ASTM D4530-2011 Standard Test Method for Determination of Carbon Residue (Micro Method)《测定碳残余物的标准试验方法(微量法)》.pdf
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1、Designation: D4530 11Standard Test Method forDetermination of Carbon Residue (Micro Method)1This standard is issued under the fixed designation D4530; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A num
2、ber in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1. Scope*1.1 This test method covers the determination of the amounto
3、f carbon residue (see Note 1) formed after evaporation andpyrolysis of petroleum materials under certain conditions andis intended to provide some indication of the relative cokeforming tendency of such materials.1.2 The test results are equivalent to the Conradson CarbonResidue test (see Test Metho
4、d D189).NOTE 1This procedure is a modification of the original method andapparatus for carbon residue of petroleum materials, where it has beendemonstrated that thermogravimetry is another applicable technique.2However, it is the responsibility of the operator to establish operatingconditions to obt
5、ain equivalent results when using thermogravimetry.1.3 This test method is applicable to petroleum products thatpartially decompose on distillation at atmospheric pressure andwas tested for carbon residue values of 0.10 to 30 % (m/m).Samples expected to be below 0.10 weight % (m/m) residueshould be
6、distilled to remove 90 % (V/V) of the flask charge(see Section 9). The 10 % bottoms remaining is then tested forcarbon residue by this test method.1.4 Ash-forming constituents, as defined by Test MethodD482, or non-volatile additives present in the sample will addto the carbon residue value and be i
7、ncluded as part of the totalcarbon residue value reported.1.5 Also in diesel fuel, the presence of alkyl nitrates, such asamyl nitrate, hexyl nitrate, or octyl nitrate, causes a highercarbon residue value than observed in untreated fuel, whichmay lead to erroneous conclusions as to the coke-formingp
8、ropensity of the fuel. The presence of alkyl nitrate in the fuelmay be detected by Test Method D4046.1.6 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.6.1 Exception6.4 and 6.5 include inch-pound units.1.7 WARNINGMercury has
9、been designated by manyregulatory agencies as a hazardous material that can causecentral nervous system, kidney and liver damage. Mercury, orits vapor, may be hazardous to health and corrosive tomaterials. Caution should be taken when handling mercury andmercury containing products. See the applicab
10、le product Ma-terial Safety Data Sheet (MSDS) for details and EPAswebsitehttp:/www.epa.gov/mercury/faq.htmfor addi-tional information. Users should be aware that selling mercuryand/or mercury containing products into your state or countrymay be prohibited by law.1.8 This standard does not purport to
11、 address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety practices and to determine the applicability ofregulatory limitations prior to use. For specific warningstatements, see 8.2.3 and 8.4.2. Referenc
12、ed Documents2.1 ASTM Standards:3D189 Test Method for Conradson Carbon Residue of Pe-troleum ProductsD482 Test Method for Ash from Petroleum ProductsD4046 Test Method for Alkyl Nitrate in Diesel Fuels bySpectrophotometryD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practi
13、ce for Automatic Sampling of Petroleum andPetroleum ProductsE1 Specification for ASTM Liquid-in-Glass ThermometersE133 Specification for Distillation Equipment2.2 Energy Institute Standard:Specification for IP Standard Thermometers43. Terminology3.1 Definitions:3.1.1 carbon residue, nthe residue for
14、med by evaporationand thermal degradation of a carbon containing material.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.06 on Analysis of Lubricants.Current edition approved May 15, 2011. Publ
15、ished July 2011. Originallyapproved in 1985. Last previous edition approved in 2007 as D453007. DOI:10.1520/D4530-11.2See Fuel, Vol 63, July 1984, pp. 931934.3For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of A
16、STMStandards volume information, refer to the standards Document Summary page onthe ASTM website.4“Methods forAnalysis and Testing,” Institute of Petroleum Standard Methodsfor Petroleum and Its Products, Part I, Vol 2. Available from Energy Institute, 61New Cavendish St., London, WIM 8AR, UK.1*A Sum
17、mary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3.1.1.1 DiscussionThe residue is not composed entirelyof carbon but is a coke that can be further changed by carbonpyrolysis.4
18、. Summary of Test Method4.1 A weighed quantity of sample is placed in a glass vialand heated to 500C under an inert (nitrogen) atmosphere in acontrolled manner for a specific time. The sample undergoescoking reactions, and volatiles formed are swept away by thenitrogen. The carbonaceous-type residue
19、 remaining is reportedas a percent of the original sample as “carbon residue (micro).”4.1.1 When the test result is expected to be below 0.10 %(m/m), the sample can be distilled to produce a 10 % (V/V)bottoms, prior to performing the test.5. Significance and Use5.1 The carbon residue value of the va
20、rious petroleummaterials serves as an approximation of the tendency of thematerial to form carbonaceous type deposits under degradationconditions similar to those used in the test method, and can beuseful as a guide in manufacture of certain stocks. However,care needs to be exercised in interpreting
21、 the results.5.2 This test method offers advantages of better control oftest conditions, smaller samples, and less operator attentioncompared to Test Method D189, to which it is equivalent.5.3 Up to twelve samples may be run simultaneously,including a control sample when the vial holder shown in Fig
22、.1 is used exclusively for sample analysis.6. Apparatus6.1 Glass Sample Vials, 2-mL capacity, 12-mm outsidediameter by approximately 35-mm high.6.2 Larger 4-dram Glass Sample Vials, 15-mL capacity(20.5 to 21-mm outside diameter by 70 6 1-mm high), may beused for samples that are expected to yield re
23、sidues 5 0.15 6 0.05Brown, viscous 15 0.5 6 0.1Lube oil consistency andappearance, 10 % bottoms ondistillate material0.11 1.5 6 0.5Large vials only 0.1 5.0 6 1.0Small vials only 0.1 1.5 6 0.5D4530 113record. Place the loaded sample vials into vial holder (up totwelve), noting position of each sample
24、 with respect to indexmark.NOTE 2A control sample can be included in each batch of samplesbeing tested. This control sample should be a typical sample that has beentested at least 20 times in the same equipment in order to define an averagepercent carbon residue and standard deviation. Results for e
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