1、Designation: D7501 12D7501 12aStandard 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 year ofor
2、iginal 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 by filtration time
3、 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 20C (68F) to provide adequate lowtemperature operability performance to at least the cloud point of the finished blend.1.2 The formal precision o
4、f 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 with its use. It is the respo
5、nsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D4057 Practice for Manual Sampling of Petroleum and Petroleum ProductsD6217 Test Method for Part
6、iculate 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 Stock (B100) for Middle Distillate Fuels3. Terminology3.1 Def
7、initions: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 wire to eliminate voltage differences.3.1.3 BXX blend, nfuel blen
8、d 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 this test method.3.1.3.1 DiscussionThe abbreviation BXX represe
9、nts 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, vto connect electrically with earth.3.2 Definitions of Terms Specific to This Standard:1 This test method is under the jurisdiction of ASTM Committee D02 on Petroleum
10、 Products Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.14 on Stability and Cleanliness of Liquid Fuels.Current edition approved April 15, 2012Nov. 1, 2012. Published July 2012February 2013. Originally approved in 2009. Last previous edition approved in 2
11、0092012 asD750109b.12. DOI: 10.1520/D7501-12.10.1520/D7501-12A.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 standards Document Summary page on the ASTM websit
12、e.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 accurately, ASTM recommends that users consult prior e
13、ditions 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 Drive, PO Box C700, West Conshohocken, PA 19428-2
14、959. United States13.2.1 air chamber, nunit to control temperature of sample for cooling with maximum 0.5C variation from set point. The unitshall use a microprocessor temperature controller with digital set point and readout. A food-grade refrigerator does not provideadequate temperature stability
15、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 has experienced which can result in separationor precipitation of minor components.3.2.3.1 DiscussionC
16、ooling some biodiesel fuels can result in precipitation or separation of minor components that have limited solubility in B100.Heating these biodiesel fuels above 40C is believed to redissolve most of these minor components and thus erase the thermalhistory of the sample.3.3 Abbreviations:3.3.1 CSFT
17、Cold Soak Filtration Test4. Summary of Test Method4.1 In this test method, 300 mL of biodiesel (B100) is stored at 4.5 6 0.5C (40 6 1F) for 16 h, allowed to warm to 25 61C (77 6 2F), and vacuum filtered through a single 0.7 m glass fiber filter at controlled vacuum levels of 7085 kPa (2125in. of Hg)
18、.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 temperature will, upon cooling totemperatures above the cloud point or standing at room temperature for extended periods, come out of soluti
19、on. This phenomenonhas been observed in both B100 and BXX blends. These substances can cause filter plugging. This method provides an acceleratedmeans of assessing the presence of these substances in B100 and their propensity to plug filters.5.1.1 B100 biodiesel fuels that give short filtration time
20、s 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 specifications as a means of controlling levels of minor filter plugging components inbiodiesel and biodiesel blends.6. Apparatus6.1 Filtration Syste
21、mArrange 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, and locking ring orspring action clip, capable of receiving 300 mL.NOTE 1Sintered glass supports were found to give much higher filtration
22、 times during initial studies and are not recommended to be used.6.1.2 Ground/Bond Wire, 0.912-2.59-mm (No. 10 through No. 19) bare stranded flexible, stainless steel or copper installed inthe flasks and grounded as shown in Fig. 1.6.1.3 Electrical Bonding Apparatus, as described inTest Method D6217
23、 or by using other suitable means of electrical groundingthat ensure safe operation of the filtration apparatus and flask. This may not be necessary in filtering biodiesel B100 because ofthe higher electrical conductivity.6.1.4 Receiving Flask, 1-L borosilicate glass vacuum filter flask, into which
24、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 equipped with a sidearm to connect the vacuum system.Afuel andsolvent resistant rubber hose, through which the grounding wire is connected to the si
25、dearm 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 of 70 to 85 kPa (2125 (21 to 25 in. of Hg) when measured at the safetyflask. A mechanical vacuum pump may be used if it has this capability. A
26、vacuum pump with free air displacement capacity of 25to 30 L/min at 60 Hz has been found to be suitable to pull the vacuum down to the required level within 30 to 40 s when guardand filtration flasks are present in the assembly.NOTE 2Water aspirated vacuum will not provide relative vacuum within the
