1、Designation: D7501 12a (Reapproved 2017)D7501 18Standard 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 indic
2、ates 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 () indicates an editorial change since the last revision or reapproval.1. Scope Scope*1.1 This test method covers the determin
3、ation by filtration time after cold soak of the suitability for a biodiesel (B100) blendstock that meets all other requirements of Specification D6751 and has a cloud point below 20 C (68 F) to provide adequate lowtemperature operability performance to at least the cloud point of the finished blend.
4、1.2 The formal precision of this test method is included in 13.1 on Precision.1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.4 This standard does not purport to address all of the safety concerns, if any, associated wit
5、h its use. It is the responsibilityof the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability ofregulatory limitations prior to use.1.5 This international standard was developed in accordance with internationally recognized princ
6、iples on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D4057 Practice for Manual Sampling
7、 of Petroleum and Petroleum ProductsD6217 Test Method for Particulate Contamination in Middle Distillate Fuels by Laboratory FiltrationD6300 Practice for Determination of Precision and Bias Data for Use in Test Methods for Petroleum Products and LubricantsD6751 Specification for Biodiesel Fuel Blend
8、 Stock (B100) for Middle Distillate Fuels3. Terminology3.1 Definitions:3.1.1 biodiesel, nfuel comprised of mono-alkyl esters of long chain fatty acids derived from vegetable oils or animal fats,designated as B100.3.1.2 bond, vto connect two parts of a system electrically by means of a conductive wir
9、e to eliminate voltage differences.3.1.3 BXX blend, nfuel blend consisting of up to 20 volume percent biodiesel designated as up to B20 conforming to therequirements of Specification D6751 with the remainder being a light middle or middle distillate grade diesel fuel and meeting therequirements of t
10、his test method.3.1.3.1 DiscussionThe abbreviation BXX represents a specific blend concentration in the range B2 to B20, where XX is the percent volume ofbiodiesel in the fuel blend.3.1.4 ground, vvtto connect electrically with earth.ground (earth).1 This test method is under the jurisdiction ofASTM
11、 Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of SubcommitteeD02.14 on on Stability, Cleanliness and Compatibility of Liquid Fuels.Current edition approved Oct. 1, 2017July 1, 2018. Published November 2017August 2018. Originally approved in 2009.
12、 Last previous edition approved in 2012 asD7501D7501 12a (2017).12a. DOI: 10.1520/D7501-12AR17.10.1520/D7501-18.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the s
13、tandards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accur
14、ately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor
15、Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13.2 Definitions of Terms Specific to This Standard:3.2.1 air chamber, nunit to control temperature of sample for cooling with maximum 0.5 C variation from set point. The unitshall use a microprocessor temperature controller with dig
16、ital set point and readout. A food-grade refrigerator does not provideadequate temperature stability for this test method.3.2.2 minor component, nmaterial present in B100, typically at concentrations well below 1 % by mass.3.2.3 thermal history, nrange of temperatures that a batch or sample of B100
17、has experienced which can result in separationor precipitation of minor components.3.2.3.1 DiscussionCooling some biodiesel fuels can result in precipitation or separation of minor components that have limited solubility in B100.Heating these biodiesel fuels above 40 C is believed to redissolve most
18、 of these minor components and thus erase the thermalhistory of the sample.3.3 Abbreviations:3.3.1 CSFTCold Soak Filtration Test4. Summary of Test Method4.1 In this test method, 300 mL of biodiesel (B100) is stored at 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 F), an
19、d vacuum filtered through a single 0.7 m glass fiber filter at controlled vacuum levels of 70 kPato 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 soluble in biodiesel (B100) at room tem
20、perature will, upon cooling totemperatures above the cloud point or standing at room temperature for extended periods, come out of solution. This phenomenonhas been observed in both B100 and BXX blends. These substances can cause filter plugging. This method provides an acceleratedmeans of assessing
21、 the presence of these substances in B100 and their propensity to plug filters.5.1.1 B100 biodiesel fuels that give short filtration times are expected to give satisfactory operation of BXX blends at least downto the cloud point of the biodiesel blends.5.2 The test method can be used in specificatio
22、ns as a means of controlling levels of minor filter plugging components inbiodiesel and biodiesel blends.6. Apparatus6.1 Filtration SystemArrange the following components as shown in Fig. 1.6.1.1 Funnel and Funnel Base, with a stainless steel filter support for a 47 mm diameter glass fiber filter, a
23、nd locking ring orspring action clip, capable of receiving 300 mL.NOTE 1Sintered glass supports were found to give much higher filtration 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. 10 through No. 19) bare stranded flexible, stainl
24、ess steel or copperinstalled in the flasks and grounded as shown in Fig. 1.6.1.3 Electrical Bonding Apparatus, as described inTest Method D6217 or by using other suitable means of electrical groundingthat ensure safe operation of the filtration apparatus and flask. This may not be necessary in filte
25、ring biodiesel B100 because ofthe higher electrical conductivity.6.1.4 Receiving Flask, 1 L borosilicate glass vacuum filter flask, into which the filtration apparatus fits, and equipped with asidearm to connect to the safety flask.6.1.5 Safety Flask, 1 L borosilicate glass vacuum filter flask equip
26、ped with a sidearm to connect the vacuum system.Afuel andsolvent resistant rubber hose, through which the grounding wire is connected to the sidearm of the receiving flask to the tube,passes through the rubber stopper in the top of the safety flask.6.1.6 Vacuum System, capable of producing a vacuum
27、of 70 kPa to 85 kPa (21 in. of Hg to 25 in. of Hg) when measured atthe safety flask. A mechanical vacuum pump may be used if it has this capability. A vacuum pump with free air displacementcapacity of 25 Lmin to 30 Lmin at 60 Hz has been found to be suitable to pull the vacuum down to the required l
28、evel within 30 sto 40 s when guard and filtration flasks are present in the assembly.NOTE 2Water aspirated vacuum will not provide relative vacuum within the prescribed range.6.1.7 Chilling Apparatus, either 6.1.7.1 or 6.1.7.2 may be used.6.1.7.1 Circulating Water Bath, capable of sustaining a tempe
29、rature of 4.5 C 6 0.5 C (40 F 6 1 F).D7501 1826.1.7.2 Air Chamber, capable of sustaining a temperature of 4.5 C 6 0.5 C (40 F 6 1 F). The unit shall use microprocessortemperature control and have a digital temperature control/display.6.1.8 Circulating Water Bath, capable of sustaining a temperature
30、of 25 C 6 0.5 C (77 F 6 1 F).6.1.9 Whatman Glass Fiber Filters (GF/F),3plain, 47 mm diameter, nominal pore size 0.7 m. Acid treated low metal TCLPfilters are not suitable for this purpose.6.2 Other Apparatus:6.2.1 Forceps, approximately 12 cm long, flat-bladed, with non-serrated, non-pointed tips.6.
