1、Designation: D4530 11D4530 15Standard 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 revisio
2、n. A number 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 U.S. Department of Defense.1. Scope*1.1 This test method covers the determination o
3、f the amount of carbon residue (see Note 1) formed after evaporation andpyrolysis of petroleum materials under certain conditions and is intended to provide some indication of the relative coke formingtendency of such materials.1.2 The test results are equivalent to the Conradson Carbon Residue test
4、 (see Test Method D189).NOTE 1This procedure is a modification of the original method and apparatus for carbon residue of petroleum materials, where it has beendemonstrated that thermogravimetry is another applicable technique.2 However, it is the responsibility of the operator to establish operatin
5、g conditionsto obtain equivalent results when using thermogravimetry.1.3 This test method is applicable to petroleum products that partially decompose on distillation at atmospheric pressure andwas tested for carbon residue values of 0.100.10 % to 30 % (m(m/m).m). Samples expected to be below 0.10 w
6、eight %(m/m)(mm) residue should be distilled to remove 90 % (V/V) of the flask charge (see Section 9). The 10 % bottoms remainingis then tested for carbon residue by this test method.1.4 Ash-forming constituents, as defined by Test Method D482, or non-volatile additives present in the sample will ad
7、d to thecarbon residue value and be included as part of the total carbon residue value reported.1.5 Also in diesel fuel, the presence of alkyl nitrates, such as amyl nitrate, hexyl nitrate, or octyl nitrate, causes a higher carbonresidue value than observed in untreated fuel, which may lead to erron
8、eous conclusions as to the coke-forming propensity of thefuel. The presence of alkyl nitrate in the fuel may be detected by Test Method D4046.1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.6.1 Exception6.4 and 6.5 inclu
9、de inch-pound units.1.7 WARNINGMercury has been designated by many regulatory agencies as a hazardous material that can cause centralnervous system, kidney and liver damage. Mercury, or its vapor, may be hazardous to health and corrosive to materials. Cautionshould be taken when handling mercury and
10、 mercury containing products. See the applicable product Material Safety Data Sheet(MSDS) for details and EPAs websitehttp:/www.epa.gov/mercury/faq.htmfor additional information. Users should be awarethat selling mercury and/or mercury containing products into your state or country may be prohibited
11、 by law.1.8 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 practices and to determine the applicability of regulatory limitationsprior to use. For specific war
12、ning statements, see 8.2.3 and 8.4.2. Referenced Documents2.1 ASTM Standards:3D189 Test Method for Conradson Carbon Residue of Petroleum ProductsD482 Test Method for Ash from Petroleum ProductsD4046 Test Method for Alkyl Nitrate in Diesel Fuels by SpectrophotometryD4057 Practice for Manual Sampling
13、of Petroleum and Petroleum Products1 This test method is under the jurisdiction ofASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of SubcommitteeD02.06 on Analysis of Liquid Fuels and Lubricants.Current edition approved May 15, 2011June 1, 2015
14、. Published July 2011 June 2015. Originally approved in 1985. Last previous edition approved in 20072011 asD4530D4530 11.07. DOI: 10.1520/D4530-11.10.1520/D4530-115.2 See Fuel, Vol 63, July 1984, pp. 931934.3 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer
15、Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards 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 pre
16、vious version. Becauseit may not be technically possible to adequately depict all changes accurately, 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 Ch
17、anges section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1D4177 Practice for Automatic Sampling of Petroleum and Petroleum ProductsE1 Specification for ASTM Liquid-in-Glass ThermometersE133 Speci
18、fication for Distillation Equipment2.2 Energy Institute Standard:Specification for IP Standard Thermometers43. Terminology3.1 Definitions:3.1.1 carbon residue, nthe residue formed by evaporation and thermal degradation of a carbon containing material.3.1.1.1 DiscussionThe residue is not composed ent
19、irely of carbon but is a coke that can be further changed by carbon pyrolysis.4. Summary of Test Method4.1 A weighed quantity of sample is placed in a glass vial and heated to 500C500 C under an inert (nitrogen) atmosphere ina controlled manner for a specific time. The sample undergoes coking reacti
