required). If thefuel is highly contaminated, more than one filter may berequired (see Section 11). Clean all glassware used in prepa-ration of glass fiber filter as described in Section 9.10.2 Using forceps, place the glass fiber filter in a clean petridish. To facilitate handling, the glass fiber filter should rest onclean glass support rods or watch glasses in the petri dish.10.3 Place the petri dish with its lid slightly ajar, in a dryingoven at 90 C 6 5 C, and leave it for 30
