1、Designation: D7501 12a (Reapproved 2017)Standard 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 D7501; 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. Scope1.1 This test method covers the determination by filtra
3、tiontime after cold soak of the suitability for a biodiesel (B100)blend stock that meets all other requirements of SpecificationD6751 and has a cloud point below 20 C (68 F) to provideadequate low temperature operability performance to at leastthe cloud point of the finished blend.1.2 The formal pre
4、cision of this test method is included in13.1 on Precision.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is there
5、sponsibility of the user of this standard to establish appro-priate safety, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.5 This international standard was developed in accor-dance with internationally recognized principles on standard-
6、ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D4057 Practice for Manual Sampling of Petroleum an
7、dPetroleum ProductsD6217 Test Method for Particulate Contamination in MiddleDistillate Fuels by Laboratory FiltrationD6300 Practice for Determination of Precision and BiasData for Use in Test Methods for Petroleum Products andLubricantsD6751 Specification for Biodiesel Fuel Blend Stock (B100)for Mid
8、dle 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 parts of a system electricallyby means of a conductive wire to eliminate voltage
9、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 D6751 with the remainderbeing a light middle or middle distillate grade diesel fuel andmeeting the requirements of this test method.3.1.3.1 D
10、iscussionThe 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 Definitions of Terms Specific to This Standard:3.2.1 air chamber, nunit to control tempera
11、ture of samplefor cooling with maximum 0.5 C variation from set point. Theunit shall use a microprocessor temperature controller withdigital set point and readout.Afood-grade refrigerator does notprovide adequate temperature stability for this test method.3.2.2 minor component, nmaterial present in
12、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.3.2.3.1 DiscussionCooling some biodiesel fuels can resultin precipitation or separa
13、tion of minor components that havelimited solubility in B100. Heating these biodiesel fuels above40 C is believed to redissolve most of these minor compo-nents and thus erase the thermal history of the sample.3.3 Abbreviations:3.3.1 CSFTCold Soak Filtration Test1This test method is under the jurisdi
14、ction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.14 on on Stability, Cleanliness and Compatibility of LiquidFuels.Current edition approved Oct. 1, 2017. Published November 2017. Originallyapproved in 2009. Last previou
15、s edition approved in 2012 as D750112a. DOI:10.1520/D7501-12AR17.2For referenced ASTM standards, 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 webs
16、ite.Copyright 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 I
17、nternational Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.14. Summary of Test Method4.1 In this test method, 300 mL of biodiesel (B100) is storedat 4.5 C 6 0.5 C (40 F 6 1 F) for 16 h, allowed to warm to25 C 6 1 C (77 F 6 2
18、F), and vacuum filtered through asingle 0.7 m glass fiber filter at controlled vacuum levels of70 kPa to 85 kPa (21 in. of Hg to 25 in. of Hg).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
19、 temperature will, upon cooling totemperatures above the cloud point or standing at roomtemperature for extended periods, 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 assessi
20、ng the presence ofthese substances in B100 and their propensity to plug filters.5.1.1 B100 biodiesel fuels that give short 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 specificatio
21、ns as a meansof controlling levels of minor filter plugging components inbiodiesel and biodiesel blends.6. Apparatus6.1 Filtration 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
22、locking ringor spring action clip, capable of receiving 300 mL.NOTE 1Sintered glass supports were found to give much higherfiltration times during initial studies and are not recommended to be used.6.1.2 Ground/Bond Wire, 0.912 mm to 2.59 mm (No. 10through No. 19) bare stranded flexible, stainless s
23、teel or copperinstalled in the flasks and grounded as shown in Fig. 1.6.1.3 Electrical Bonding Apparatus, as described in TestMethod D6217 or by using other suitable means of electricalgrounding that ensure safe operation of the filtration apparatusand flask. This may not be necessary in filtering b
