1、Designation: D7321 16aD7321 18Standard Test Method forParticulate Contamination of Biodiesel B100 Blend StockBiodiesel Esters and Biodiesel Blends by LaboratoryFiltration1This standard is issued under the fixed designation D7321; the number immediately following the designation indicates the year of
2、original 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 of the mass of p
3、articulate 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 discharges of stati
4、c 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 units of measureme
5、nt 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 safety, health, and healthenvironmental practices and determine theapplicab
6、ility of regulatory limitations prior to use.1.4 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the Worl
7、d Trade Organization Technical Barriers to Trade (TBT) Committee.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 fo
8、r Generation and Dissipation of Static 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 o
9、r animal fats,designated B100.3.1.2 biodiesel blend, BXX, na fuel composed of biodiesel blendstock with hydrocarbon-based diesel 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, vvtto connect electrically wit
10、h earth.ground (earth).3.2 Definitions of Terms Specific to This Standard: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 filter.1 This test method is under the jurisdiction ofASTM Committee D02
11、on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of SubcommitteeD02.14 on Stability Stability, Cleanliness and CleanlinessCompatibility of Liquid Fuels.Current edition approved July 1, 2016July 1, 2018. Published August 2016August 2018. Originally approved in 2008
12、. Last previous edition approved in 2016 asD7321 16.D7321 16a. DOI: 10.1520/D7321-16A.10.1520/D7321-18.2 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 standards
13、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 accurately, AS
14、TM 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 Drive, PO
15、 Box C700, West Conshohocken, PA 19428-2959. United States13.2.2 glass fiber filter, nglass fiber filter used in this test method.4. Summary of Test Method4.1 B100 Biodiesel Blend Stock Filtration:4.1.1 Ameasured volume of 400 mLto 450 mLof biodiesel ester (B100) is vacuum filtered through one 0.7 m
16、 glass fiber filter.If upon visual inspection particulate contamination is observed, this may result in a high filtration time. In such cases, when thecontamination is high or of a nature that induces slow filtration rates, two or more filtrations using a fresh filter each time may berequired to com
17、plete filtration in a reasonable time.4.1.2 After the filtration has been completed, 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 equivalen
18、tin milligrams per litre.4.2 BXX Biodiesel Blend Filtration:4.2.1 A measured volume of 800 mL to 900 mL of biodiesel blend (BXX) is vacuum filtered through one 0.7 m glass fiberfilter. If upon visual inspection particulate contamination is observed, this may result in a high filtration time. In such
19、 cases, whenthe contamination is high or of a nature that induces slow filtration rates, two or more filtrations using a fresh filter each time maybe 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 weig
20、hed.The particulate contaminationlevel is determined by the mass gained 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 th
21、e size and nature of the individual particles,in the rapidity with 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
22、and purchase documents as a means of controlling particulate contaminationlevels 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
23、action clip.6.1.2 Ground/Bond Wire, 0.912 mm to 2.59 mm (No. 10 through 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
24、 safe operation of the filtrationapparatus and flask can be used. 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 Lor larger borosilicate glass vacuum filter fla
25、sk, into which the filtration apparatus fits, equipped witha sidearm to connect to the safety flask.6.1.4 Safety Flask, 1.5 L or larger borosilicate glass vacuum filter flask equipped with a sidearm to connect the vacuum system.Afuel and solvent resistance rubber hose through which the grounding wir
26、e passes shall connect the sidearm of the receiving flaskto the tube passing through the rubber stopper in the top of the safety flask.FIG. 1 Schematic of Filtration SystemD7321 1826.1.5 Vacuum System, either a water aspirated or a mechanical vacuum pump may be used if capable of producing a vacuumo
27、f 1 kPa to 100 kPa below atmospheric pressure when measured at the receiving flask.6.2 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
28、 glass fiber filter, it is placed on the pan sothat 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 convect
29、ed (without fan-assisted air circulation), controlling 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 cont
30、ain at least 1 Lof fluid and marked at 10 mLintervals. For samples that filter slowly, 100 mLgraduated 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 diame
31、ter, have also been found suitable to support 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 Reage
32、nts of the American Chemical Society, wheresuch 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, refer
33、ences to water mean reagent water as defined by 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 Liquid or Powder De
34、tergent, 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 The sample container sho
35、uld be 500 mL(615 mL) in volume and have a screw-on cap with an inert liner. Glass containersare preferred to facilitate a visual inspection of the contents and the container before and after filling. Glass containers also allowfor visual inspection of the container, after the sample is emptied, to
36、confirm complete rinsing of the container. Epoxy-lined samplecans, polytetrafluoroethylene (PTFE) bottles, and high density linear polyethylene bottles have also been found suitable as samplecontainers, but they are less desirable since visual inspection of the interior of the container is more diff
37、icult.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 protect thesample from any external
38、 contamination.8.1.2 If it is not possible to sample in a 500 mL bottle, or the sample has already been received in a 1 L bottle, follow 8.1.2.1.8.1.2.1 Vigorously shake the sample for 1 min, and transfer 400 mL to 450 mL (615 mL) to a clean fresh 500 mL bottle. If aclean fresh 500 mL bottle is not
39、available, use a clean fresh 1 L bottle.8.1.3 Precautions to avoid sample contamination shall include selection of an appropriate sampling point. Samples shouldpreferentially be obtained dynamically from a sampling loop in a distribution line, or from the flushing line of a field samplingkit. Ensure
40、 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 PracticeD4057 or equivalent, taking precautions for cleanliness of all equipment used. Ensure that the sampl
41、e has not passed throughintermediate containers prior to placement in the prepared container.NOTE 5Samples obtained from static storage may give results that are not representative of the bulk contents of the tank because of particulate matter3 Reagent Chemicals, American Chemical Society Specificat
42、ions, American Chemical Society, Washington, DC. For suggestions 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 Conventio
43、n, Inc. (USPC), Rockville, MD.D7321 183settling. 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 filled.8.1.4 Visually inspect the sample container before collecting the samples to verify that
44、 there are no visible particles presentinside the container. Collect 800 mL to 900 mL (615 mL), in a 1 L sample bottle or 400 mL to 500 mL (615 mL) in a 500 mL(615 mL) sample bottle and ensure that there is an ullage (vapor space) of at least 10 % of the container volume to allow for liquidexpansion
45、. Protect the fuel sample from prolonged exposure to light by wrapping the container in aluminum foil or storing it inthe dark to reduce the possibility of particulate formation by light-promoted reactions. Do not transfer the fuel sample from itsoriginal sample container into an intermediate storag
46、e container. If the original sample container is damaged or leaking, then a newsample 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.
47、 Store at a temperature no higher than 10 C; sampleswith cloud 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 (615 mL) in volume and have a screw-on cap with an inert liner. Glasscontainers are
48、 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, after the sample is emptied, to confirm complete rinsing of the container.Epoxy-lined sample cans, polytetrafluoroethylene (PTFE
49、) bottles, and high density linear polyethylene bottles have 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 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 that the v
