1、Designation: D7321 14D7321 16Standard 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 D7321; the number immediately following the designation indica
2、tes 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*1.1 This test method covers the determination o
3、f the mass of particulate contamination in B100 biodiesel in accordance withSpecification D6751 and BXX blends that are prepared against all No. 1 and No. 2 grade fuels allowed within Specifications D396and D975.NOTE 1Middle distillate fuels with flash points less than 38 C have been ignited by disc
4、harges of static electricity when the fuels have been filteredthrough inadequately bonded or grounded glass fiber filter systems. See Guide D4865 for a more detailed discussion of static electricity formation anddischarge.1.2 The values stated in SI units are to be regarded as standard. No other uni
5、ts of measurement are included in this standard.1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regu
6、latorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D396 Specification for Fuel OilsD975 Specification for Diesel Fuel OilsD1193 Specification for Reagent WaterD4057 Practice for Manual Sampling of Petroleum and Petroleum ProductsD4865 Guide for Generation and Dissipation of St
7、atic Electricity in Petroleum Fuel SystemsD6751 Specification for Biodiesel Fuel Blend 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 B100.3.1.
8、2 biodiesel blend, BXX, nblend of biodiesel fuel with petroleum based biodiesel fuel.3.1.3 bond, vto connect two parts of a system electrically by 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 S
9、tandard:3.2.1 filtered flushing fluids, nany of three solvents, methanol, propan-2-ol (isopropanol), or 2,2,4-trimethylpentane, filteredthrough a nominal 0.45 m 0.45 m filter.3.2.2 glass fiber filter, nglass fiber filter used in this test method.1 This test method is under the jurisdiction ofASTM Co
10、mmittee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of SubcommitteeD02.14 on Stability and Cleanliness of Liquid Fuels.Current edition approved June 1, 2014June 1, 2016. Published July 2014August 2016. Originally approved in 2008. Last previous edition ap
11、proved in 20112014 asD7321 11D7321 14.1. DOI: 10.1520/D7321-14.10.1520/D7321-16.2 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 o
12、n 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 accurately, ASTM recommends that user
13、s 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 Drive, PO Box C700, West Conshoh
14、ocken, PA 19428-2959. United States14. Summary of Test Method4.1 B100 Biodiesel Blend Stock Filtration:4.1.1 Ameasured volume of about 400 mL400 mLof biodiesel ester (B100) is vacuum filtered through one 0.7 m 0.7 m glassfiber filter. When If upon visual inspection particulate contamination is obser
15、ved, this may result in a high filtration time. In suchcases, when the contamination is high or of a nature that induces slow filtration rates, two or more filtrations using a fresh filtereach time may be required to complete filtration in a reasonable time.4.1.2 After the filtration has been comple
16、ted, the filter is washed with solvent, dried, and weighed.The particulate contaminationlevel is determined by the mass gained by the glass fiber filter, and is reported in units of grams per cubic metre or its equivalentin milligrams per litre.4.2 BXX Biodiesel Blend Filtration:4.2.1 A measured vol
17、ume of about 800 mL 800 mL of biodiesel blend (BXX) is vacuum filtered through one 0.7 m 0.7 mglass fiber filter. When If upon visual inspection particulate contamination is observed, this may result in a high filtration time. Insuch cases, when the contamination is high or of a nature that induces
18、slow filtration rates, two or more filtrations using a freshfilter each time may be required to complete filtration in a reasonable time.4.2.2 After the filtration has been completed, the filter is washed with solvent, dried, and weighed.The particulate contaminationlevel is determined by the mass g
19、ained from the glass fiber filter, and is reported in units of grams per cubic metre or its equivalentin milligrams per litre.5. Significance and Use5.1 The mass of particulates present in a fuel is a significant factor, along with the size and nature of the individual particles,in the rapidity with
20、 which fuel system filters and other small orifices in fuel systems can become plugged. This test methodprovides a means of assessing the mass of particulates present in a fuel sample.5.2 The test method can be used in specifications and purchase documents as a means of controlling particulate conta
21、minationlevels in the fuels purchased.6. Apparatus6.1 Filtration SystemArrange the following components as shown in Fig. 1.6.1.1 Funnel and Funnel Base, with filter support for a 47 mm diameter glass fiber, and locking ring or spring action clip.6.1.2 Ground/Bond Wire, 0.912 mm to 2.59 mm (No. 10 th
22、rough No. 19) bare stranded flexible, stainless steel, or copperinstalled in the flasks and grounded as shown in Fig. 1.NOTE 2The electrical bonding apparatus shown in Fig. 1 or other suitable means of electrical grounding that ensure safe operation of the filtrationapparatus and flask can be used.
