1、Designation: D 7321 08An American National StandardStandard 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 D 7321; the number immediately following
2、 the designation 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.1. Scope1.1 This test method cov
3、ers the determination of the mass ofparticulate contamination in B100 biodiesel in accordance withSpecification D 6751 and BXX blends that are prepared againstall No. 1 and No. 2 grade fuels allowed within SpecificationsD 396, D 975, D 2880, and D 3699.NOTE 1Middle distillate fuels with flash points
4、 less than 38C havebeen ignited by discharges of static electricity when the fuels have beenfiltered through inadequately bonded or grounded glass fiber filtersystems. See Guide D 4865 for a more detailed discussion of staticelectricity formation and discharge.1.2 The values stated in SI units are t
5、o be regarded as thestandard. The values given in parentheses are for informationonly.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 a
6、nd determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 396 Specification for Fuel OilsD 975 Specification for Diesel Fuel OilsD 1193 Specification for Reagent WaterD 2880 Specification for Gas Turbine Fuel OilsD 3699 Specification for Kero
7、sineD 4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD 4865 Guide for Generation and Dissipation of StaticElectricity in Petroleum Fuel SystemsD 5452 Test Method for Particulate Contamination in Avia-tion Fuels by Laboratory FiltrationD 6751 Specification for Biodiesel Fuel Blen
8、d 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 blend, BXX, nblend of biodiesel fuel withpetroleum based biodiesel fuel.3.1
9、.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 control glass fiber filter, nlower of the two stackedglass fiber filters us
10、ed in this test method.3.2.2 filtered flushing fluids, neither of two solvents,heptane or 2,2,4-trimethylpentane, filtered through a nominal0.45 m filter.3.2.3 test glass fiber filter, nupper of the two stacked glassfiber filters used in this test method.4. Summary of Test Method4.1 B100 Biodiesel B
11、lend Stock Filtration:4.1.1 Ameasured volume of about 400 mLof biodiesel ester(B100) is vacuum filtered through two 0.7 m glass fiber filters(a test filter and a control filter). When the contamination ishigh or of a nature that induces slow filtration rates, two ormore filtrations using a fresh fil
12、ter set consisting of test andcontrol filters each time may be required to complete filtrationin a reasonable time.4.1.2 After the filtration has been completed, the test filterand control filters are washed with solvent, dried, and weighed.The particulate contamination level is determined by subtra
13、ct-ing the mass gain from the control filter from the mass gainedby the test filter, and is reported in units of g/m3or itsequivalent in mg/L.4.2 BXX Biodiesel Blend Filtration:1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct res
14、ponsibility of SubcommitteeD02.14 on Stability and Cleanliness of Liquid Fuels.Current edition approved March 15, 2008. Published April 2008.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volu
15、me information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.4.2.1 A measured volume of about 800 mL of biodieselblend (BXX) is vacuum filtered through two 0.7 m glas
16、s fiberfilters (a test filter and a control filter). When the contaminationis high or of a nature that induces slow filtration rates, two ormore filtrations using a fresh filter set consisting of test andcontrol filters each time may be required to complete filtrationin a reasonable time.4.2.2 After
17、 the filtration has been completed, the test filterand control filters are washed with solvent, dried, and weighed.The particulate contamination level is determined by subtract-ing the mass gain from the control filter from the mass gainedby the test filter, and is reported in units of g/m3or itsequ
18、ivalent in mg/L.5. Significance and Use5.1 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
19、 a means of assessing the mass ofparticulates present in a fuel sample.5.2 The test method can 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
20、 Fig. 1.6.1.1 Funnel and Funnel Base, with filter support for a47-mm diameter glass fiber, and locking ring or spring actionclip.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
21、 2The electrical bonding apparatus described in Test MethodD 5452 or other suitable means of electrical grounding that 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 coppersince copper ions
22、 catalyze gum formation during the stability test.6.1.3 Receiving Flask, 1.5 L or larger borosilicate glassvacuum 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 eq
23、uipped 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 flask.6.1.5 Vacuum System, either a water aspirat
24、ed or a mechani-cal vacuum pump may 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, if used for the balance case. Air ionizers ifused should be replaced annually.NOTE 3When using a solid-pan
25、 balance, the air ionizer may beomitted provided that, when weighing a glass fiber filter, it is placed 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 hand
26、ling clean sample containerlids.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 filter.6.2.6 Forceps, approximately 12-cm long, flat-bladed, withno
27、n-serrated, non-pointed tips.6.2.7 Graduated Cylinders, to contain at least 1 L of fluidand marked 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
28、.NOTE 4Small watch glasses, approximately 5 to 7 cm in diameter,have also been found suitable to support the glass fiber 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
29、 to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,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 determi
30、nation.7.2 Purity of WaterUnless otherwise indicated, referencesto water mean reagent water as defined by Types I, II and III ofSpecification D 1193.7.3 Flushing Fluids:7.3.1 Heptane,(WarningFlammable).7.3.2 2,2,4-trimethylpentane (isooctane),(WarningFlammable).7.4 propan-2-ol (2-propanol; isopropyl
31、 alcohol),(WarningFlammable).3Reagent Chemicals, American Chemical Society Specifications , AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., an
32、d the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.FIG. 1 Schematic of Filtration SystemD73210827.5 Liquid or Powder Detergent, water-soluble, for cleaningglassware.7.6 Test Glass Fiber Filters, plain, 47-mm diameter, nomi-nal pore size 0
33、.7-m.7.7 Control Glass Fiber Filters, (see Note 7), 47-mmdiameter, nominal pore size 0.7-m.7.7.1 Glass fiber filters with a grid imprinted on their surfacemay be used as control glass fiber filters for identification.7.8 Protective Cover, polyethylene film or clean aluminumfoil.8. Sampling8.1 Sampli
34、ng for Procedure for Biodiesel Blend Stock(B100):8.1.1 The sample container should be 500 mL (60.15 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. Glasscontainers also
35、 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 less des
36、irable 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 flushing
37、 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 mL bottle, 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 500 m
38、L (60.15 L) bottle. If a cleanfresh 500 mL (60.15 L) bottle is not available, use a cleanfresh 1 L (60.15 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 samplingloop in a
39、 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 D 4057 or equivalent, taki
40、ng 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 because of p
41、articulatematter 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 partic
42、les 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-promot
43、ed 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 analyz
44、ed 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 10C(50F); samples with cloud points above 10C may be stored atroom temperature.8.2 Sampling for Procedure for Biodiesel Blends (BXX):8.2.1 The sample contai
45、ner for BXX shall be 1 L (60.15 L)in volume 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. Glasscontainers also allow for visual inspection of the container,after the sample is em
46、ptied, 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 theseare less desirable since visual inspection of the interior of thecontainer is m
47、ore 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 sample from
48、any external contamina-tion. The expectation is, allowing for ullage, that the volume inthe 1-L sample bottle will be 800 mL (60.15 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 9.1.1-9.1.4.9.1.1 Remov
49、e 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) 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 Filters10.1 Each set
