1、Designation: D 7501 09Standard Test Method forDetermination of Fuel Filter Blocking Potential of Biodiesel(B100) Blend Stock by Cold Soak Filtration Test (CSFT)1This standard is issued under the fixed designation D 7501; the number immediately following the designation indicates the year oforiginal
2、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. Scope1.1 This test method covers the determination by filtrationtime after co
3、ld soak of the suitability for a biodiesel (B100)blend stock that meets all other requirements of SpecificationD 6751 and has a cloud point below 68F (20C) to provideadequate low temperature operability performance to at leastthe cloud point of the finished blend.1.2 The formal precision of this tes
4、t method has not yet beendetermined. Interim precision for repeatability is included in13.1.1.3 The values stated in inch-pound units are to be regardedas standard. The values given in parentheses are mathematicalconversions to SI units that are provided for information onlyand are not considered st
5、andard.1.4 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 limitations prior to use.2. Refer
6、enced Documents2.1 ASTM Standards:2D 4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD 5452 Test Method for Particulate Contamination in Avia-tion Fuels by Laboratory FiltrationD 6300 Practice for Determination of Precision and BiasData for Use in Test Methods for Petroleum Produ
7、cts andLubricantsD 6751 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 as B100.3.1.2 bond, vto connect two
8、 parts of a system electricallyby means of a conductive wire to eliminate voltage differences.3.1.3 BXX blend, nfuel blend consisting of up to 20volume percent biodiesel designated as up to B20 conformingto the requirements of Specification D 6751 with the remainderbeing a light middle or middle dis
9、tillate grade diesel fuel andmeeting the requirements of this test method.3.1.3.1 DiscussionThe abbreviation BXX represents aspecific blend concentration in the range B2 to B20, where XXis the percent volume of biodiesel in the fuel blend.3.1.4 ground, vto connect electrically with earth.3.2 Definit
10、ions of Terms Specific to This Standard:3.2.1 air chamber, nunit to control temperature of samplefor cooling with maximum 0.5C variation from set point. Theunit shall use a microprocessor temperature controller withdigital set point and readout.Afood-grade refrigerator does notprovide adequate tempe
11、rature stability for this test method.3.2.2 minor component, nmaterial present in B100, typi-cally at concentrations well below 1% by mass.3.2.3 thermal history, nrange of temperatures that a batchor sample of B100 has experienced which can result inseparation or precipitation of minor components.3.
12、2.3.1 DiscussionCooling some biodiesel fuels can resultin precipitation or separation of minor components that havelimited solubility in B100. Heating these biodiesel fuels above40C is believed to redissolve most of these minor componentsand thus erase the thermal history of the sample.3.3 Abbreviat
13、ions:3.3.1 CSFTCold Soak Filtration Test4. Summary of Test Method4.1 In this test method, 300 mL of biodiesel (B100) is storedat 40 6 1F (4.5 6 0.5C) for 16 h, allowed to warm to 77 62F (25 6 1C), and vacuum filtered through a single 0.7 mglass fiber filter at controlled vacuum levels of 2125 in. of
14、 Hg.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 April 1, 2009. Published April 2009.2For referenced ASTM standards, v
15、isit 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.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428
16、-2959, United States.4.2 The filtration time is reported in seconds.5. Significance and Use5.1 Some substances that are soluble or appear to be solublein biodiesel (B100) at room temperature will, upon cooling totemperatures above the cloud point or standing at roomtemperature for extended periods,
17、come out of solution. Thisphenomenon has been observed in both B100 and BXX blends.These substances can cause filter plugging. This methodprovides an accelerated means of assessing the presence ofthese substances in B100 and their propensity to plug filters.5.1.1 B100 biodiesel fuels that give short
18、 filtration times areexpected to give satisfactory operation of BXX blends at leastdown to the cloud point of the biodiesel blends.5.2 The test method can be used in specifications as a meansof controlling levels of minor filter plugging components inbiodiesel and biodiesel blends.6. Apparatus6.1 Fi
19、ltration SystemArrange the following componentsas shown in Fig. 1.6.1.1 Funnel and Funnel Base, with a stainless steel filtersupport for a 47-mm diameter glass fiber filter, and locking ringor spring action clip, capable of receiving 300 mL.NOTE 1Sintered glass supports were found to give much highe
20、rfiltration times during initial studies and are not recommended to be used.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. 1.6.1.3 Electrical Bonding Apparatus, as described in TestMe
21、thod D 5452 or by using other suitable means of electricalgrounding that ensure safe operation of the filtration apparatusand flask.6.1.4 Receiving Flask, 1-L borosilicate glass vacuum filterflask, into which the filtration apparatus fits, and equipped witha sidearm to connect to the safety flask.6.