24、iodiesel B100because of the higher electrical conductivity.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.6.1.5 Safety Flask, 1 L borosilicate glass vacuum filter flaskequipped with
25、 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 the safetyflask.6.1.6 Vacuum System, capable of producing a vacuum of70 kPa
26、 to 85 kPa (21 in. of Hg to 25 in. of Hg) whenmeasured at the safety flask. A mechanical vacuum pump maybe used if it has this capability. A vacuum pump with free airdisplacement capacity of 25 L min to 30 L min at 60 Hz hasbeen found to be suitable to pull the vacuum down to therequired level withi
27、n 30 s to 40 s when guard and filtrationflasks are present in the assembly.NOTE 2Water aspirated vacuum will not provide relative vacuumwithin the prescribed range.6.1.7 Chilling Apparatus, either 6.1.7.1 or 6.1.7.2 may beused.FIG. 1 Schematic of Filtration SystemD7501 12a (2017)26.1.7.1 Circulating
28、 Water Bath, capable of sustaining atemperature of 4.5 C 6 0.5 C (40 F 6 1 F).6.1.7.2 Air Chamber, capable of sustaining a temperature of4.5 C 6 0.5 C (40 F 6 1 F). The unit shall use micropro-cessor temperature control and have a digital temperaturecontrol/display.6.1.8 Circulating Water Bath, capa
29、ble of sustaining a tem-perature of 25 C 6 0.5 C (77 F 6 1 F).6.1.9 Whatman Glass Fiber Filters (GF/F),3plain, 47 mmdiameter, nominal pore size 0.7 m. Acid treated low metalTCLP filters are not suitable for this purpose.6.2 Other Apparatus:6.2.1 Forceps, approximately 12 cm long, flat-bladed, withno
30、n-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 fiber filters.6.2.3.
31、1 Small Watch Glasses, approximately 5 cm 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 aluminumfoil.6.2.5 Timer, capable of
32、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 60.5 C(61 F).7. Reagents and Materials7.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated,
33、 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 permit its use
34、without lessening the accu-racy of the determination.7.2 Flushing FluidsFlushing fluids are not required for thetest as the filter is not weighed. However, heptane or isooctanemay be used to wash the apparatus after filtration to removeany residue.7.2.1 Heptane, (Warning Flammable.)7.2.2 2,2,4-trime
35、thylpentane (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 line or fr
36、omthe 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 the tank.
37、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 D4057 or equivalent,taking precautions for
38、cleanliness of all equipment used. Thisis interpreted to mean a representative sample in accordancewith Practice D4057, 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 of particulat
39、e 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 container.8.2.
40、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 contain-ers prio
41、r 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-promoted reactio
42、ns.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 20 C (68 F):8.4.1 Upon re
43、ceipt of a biodiesel blend stock (B100)sample, the entire sample is to be heated to 40 C (104 F) 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 to sit fo
44、r 24 h at a temperature no lower than 20 C(68 F).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 conditioning
45、 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 mL 6 15 mL bottle. If a300 mL sample was received is a
46、lready in such a bottle,proceed with the test procedure in Section 11.3Whatman filters were used in the ILS. See Section 13.D7501 12a (2017)39. 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 Filtrati
47、on apparatus shall be clean and dry prior to use.9.1.2 Remove any labels, tags, and so forth.10. Preparation of Glass Fiber Filter10.1 Each filtration uses one filter as specified in 6.1.9. Theglass fiber filter used for each individual test may be identifiedby marking the petri dish used to hold an
48、d transport the filter.10.2 Clean all glassware used in preparation of glass fiberfilter as described in 9.1.10.3 Using forceps, place the filter on clean glass supportrods or watch glasses in petri dish.10.4 Place the petri dish, with its lid slightly ajar, in a dryingoven at 90 C 6 2 C (194 F 6 3.
49、6 F) and leave it for30 min.10.5 Remove the petri dish from the drying oven. Keep thepetri dish 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 thefunnel and secure with locking ring or spring clip.10.7 Protect the funnel opening of the assembled filtrationapparatus with a c