23、If the filtrate is to be subsequently tested for stability, it is advisable not to use copper since copper ions catalyze gumformation during the stability test.6.1.3 Receiving Flask, 1.5 L 1.5 L or larger borosilicate glass vacuum filter flask, into which the filtration apparatus fits,equipped with
24、a sidearm to connect to the safety flask.6.1.4 Safety Flask, 1.5 L 1.5 L or larger borosilicate glass vacuum filter flask equipped with a sidearm to connect the vacuumsystem. A fuel and solvent resistance rubber hose through which the grounding wire passes shall connect the sidearm of thereceiving f
25、lask to the tube passing through the rubber stopper in the top of the safety flask.6.1.5 Vacuum System, either a water aspirated or a mechanical vacuum pump may be used if capable of producing a vacuumof 1 kPa to 100 kPa below atmospheric pressure when measured at the receiving flask.FIG. 1 Schemati
26、c of Filtration SystemD7321 1626.2 Other Apparatus:6.2.1 Air Ionizer, if used for the balance case. Air ionizers if used should be replaced annually.NOTE 3When using a solid-pan balance, the air ionizer may be omitted provided that, when weighing a glass fiber filter, it is placed on the pan sothat
27、no part protrudes over the edge of the pan.6.2.2 Analytical Balance, single- or double-pan, with the precision standard deviation of 0.07 mg or less.6.2.3 Crucible Tongs, for handling clean sample container lids.6.2.4 Drying Oven, naturally convected (without fan-assisted air circulation), controlli
28、ng to 90 C 6 5 C.6.2.5 Flushing Fluid Dispenser, an apparatus for dispensing flushing fluid through a nominal 0.45 m filter.6.2.6 Forceps, approximately 12 cm long, flat-bladed, with non-serrated, non-pointed tips.6.2.7 Graduated Cylinders, to contain at least 1 L 1 L of fluid and marked at 10 mL in
29、tervals. For samples that filter slowly,100 mL graduated cylinders may be required.6.2.8 Petri Dishes, approximately 12.5 cm in diameter, with removable glass supports for glass fiber filters.NOTE 4Small watch glasses, approximately 5 cm to 7 cm in diameter, have also been found suitable to support
30、the glass fiber filter.7. Reagents and Materials7.1 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, wheresuc
31、h specifications are available.3 Other grades may 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 Purity of WaterUnless otherwise indicated, references to water mean reagent water as defined b
32、y Types I, II and III ofSpecification D1193.7.3 Flushing Fluids:7.3.1 Methanol, (Warning Flammable).7.3.2 2,2,4-trimethylpentane (isooctane), (WarningFlammable).7.3.3 propan-2-ol (2-propanol; isopropyl alcohol), (WarningFlammable).7.4 propan-2-ol (2-propanol; isopropyl alcohol), (WarningFlammable).7
33、.4 Liquid or Powder Detergent, water-soluble, for cleaning glassware.7.5 Glass Fiber Filter, plain, with a diameter of 47 mm and a nominal pore size of 0.7 m.7.6 Protective Cover, polyethylene film or clean aluminum foil.8. Sampling8.1 Sampling for Procedure for Biodiesel Blend Stock (B100):8.1.1 Th
34、e sample container should be 500 mL 500 mL (60.015 L) in volume and have a screw-on cap with an inert liner. Glasscontainers are preferred to facilitate a visual inspection of the contents and the container before and after filling. Glass containersalso allow for visual inspection of the container,
35、after the sample is emptied, to confirm complete rinsing of the container.Epoxy-lined sample cans, polytetrafluoroethylene (PTFE) bottles, and high density linear polyethylene bottles have also beenfound suitable as sample containers, but they are less desirable since visual inspection of the interi
36、or of the container is moredifficult.8.1.1.1 It is imperative that the entire contents of the sample container are filtered during the B100 filtration. This includes notonly all of the fuel but also all rinsings of the interior of the container with flushing fluid. Because of this, take care to prot
37、ect thesample from any external contamination.8.1.2 If it is not possible to sample in a 500 mLbottle, or the sample has already been received in a 1 L1 Lbottle, follow 8.1.2.1.8.1.2.1 Vigorously shake the sample for 1 min, 1 min, and transfer 400 mL400 mLto a clean fresh 500 mL(60.015 L) 500 mL(60.
