1、Designation: D 189 06Designation: 13/94An American National StandardBritish Standard 4380Standard Test Method forConradson Carbon Residue of Petroleum Products1This standard is issued under the fixed designation D 189; the number immediately following the designation indicates the year oforiginal ad
2、option or, in the case of revision, the 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.
3、1. Scope*1.1 This test method covers the determination of the amountof carbon residue (Note 1) left after evaporation and pyrolysisof an oil, and is intended to provide some indication of relativecoke-forming propensities. This test method is generally ap-plicable to relatively nonvolatile petroleum
4、 products whichpartially decompose on distillation at atmospheric pressure.Petroleum products containing ash-forming constituents asdetermined by Test Method D 482 or IP Method 4 will have anerroneously high carbon residue, depending upon the amountof ash formed (Note 2 and Note 4).NOTE 1The term ca
5、rbon residue is used throughout this test methodto designate the carbonaceous residue formed after evaporation andpyrolysis of a petroleum product under the conditions specified in this testmethod. The residue is not composed entirely of carbon, but is a cokewhich can be further changed by pyrolysis
6、. The term carbon residue iscontinued in this test method only in deference to its wide common usage.NOTE 2Values obtained by this test method are not numerically thesame as those obtained by Test Method D 524. Approximate correlationshave been derived (see Fig. X1.1), but need not apply to all mate
7、rialswhich can be tested because the carbon residue test is applied to a widevariety of petroleum products.NOTE 3The test results are equivalent to Test Method D 4530, (seeFig. X1.2).NOTE 4In diesel fuel, the presence of alkyl nitrates such as amylnitrate, hexyl nitrate, or octyl nitrate causes a hi
8、gher residue value thanobserved in untreated fuel, which can lead to erroneous conclusions as tothe coke forming propensity of the fuel. The presence of alkyl nitrate inthe fuel can be detected by Test Method D 4046.1.2 The values stated in SI units are to be regarded as thestandard. The values give
9、n in parentheses are for informationonly.1.3 This standard does not purport to 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 and health practices and determine the applica-bility of regulatory
10、 limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 482 Test Method for Ash from Petroleum ProductsD 524 Test Method for Ramsbottom Carbon Residue ofPetroleum ProductsD 4046 Test Method for Alkyl Nitrate in Diesel Fuels bySpectrophotometryD 4057 Practice for Manual Sampling of Pet
11、roleum andPetroleum ProductsD 4175 Terminology Relating to Petroleum, PetroleumProducts, and LubricantsD 4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD 4530 Test Method for Determination of Carbon Residue(Micro Method)E1 Specification for ASTM Liquid-in-Glass ThermometersE
12、133 Specification for Distillation Equipment3. Terminology3.1 Definitions:3.1.1 carbon residue, nthe residue formed by evaporationand thermal degradation of a carbon containing material.3.1.2 DiscussionThe residue is not composed entirely ofcarbon but is a coke that can be further changed by carbon1
13、This 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, 2006. Published December 2006. Originallyapproved in 1924. Last previous edition appr
14、oved in 2005 as D 189-05.In the IP, this test method is under the jurisdiction of the StandardizationCommittee and is issued under the fixed designation IP 13. The final numberindicates the year of last revision. This test method was adopted as a jointASTMIPstandard in 1964.This procedure is a modif
15、ication of the original Conradson method and apparatusfor Carbon Test and Ash Residue in Petroleum Lubricating Oils. See Proceedings,Eighth International Congress of Applied Chemistry, New York, Vol 1, p. 131,September 1912; also Journal of Industrial and Engineering Chemistry, IECHA,Vol 4, No. 11,
16、December 1912.In 1965, a new Fig. 2 on reproducibility and repeatability combining ASTM andIP precision data replaced old Fig. 2 and Note 4.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volum
17、e information, refer to the standards Document Summary page onthe ASTM website.1*A Summary 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.pyrolysis. The term carbon residue is re
18、tained in deference toits wide common usage. D 41754. Summary of Test Method4.1 Aweighed quantity of sample is placed in a crucible andsubjected to destructive distillation. The residue undergoescracking and coking reactions during a fixed period of severeheating. At the end of the specified heating
19、 period, the testcrucible containing the carbonaceous residue is cooled in adesiccator and weighed. The residue remaining is calculated asa percentage of the original sample, and reported as Conradsoncarbon residue.5. Significance and Use5.1 The carbon residue value of burner fuel serves as arough a
20、pproximation of the tendency of the fuel to formdeposits in vaporizing pot-type and sleeve-type burners. Simi-larly, provided alkyl nitrates are absent (or if present, providedthe test is performed on the base fuel without additive) thecarbon residue of diesel fuel correlates approximately withcombu
21、stion chamber deposits.5.2 The carbon residue value of motor oil, while at one timeregarded as indicative of the amount of carbonaceous depositsa motor oil would form in the combustion chamber of anengine, is now considered to be of doubtful significance due tothe presence of additives in many oils.