22、1.5 Safety Flask, 1-L borosilicate glass vacuum filter flaskequipped with a sidearm to connect the vacuum system. A fueland solvent resistant rubber hose, through which the groundingwire is connected to the sidearm of the receiving flask to thetube, passes through the rubber stopper in the top of th
23、e safetyflask.6.1.6 Vacuum System, capable of producing a vacuum of 70to 100 kPa below atmospheric pressure when measured at thesafety flask. A mechanical vacuum pump may be used if it hasthis capability.NOTE 2Water aspirated vacuum will not provide relative vacuumwithin the prescribed range.6.1.7 C
24、hilling Apparatus, either 6.1.7.1 or 6.1.7.2 may beused.6.1.7.1 Circulating Water Bath, capable of sustaining atemperature of 40 6 1F (4.5 6 0.5C).6.1.7.2 Air Chamber, capable of sustaining a temperature of40 6 1F (4.5 6 0.5C). The unit shall use microprocessortemperature control and have a digital
25、temperature control/display.6.1.8 Circulating Water Bath, capable of sustaining a tem-perature of 77 6 1F (25 6 0.5C).FIG. 1 Schematic of Filtration SystemD75010926.1.9 Glass Fiber Filters, plain, 47-mm diameter, nominalpore size 0.7-m.6.2 Other Apparatus:6.2.1 Forceps, approximately 12-cm long, fla
26、t-bladed, withnon-serrated, non-pointed tips.6.2.2 Graduated Cylinders, to contain at least 0.5 L of fluidand marked at 10-mL intervals. Samples that filter slowly mayrequire 100-mL graduated cylinders.6.2.3 Petri Dishes, approximately 12.5 cm in diameter, withremovable glass supports for glass fibe
27、r filters.6.2.3.1 Small Watch Glasses, approximately 5 to 7 cm indiameter, have been found suitable to support the glass fiberfilters.NOTE 3B100 will dissolve some plastics. This can cause the filters toadhere to the plastic.6.2.4 Protective Cover, polyethylene film or clean alumi-num foil.6.2.5 Tim
28、er, capable of displaying elapsed times of at least900 s to the nearest 0.1 s.6.2.6 Thermometer or RTD Sensor, for measuring sampletemperature, should be capable of measurement 61F(60.5C).7. Reagents and Materials7.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwi
29、se 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. Other grades may beused, provided it is first ascertained that the reagent is ofsufficient purity to pe
30、rmit its use without lessening the accu-racy of the determination.7.2 Flushing FluidsFlushing fluids are not required forthe test as the filter is not weighed. However, heptane orisooctane may be used to wash the apparatus after filtration toremove any residue.7.2.1 Heptane,(WarningFlammable.)7.2.2
31、2,2,4-trimethylpentane (isooctane),(WarningFlammable.)7.3 Liquid or Powder Detergent, water-soluble, for cleaningglassware.8. Sampling8.1 A separate representative sample shall be collected forthis test method. Samples may preferentially be obtaineddynamically from a sampling loop in a distribution
32、line or fromthe flushing line of a field sampling kit. Ensure that the line tobe sampled is flushed with fuel before collecting the sample.Alternatively, circulate or agitate the contents of the tank inorder to collect a representative sample that includes anyprecipitates that might have settled in
33、the tank. One option is tosample the tank immediately after filling, before the contentshave time to settle.8.1.1 Where it is necessary to obtain samples from staticstorage using a sampling container or intermediate containers,follow the procedures given in Practice D 4057 or equivalent,taking preca
34、utions for cleanliness of all equipment used. Thisis interpreted to mean a representative sample in accordancewith Practice D 4057, and refers to an “all-levels” sample.(WarningSamples obtained from static storage can giveresults which are not representative of the bulk contents of thetank because o
35、f particulate matter settling.)8.2 Precautionsto avoid sample contamination include:8.2.1 Selection of an appropriate sampling point.8.2.2 Use of clean sample containers. Visually inspect thesample container before taking the samples to verify that thereare no visible particles present inside the co
36、ntainer.8.2.3 Keeping a clean protective cover over the top of thesample container until the cap is replaced after filling.8.2.4 If the primary sample container cannot be selectedsuch that it is suitable for this test procedure, the sample shallpass through only a minimum number of intermediate cont
