ASTM D4530-2007 Standard Test Method for Determination of Carbon Residue (Micro Method)《碳残留物的测定用标准试验方法(微量法)》.pdf
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1、Designation: D 4530 07An American National StandardStandard Test Method forDetermination of Carbon Residue (Micro Method)1This standard is issued under the fixed designation D 4530; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, t
2、he year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) 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
3、the determination of the amountof 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 Ca
4、rbonResidue test (see Test Method D 189).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 est
5、ablish operatingconditions to obtain 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
6、 weight % (m/m) residueshould be 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 MethodD 482, or non-volatile additives present in the sample will addto
7、 the carbon residue value and be included 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 c
8、onclusions as to the coke-formingpropensity of the fuel. The presence of alkyl nitrate in the fuelmay be detected by Test Method D 4046.1.6 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.7 This standard does not purport to a
9、ddress 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. Referenced
10、 Documents2.1 ASTM Standards:3D 189 Test Method for Conradson Carbon Residue ofPetroleum ProductsD 482 Test Method for Ash from Petroleum ProductsD 4046 Test Method for Alkyl Nitrate in Diesel Fuels bySpectrophotometryD 4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD 4177 Pract
11、ice for Automatic Sampling of Petroleum andPetroleum ProductsE1 Specification for ASTM Liquid-in-Glass ThermometersE 133 Specification for Distillation Equipment2.2 Energy Institute Standard:Specification for IP Standard Thermometers43. Terminology3.1 Definitions:3.1.1 carbon residue, nin petroleum
12、products, the partremaining after a sample has been subjected to thermaldecomposition.3.1.1.1 DiscussionThe amount of residue is dependent onthe test conditions of evaporation and pyrolysis. The term maybe misleading here in that the residue may contain other thancarbon decomposition products. Howev
13、er, the term is retaineddue to its wide common usage.4. 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 sw
14、ept away by the1This 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 Nov. 1, 2007. Published December 2007. Originallyapproved in 1985. Last previ
15、ous edition approved in 2006 as D 453006e1.2See 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 ASTMStandards volume information, refer to the standards Document Summary p
16、age onthe ASTM website.4“Methods for Analysis 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 Summary of Changes section appears at the end of this standard.Copyright AST
17、M International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.Copyright by ASTM Intl (all rights reserved); Mon Apr 21 02:18:11 EDT 2008Downloaded/printed byGuo Dehua (CNIS) pursuant to License Agreement. No further reproductions authorized.nitrogen. The carbon
18、aceous-type residue 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 resi
19、due value of the various 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 exerci
20、sed in interpreting the results.5.2 This test method offers advantages of better control oftest conditions, smaller samples, and less operator attentioncompared to Test Method D 189, to which it is equivalent.5.3 Up to twelve samples may be run simultaneously,including a control sample when the vial
21、 holder shown in Fig.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
22、expected to yield residues 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 0.5D4530073Copyright by ASTM Intl (all rights reserved); Mon Apr 21 02:18:11 EDT 2008Downloa
23、ded/printed byGuo Dehua (CNIS) pursuant to License Agreement. No further reproductions authorized.results that are outside these limits indicate problems with the procedureor the equipment.8.2 Processing of Samples:8.2.1 With the oven at less than 100C, place the vial holderinto the oven chamber and
24、 secure lid. Purge with nitrogen forat least 10 min at 600 mL/min. Then decrease the purge to 150mL/min and heat the oven slowly to 500C at 1015C/min.8.2.2 If the sample foams or spatters, causing loss ofsample, discard and repeat the test.NOTE 3Spattering may be due to water that can be removed by
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