27、 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 temperature of 4.5 6 0.5C (40 6 1F).6.1.7.2 Air Chamber, capable of sustaining a temperature of 4.5 6 0.5C (40 6 1F). The unit shall use microprocessortemperature
28、 control and have a digital temperature control/display.D7501 12a26.1.8 Circulating Water Bath, capable of sustaining a temperature of 25 6 0.5C (77 6 1F).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
29、 this purpose.6.2 Other Apparatus:6.2.1 Forceps, approximately 12-cm long, flat-bladed, with non-serrated, non-pointed tips.6.2.2 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
30、, approximately 12.5 cm in diameter, with removable glass supports for glass fiber filters.6.2.3.1 Small Watch Glasses, approximately 5 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
31、 plastic.6.2.4 Protective Cover, polyethylene film or clean aluminum foil.6.2.5 Timer, capable of displaying elapsed times 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 60.5C (61F).7. Reagents and Materials7
32、.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that allreagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, wheresuch specifications are available. Other grades may
33、be used, provided it is first ascertained that the reagent is of sufficient purityto permit its use without lessening the 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
34、apparatus after filtration to remove any residue.7.2.1 Heptane, (Warning Flammable.)7.2.2 2,2,4-trimethylpentane (isooctane), (WarningFlammable.)7.3 Liquid or Powder Detergent, water-soluble, for cleaning glassware.8. Sampling8.1 Aseparate representative sample shall be collected for this test metho
35、d. Samples may preferentially 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 is3 Whatman filters were used in the ILS. See Section 13.FIG. 1 Schematic of Filtration SystemD7501 12a3flushed with
36、fuel before collecting the sample. Alternatively, circulate or agitate the contents of the tank in order to collect arepresentative 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 s
37、ettle.8.1.1 Where it is necessary to obtain samples from static storage using a sampling container or intermediate containers, followthe procedures given in Practice D4057 or equivalent, taking precautions for cleanliness of all equipment used. This is interpretedto mean a representative sample in a
38、ccordance with Practice D4057, and refers to an “all-levels” sample. (WarningSamplesobtained from static storage can give 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
39、of an appropriate sampling point.8.2.2 Use of clean sample containers. Visually inspect the sample container before taking 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 i
40、s replaced after filling.8.2.4 If the primary sample container cannot be selected such that it is suitable for this test procedure, 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 30
41、0 mL of sample, protect the fuel sample from prolonged exposure to light bywrapping the container in aluminum foil or storing 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
42、 received in a container not suitable for thistest, follow the sampling condition procedure in 8.4.8.4 Sample Conditioningfor samples received that might have been cooled to temperatures below 20C (68F):8.4.1 Upon receipt of a biodiesel blend stock (B100) sample, the entire sample is to be heated to
43、 40C (104F) for at least 3 hunder an inert atmosphere to erase any thermal history and to dissolve any solids that might have precipitated during transit. Afterheating for the required time, allow the sample to sit for 24 h at a temperature no lower than 20C (68F).8.4.2 This sample conditioning step
44、 may be omitted if the sample was collected from a heated tank at a production facility. Inthis case, proceed directly 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 sampli
45、ng.8.6 Shake the sample vigorously for 1 min. If the sample is not already in a 500-mL bottle suitable for this test procedure,transfer 300 mL to a clean, fresh 500 6 15-mL bottle. If a 300-mL sample was received is already in such a bottle, proceed withthe test procedure in Section 11.9. Preparatio
46、n of Apparatus and Sample Containers9.1 Clean all components of the filtration apparatus using the 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 labels, tags, and so forth.10. Preparation of Glass Fiber Filter10.1 Each filtration us
47、es one filter as specified in 6.1.9. The glass fiber filter used for each individual test may be identified bymarking 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 cl
48、ean 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 6 2C (194 6 3.6F) 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 fromcontami
49、nation from the atmosphere. Allow 30 min for the filter to come to equilibrium with room air temperature and humidity.10.6 Using clean forceps, place the filter centrally on the filter support of the filtration apparatus (see Fig. 1). Install the funneland secure with locking ring or spring clip.10.7 Protect the funnel opening of the assembled filtration apparatus with a clean protective cover until ready for use.11. Procedure11.1 Place 300 mL of sample in a 500 mL glass bottle and set in a liquid or air chamber at 4.5 6 0.5C