37、ain-ers prior to placement in the final container.8.2.5 After filling the sample container with 300 mL ofsample, protect the fuel sample from prolonged exposure tolight by wrapping the container in aluminum foil or storing itin the dark to reduce the possibility of particulate formation bylight-prom
38、oted reactions.8.3 If 300 mL of sample is not received in a 500-mL bottleor the sample has been received in a container not suitable forthis test, follow the sampling condition procedure in 8.4.8.4 Sample Conditioningfor samples received that mighthave been cooled to temperatures below 68F (20C):8.4
39、.1 Upon receipt of a biodiesel blend stock (B100)sample, the entire sample is to be heated to 104F (40C) forat least 3 h under an inert atmosphere to erase any thermalhistory and to dissolve any solids that might have precipitatedduring transit. After heating for the required time, allow thesample t
40、o sit for 24 h at a temperature no lower than 68F(20C).8.4.2 This sample conditioning step may be omitted if thesample was collected from a heated tank at a productionfacility. In this case, proceed directly to 8.5.8.4.3 If there is any doubt about the thermal history of thesample, the sample condit
41、ioning step shall be performed.8.5 Analyze fuel samples as soon as possible after sampling.8.6 Shake the sample vigorously for 1 min. If the sample isnot already in a 500-mL bottle suitable for this test procedure,transfer 300 mL to a clean, fresh 500 6 15-mL bottle. If a300-mL sample was received i
42、s already in such a bottle,proceed with the test procedure in Section 11.9. Preparation of Apparatus and Sample Containers9.1 Clean all components of the filtration apparatus usingthe reagents described in 7.2 and 7.3.9.1.1 Filtration apparatus shall be clean and dry prior to use.9.1.2 Remove any la
43、bels, tags, and so forth.10. Preparation of Glass Fiber Filter10.1 Each filtration uses one filter. The glass fiber filter usedfor each individual test may be identified by marking the petridish used to hold and transport the filter.10.2 Clean all glassware used in preparation of glass fiberfilter a
44、s described in 9.1.10.3 Using forceps, place the filter on clean glass supportrods or watch glasses in petri dish.D750109310.4 Place the petri dish, with its lid slightly ajar, in a dryingoven at 194F (90 6 2C and leave it for 30 min.10.5 Remove the petri dish from the drying oven. Keep thepetri dis
45、h cover ajar, such that the filter is protected fromcontamination from the atmosphere.Allow 30 min for the filterto come to equilibrium with room air temperature and humid-ity.10.6 Using clean forceps, place the filter centrally on thefilter support of the filtration apparatus (see Fig. 1). Install
46、thefunnel and secure with locking ring or spring clip.10.7 Protect the funnel opening of the assembled filtrationapparatus with a clean protective cover until ready for use.11. Procedure11.1 Place 300 mL of sample in a 500 mL glass bottle andset in a liquid or air chamber at 40 6 1F (4.5 6 0.5C) for
47、 166 0.25 h. A refrigerator is not suitable for this procedure.11.2 After the 16-h cold soak at 40 6 2F (4.5 6 1.1C) iscompleted, remove sample from bath and place in a circulatingwater bath with the temperature set to 77 6 1F (25 6 0.5C)according to 11.2.1 or 11.2.2. The sample shall be completelyl
48、iquid before filtration.11.2.1 If the sample is completely liquid after the 16-h coldsoak, heat the sample at 77 6 1F (25 6 0.5C) for 2 6 0.25h. Otherwise follow 11.2.2.11.2.2 If the sample is solid or contains any solids or hazeafter the 16-h cold soak, heat the sample at 77 6 1F (25 60.5C) for 4 6
49、 0.25 h.11.2.3 Verify that the sample is at 77 6 1F (25 6 0.5C) bydipping without stirring or agitating the sample with an RTDsensor or thermometer.11.3 Filter the samples as quickly as possible upon removalfrom the warming bath once the desired warming time haselapsed according to 11.2.1 or 11.2.2, whichever applies.11.4 Complete assembly of the receiving flask, 0.7 m glassfiber filter and funnel as a unit (see Fig. 1) before swirling thesample. To minimize operator exposure to fumes, the filteringprocedure may be performed