31、2.2 Graduated Cylinders, to contain at least 0.5 L of fluid and 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, with removable glass supports for glass fiber filters.6.2.3.1 Small Watch Glasses, approx
32、imately 5 cm to 7 cm in diameter, have been found suitable to support the glass fiber filters.NOTE 3B100 will dissolve some plastics. This can cause the filters to adhere to the plastic.6.2.4 Protective Cover, polyethylene film or clean aluminum foil.6.2.5 Timer, capable of displaying elapsed times
33、of at least 900 s to the nearest 0.1 s.6.2.6 Thermometer or RTD Sensor, for measuring sample temperature, should be capable of measurement 60.5 C (61 F).7. Reagents and Materials7.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that
34、allreagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, wheresuch specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficient purityto permit its use without lessening the
35、 accuracy of the determination.7.2 Flushing FluidsFlushing fluids are not required for the test as the filter is not weighed. However, heptane or isooctane maybe used to wash the apparatus after filtration to remove any residue.7.2.1 Heptane, (Warning Flammable.)7.2.2 2,2,4-trimethylpentane (isoocta
36、ne), (WarningFlammable.)7.3 Liquid or Powder Detergent, water-soluble, for cleaning glassware.3 Whatman filters were used in the ILS. See Section 13.FIG. 1 Schematic of Filtration SystemD7501 1838. Sampling8.1 Aseparate representative sample shall be collected for this test method. Samples may prefe
37、rentially be obtained dynamicallyfrom a sampling loop in a distribution line or from the flushing line of a field sampling kit. Ensure that the line to be sampled isflushed with fuel before collecting the sample. Alternatively, circulate or agitate the contents of the tank in order to collect arepre
38、sentative sample that includes any precipitates that might have settled in the tank. One option is to sample the tankimmediately after filling, before the contents have time to settle.8.1.1 Where it is necessary to obtain samples from static storage using a sampling container or intermediate contain
39、ers, followthe procedures given in Practice D4057 or equivalent, taking precautions for cleanliness of all equipment used. This is interpretedto mean a representative sample in accordance with Practice D4057, and refers to an “all-levels” sample. (WarningSamplesobtained from static storage can give
40、results which are not representative of the bulk contents of the tank because of particulatematter 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 the sample container before taking
41、 the samples to verify that there areno visible particles present inside the container.8.2.3 Keeping a clean protective cover over the top of the sample container until the cap is replaced after filling.8.2.4 If the primary sample container cannot be selected such that it is suitable for this test p
42、rocedure, the sample shall passthrough only a minimum number of intermediate containers prior to placement in the final container.8.2.5 After filling the sample container with 300 mL of sample, protect the fuel sample from prolonged exposure to light bywrapping the container in aluminum foil or stor
43、ing it in the dark to reduce the possibility of particulate formation by light-promotedreactions.8.3 If 300 mL of sample is not received in a 500 mL bottle or the sample has been received in a container not suitable for thistest, follow the sampling condition procedure in 8.4.8.4 Sample Conditioning
44、for samples received that might have been cooled to temperatures below 20 C (68 F):8.4.1 Upon receipt of a biodiesel blend stock (B100) sample, the entire sample is to be heated to 40 C (104 F) for at least 3 hunder an inert atmosphere to erase any thermal history and to dissolve any solids that mig
45、ht have precipitated during transit. Afterheating for the required time, allow the sample to sit for 24 h at a temperature no lower than 20 C (68 F).8.4.2 This sample conditioning step may be omitted if the sample was collected from a heated tank at a production facility. Inthis case, proceed direct
46、ly to 8.5.8.4.3 If there is any doubt about the thermal history of the sample, the sample conditioning 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 is not already in a 500 mL bottle suitable for this test
47、 procedure,transfer 300 mL to a clean, fresh 500 mL 6 15 mL bottle. If a 300 mL sample was received is already in such a bottle, proceedwith the test procedure in Section 11.9. Preparation of Apparatus and Sample Containers9.1 Clean all components of the filtration apparatus using the reagents descr
48、ibed in 7.2 and 7.3.9.1.1 Filtration 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. The glass fiber filter used for each individual test may be identified bymar
49、king the petri dish used to hold and transport the filter.10.2 Clean all glassware used in preparation of glass fiber filter as described in 9.1.10.3 Using forceps, place the filter on clean glass support rods or watch glasses in petri dish.10.4 Place the petri dish, with its lid slightly ajar, in a drying oven at 90 C 6 2 C (194 F 6 3.6 F) and leave it for 30 min.10.5 Remove the petri dish from the drying oven. Keep the petri dish cover ajar, such that the filter is protected fromcontamination from the atmosphere.