38、015 L) bottle. If a clean fresh 500 mL (60.015 L) 500 mL (60.015 L) bottle is not available, use a clean fresh 1 L 1 L(60.015 L) bottle.8.1.3 Precautions to avoid sample contamination shall include selection of an appropriate sampling point. Samples shouldpreferentially be obtained dynamically from
39、a sampling loop in a distribution line, or from the flushing line of a field samplingkit. Ensure that the line to be sampled is flushed with fuel before taking the sample.8.1.3.1 Where it is desirable or only possible to obtain samples from static storage, follow the procedures given in PracticeD405
40、7 or equivalent, taking precautions for cleanliness of all equipment used. Ensure that the sample has not passed throughintermediate containers prior to placement in the prepared container.3 Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For s
41、uggestions on the testing of reagents not listed bythe American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.D7321 163NOTE 5Samples o
42、btained from static storage may give results that are not representative of the bulk contents of the tank because of particulate mattersettling. Where possible, the contents of the tank should be circulated or agitated before sampling, or the sampling should be performed shortly after atank has been
43、 filled.8.1.4 Visually inspect the sample container before taking the samples to verify that there are no visible particles present insidethe container. Fill the sample container 90 volume %percent full, leaving space for vapor expansion. Protect the fuel sample fromprolonged exposure to light by wr
44、apping the container in aluminum foil or storing it in the dark to reduce the possibility ofparticulate formation by light-promoted reactions. Do not transfer the fuel sample from its original sample container into anintermediate storage container. If the original sample container is damaged or leak
45、ing, then a new sample must be obtained.8.1.5 Analyze fuel samples as soon as possible after sampling. When a fuel cannot be analyzed within one day, it should beblanketed with an inert gas such as oxygen-free nitrogen, argon, or helium. Store at a temperature no higher than 10 C; sampleswith cloud
46、points above 10 C may be stored at room temperature.8.2 Sampling for Procedure for Biodiesel Blends (BXX):8.2.1 The sample container for BXX shall be 1 L 1 L (60.015 L) in volume and have a screw-on cap with an inert liner. Glasscontainers are preferred to facilitate a visual inspection of the conte
47、nts and the container before and after filling. Glass containersalso allow for visual inspection of the container, after the sample is emptied, to confirm complete rinsing of the container.Epoxy-lined sample cans, polytetrafluoroethylene (PTFE) bottles, and high density linear polyethylene bottles h
48、ave also beenfound suitable as sample containers, but these are less desirable since visual inspection of the interior of the container is moredifficult.8.2.1.1 It is important to note that the entire contents of the sample container are filtered during the BXX filtration. This includesnot only all
49、of the fuel but also all rinsings of the interior of the container with flushing fluid. Because of this, take care to protectthe sample from any external contamination. The expectation is, allowing for ullage, that the volume in the 1 L sample bottle willbe 800 mL (60.015 L).800 mL (60.015 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 as described in 9.1.1 9.1.4.9.1.1 Remove any labels, tags, and so forth.9.1.2 Rinse apparatus thoroughly with propan-2-ol that