20、ons, and volatiles formed are swept away by thenitrogen. The carbonaceous-type residue remaining is reported as 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/V)V)bottoms
21、, prior to performing the test.5. Significance and Use5.1 The carbon residue value of the various petroleum materials serves as an approximation of the tendency of the material toform carbonaceous type deposits under degradation conditions similar to those used in the test method, and can be useful
22、as a guidein manufacture of certain stocks. However, care needs to be exercised in interpreting the results.5.2 This test method offers advantages of better control of test conditions, smaller samples, and less operator attention comparedto Test Method D189, to which it is equivalent.4 “Methods for
23、Analysis and Testing,” Institute of Petroleum Standard Methods for Petroleum and Its Products, Part I, Vol 2. Available from Energy Institute, 61 NewCavendish St., London, WIM 8AR, UK.FIG. 1 Sample Vial Holder and VialD4530 1525.3 Up to twelve samples may be run simultaneously, including a control s
24、ample when the vial holder shown in Fig. 1 is usedexclusively for sample analysis.6. Apparatus6.1 Glass Sample Vials, 2-mL2 mL capacity, 12-mm12 mm outside diameter by approximately 35-mm35 mm high.6.2 Larger 4-dram Glass Sample Vials, 15-mL15 mL capacity (20.5(20.5 mm to 21-mm21 mm outside diameter
25、 by 7070 mm6 1-mm1 mm high), may be used for samples that are expected to yield residues 5 0.15 0.05Brown, viscous 15 0.5 0.1Lube oil consistency andappearance, 10 % bottoms ondistillate material0.11 1.5 0.5Large vials only 0.1 5.0 1.0Small vials only 0.1 1.5 0.5D4530 154can be started when the oven
26、 has been cooled to below 100C.100 C.8.3 Final WeighingTransfer sample vials (maintained in place in the vial holder) to desiccator and allow vials to cool to roomtemperature. Weigh the cooled vials to the nearest 0.1 mg 0.1 mg and record. Handle the vials with forceps. Discard the used glasssample
27、vials.8.4 Occasionally examine the condensate trap at the bottom of the oven chamber; empty if necessary and replace.(WarningThe condensate trap residue may have some carcinogenic materials present. Avoid contact with the trap residue;dispose of it in accordance with local laboratory practice.)9. Pr
28、ocedure for Carbon Residue on 10 % (V/V) Distillation Residue9.1 This procedure is applicable to light distillate materials, such as ASTM No. 1 and No. 2 fuel oil or materials expected tohave less than 0.1 % (m/m) carbon residue.9.2 Adistillation analysis using either a 100100 mLor 200-mL200 mLstart
29、ing volume is required in order to collect a sufficientamount of the 10 % (V/V) residue needed in this analysis. For a 100-mL100 mL distillation, assemble the distillation apparatusdescribed in Specification E133, using flask B (125-mL(125 mL bulb volume), flask support board with 50-mm50 mm diamete
30、ropening, and graduated cylinder B (100-mL(100 mL capacity). For a 200-mL200 mL distillation, assemble the distillationapparatus described in Specification E133, using flask D (250-mL(250 mL bulb volume), flask support board with 50-mm50 mmdiameter opening, and graduated cylinder C (200-mL(200 mL ca
31、pacity). A thermometer is not required, but the use of the ASTMHigh Distillation Thermometer 8F or 8C, as prescribed in Specification E1, or the IP High Distillation Thermometer 6C, asprescribed in the Specification for IP Thermometers, is recommended.9.3 Depending upon which distillation flask is u
32、sed, place either 100100 mL or 200 mL 200 mL of sample (as measured atambient temperature) into a tared distillation flask that is held at a temperature between 13C13 C and ambient. Maintain thecondenser bath temperature between 00 C and 60C60 C so as to provide a sufficient temperature differential
33、 for samplecondensation, while avoiding any solidification of waxy material in the condenser tube. Use, without cleaning, the cylinder fromwhich the sample was measured as the receiver, and place it so that the tip of the condenser does not touch the wall of the cylinder.The receiver temperature is
34、required to be maintained at the same temperature (within 63C)63 C) as the sample taken at thestart of the test in order to obtain an accurate volume measurement in the receiving flask.9.4 Apply the heat to the flask at a uniform rate so regulated that the first drop of condensate exits from the con
