1、Designation: D7321 16D7321 16aStandard 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 and health practices and determine the applicability of regulatorylimitatio
6、ns 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 Static Electricit
7、y 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 B100.3.1.2 biodiesel ble
8、nd, BXX, nblend a fuel composed of biodiesel fuel with petroleum based biodiesel blendstock withhydrocarbon-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, vto connect electrically with earth.3.
9、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.3.2.2 glass fiber filter, nglass fiber filter used in this test method.1 This test method i
10、s under the jurisdiction ofASTM Committee 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, 2016July 1, 2016. Published August 2016. Originally approved in 2008.
11、 Last previous edition approved in 20142016 asD7321 14.D7321 16. DOI: 10.1520/D7321-16.10.1520/D7321-16A.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 standard
12、s 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,
13、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 Drive,
14、PO Box C700, West Conshohocken, PA 19428-2959. United States14. Summary of Test Method4.1 B100 Biodiesel Blend Stock Filtration:4.1.1 Ameasured volume of about 400 mLto 450 mLof biodiesel ester (B100) is vacuum filtered through one 0.7 m glass fiberfilter. If upon visual inspection particulate conta
15、mination is observed, this may result in a high filtration time. In such 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.4.1.2 After the filtratio
16、n 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 equivalentin milligrams per litre.4.2 BXX Biodiesel Blend Filtration:4.2
17、.1 A measured volume of about 800 mL to 900 mL of biodiesel blend (BXX) is vacuum filtered through one 0.7 m glassfiber filter. If upon visual inspection particulate contamination is observed, this may result in a high filtration time. In such cases,when the contamination is high or of a nature that
18、 induces slow filtration rates, two or more filtrations using a fresh filter each timemay 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 t
19、he 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 the size and nature of the individual particles,in the rapi
20、dity 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 and purchase documents as a means of controlling particul
21、ate 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 action clip.6.1.2 Ground/Bond Wire, 0.912 mm to 2.59 mm (
22、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 safe operation of the filtrationapparatus and flask can
23、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 flask, into which the filtration apparatus fits, equipped wi
24、tha 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 wire passes shall connect the sidearm of the receiving flask
25、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 Schematic of
26、Filtration SystemD7321 16a26.2 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 no p
27、art 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), controlling t
28、o 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 Lof fluid and marked at 10 mLintervals. F
29、or 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 diameter, have also been found suitable to support the glass
30、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, wheresuch specific
31、ations 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 by Types I,
32、 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 Detergent, water-soluble, for cleaning glassware.7.5 Glass
33、 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 should be 500 mL (60.015 L)(615 mL) in volume and have a sc
34、rew-on cap with an inert liner.Glass containers are preferred to facilitate a visual inspection of the contents and the container before and after filling. Glasscontainers also allow for visual inspection of the container, after the sample is emptied, to confirm complete rinsing of thecontainer. Epo
35、xy-lined sample cans, polytetrafluoroethylene (PTFE) bottles, and high density linear polyethylene bottles have alsobeen found suitable as sample containers, but they are less desirable since visual inspection of the interior of the container is moredifficult.8.1.1.1 It is imperative that the entire
36、 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 contamination.8.1.2 If it is not possible to
37、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 (60.015 L)bottle. If a clean fresh 500 mL (60.015 L) bottle is not available, use a clean f
38、resh 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 a sampling loop in a distribution line, or from the flushing line of a field samplingkit. Ensure that the lin
39、e 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 sample has not pas
40、sed 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 mattersettling. Where possible, the contents of the tank should be circulate
41、d or agitated before sampling, or the sampling should be performed shortly after atank has been filled.3 Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed bythe American Chemical Society, see
42、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 16a38.1.4 Visually inspect the sample container before takingcollecting the samples to verify that there
43、 are no visible particlespresent inside the container. Fill the sample container 90 volume percent full, leaving space for vaporCollect 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 isan ullage (vapor space) of
44、at least 10 % of the container volume to allow for liquid expansion. Protect the fuel sample fromprolonged exposure to light by wrapping 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 sa
45、mple from its original sample container into anintermediate storage container. If the original sample container is damaged or leaking, 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 beblankete
46、d with an inert gas such as oxygen-free nitrogen, argon, or helium. 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 (60.015 L)(615 m
47、L) in volume and have a screw-on cap with an inert liner.Glass containers are preferred to facilitate a visual inspection of the contents and the container before and after filling. Glasscontainers also allow for visual inspection of the container, after the sample is emptied, to confirm complete ri
48、nsing of thecontainer. Epoxy-lined sample cans, polytetrafluoroethylene (PTFE) bottles, and high density linear polyethylene bottles have alsobeen found 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
49、 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, allowing for ullage, is that the volume in the 1 L sample bottlewill be 800 mL (60.015 L).to 900 mL, allowing for 10 % ullage.8.2.2 Follow 8.1.3 8.1.5.9. Preparation of Apparatus and Sample Containers9.1 Clean all components of the
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