35、denser between1010 min and 15 min 15 min (for 200-mL200 mL samples) or between 55 min and 15 min 15 min (for 100-mL100 mL samples)after initial application of heat. After If performing a manual distillation, after the first drop falls, move the receiving cylinder sothat the tip of the condenser tube
36、 touches the wall of the cylinder. Then regulate the heat so that the distillation proceeds at auniform rate of 88 mLmin to 1010 mL mL/min min (for 200-mL200 mL samples) or 44 mLmin to 55 mL mL/min min (for100-mL100 mL samples). For 200-mL200 mL samples, continue the distillation until approximately
37、 178 mL 178 mL of distillatehas been collected, and then discontinue heating and allow the condenser to drain until 180 mL 180 mL (90 % (V/V)(VV) of thecharge to the flask) has been collected in the cylinder. For 100-mL100 mL samples, continue the distillation until approximately88 mL 88 mL of disti
38、llate has been collected, and then discontinue heating and allow the condenser to drain until 90 mL 90 mL(90 % (V/V)(VV) of the charge to the flask) has been collected in the cylinder.FIG. 3 Carbon Residue (Micro) Precision DataD4530 1559.5 Catch final drainage, if any, by immediately replacing the
39、cylinder with a suitable container, such as a small Erlenmeyerflask. Add to this container, while still warm, the distillation residue left in the distilling flask, and mix well. The contents of thecontainer then represents a 10 % (V/V) distillation residue from the original product.9.6 If the disti
40、llation residue is too viscous to flow freely at ambient temperature, it is necessary to warm the distillation residueto a sufficient temperature that will allow a portion of the material to be transferred into a previously weighted vial for analysis(see Table 1). After allowing the material in the
41、vial to cool to ambient temperature, determine the mass of the test specimen tothe nearest 0.1 mg 0.1 mg and carry out the carbon residue test in accordance with the procedure described in Section 8.10. Calculation10.1 Calculate the mass % carbon residue in the original sample, or in the 10 % distil
42、lation bottoms as follows:10.1.1 Calculate percent residue as follows:%carbon residue5A 3100!W (1)where:A = carbon residue, g, andW = sample used, g.11. Report11.1 For values up to 10 %, report the value obtained as Micro Method carbon residue, percent to the nearest 0.01 % (m/m).For values above 10
43、 %, report the value obtained to the nearest 0.1% (m/m). For Micro Method carbon residue on 10 % distillationresidue, percent to the nearest 0.1 % (m/m).12. Precision and Bias512.1 The precision of this test method as determined by (see Note 5) statistical examination of interlaboratory results is a
44、sfollows:NOTE 5Precision data were generated by a task force in 2004. The round robin involved nine laboratories and six petroleum materials in duplicateanalysis. The range for values samples was from 0.1 % to 25 % (m/m). No precision data or correlation data exists for results obtained using 10 % b
45、ottomsor 15-mL15 mL vials, or both. See X1.1 and Fig. X1.1 regarding a separate 1983 correlation study6 that was performed between Test Methods D189 andD4530.12.2 RepeatabilityThe difference between two test results, obtained by the same operator with the same apparatus underconstant operating condi
46、tions on identical test material, would, in the long run, in the normal and correct operation of the testmethod, exceed the values shown in Fig. 3 in only one case in twenty.12.3 ReproducibilityThe difference between two single and independent results, obtained by different operators working indiffe
47、rent laboratories on identical test material, would, in the long run, in the normal and correct operation of the test method,exceed the values shown in Fig. 3 in only one case in twenty.12.4 BiasThe procedure in Test Method D4530 for measuring carbon residue of petroleum by the carbon residue method
48、 hasno bias because the mass % of carbon residue can be defined only in terms of the test method.13. Keywords13.1 carbon residue; carbon residue (micro method); diesel fuel; lubricating oil; petroleum productsAPPENDIXES(Nonmandatory Information)X1. CORRELATION TO OTHER METHODSX1.1 A correlation (see
49、 Fig. X1.1) has been derived between the carbon residue test by the micro method and the Conradsoncarbon residue test (see Test Method D189) in a cooperative program involving 18 laboratories and six petroleum materials.5 Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D02-1589.6 Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D02-1192.D4530 156X1.2 Statistical analysis using modified