22、 For example, anash-forming detergent additive may increase the carbon residuevalue of an oil yet will generally reduce its tendency to formdeposits.5.3 The carbon residue value of gas oil is useful as a guidein the manufacture of gas from gas oil, while carbon residuevalues of crude oil residuums,
23、cylinder and bright stocks, areuseful in the manufacture of lubricants.6. Apparatus (see Fig. 1)6.1 Porcelain Crucible, wide form, glazed throughout, or asilica crucible; 29- to 31-mL capacity, 46 to 49 mm in rimdiameter.6.2 Iron Crucible Skidmore iron crucible, flanged andringed, 65- to 82-mL capac
24、ity, 53 to 57 mm inside and 60- to67-mm outside diameter of flange, 37 to 39 mm in heightsupplied with a cover without delivery tubes and having thevertical opening closed. The horizontal opening of about 6.5mm shall be kept clean. The outside diameter of the flat bottomshall be 30 to 32 mm.FIG. 1 A
25、pparatus for Determining Conradson Carbon ResidueD1890626.3 Iron Crucible Spun sheet-iron crucible with cover; 78to 82 mm in outside diameter at the top, 58 to 60 mm in height,and approximately 0.8 mm in thickness. Place at the bottom ofthis crucible, and level before each test, a layer of about 25
26、mLof dry sand, or enough to bring the Skidmore crucible, withcover on, nearly to the top of the sheet-iron crucible.6.4 Wire Support Triangle of bare Nichrome wire ofapproximately No. 13B provided at the top with a chimney 50 to 60 mmin height and 50 to 56 mm in inside diameter, which is attachedto
27、the lower part having the perpendicular sides by a cone-shaped member, bringing the total height of the complete hoodto 125 to 130 mm. The hood can be made from a single pieceof metal, provided it conforms to the foregoing dimensions. Asa guide for the height of the flame above the chimney, a bridge
28、made of approximately 3-mm iron or Nichrome wire, andhaving a height of 50 mm above the top of the chimney, shallbe attached.6.6 InsulatorHeat-resistant block, refractory ring, or hol-low sheet-metal box, 150 to 175 mm in diameter if round, or ona side if square, 32 to 38 mm in thickness, provided w
29、ith ametal-lined, inverted cone-shaped opening through the center;83 mm in diameter at the bottom, and 89 mm in diameter at thetop. In the case of the refractory ring no metal lining isnecessary, providing the ring is of hard, heat-resistant material.NOTE 5It is not know what type of insulators were
30、 used in the roundrobin conducted for obtaining the precision given in Section 13.6.7 Burner, Meker type, having an orifice approximately 24mm in diameter.7. Sampling7.1 For sampling techniques see Practices D 4057 andD 4177.8. Procedure8.1 Shake thoroughly the sample to be tested, first heating to5
31、0 6 10C for 0.5 h when necessary to reduce its viscosity.Immediately following the heating and shaking, filter testportion through a 100 mesh screen. Weigh to the nearest 5 mga 10-g sample of the oil to be tested, free of moisture and othersuspended matter, into a tared porcelain or silica cruciblec
32、ontaining two glass beads about 2.5 mm in diameter. Placethis crucible in the center of the Skidmore crucible. Level thesand in the large sheet-iron crucible and set the Skidmorecrucible on it in the exact center of the iron crucible. Applycovers to both the Skidmore and the iron crucible, the one o
33、nthe latter fitting loosely to allow free exit to the vapors asformed.8.2 On a suitable stand or ring, place the bare Nichromewire triangle and on it the insulator. Next center the sheet-ironcrucible in the insulator with its bottom resting on top of thetriangle, and cover the whole with the sheet-i
34、ron hood in orderto distribute the heat uniformly during the process (see Fig. 1).8.3 Apply heat with a high, strong flame from the Meker-type gas burner, so that the pre-ignition period will be 10 6 1.5min (a shorter time can start the distillation so rapidly as tocause foaming or too high a flame)
35、. When smoke appearsabove the chimney, immediately move or tilt the burner so thatthe gas flame plays on the sides of the crucible for the purposeof igniting the vapors. Then remove the heat temporarily, andbefore replacing adjust by screwing down the pinch-cock onthe gas tubing so that the ignited
36、vapors burn uniformly withthe flame above the chimney but not above the wire bridge.Heat can be increased, if necessary, when the flame does notshow above the chimney. The period of burning the vaporsshall be 13 6 1 min. If it is found impossible to meet therequirements for both flame and burning ti
37、me, the requirementfor burning time is the more important.8.4 When the vapors cease to burn and no further bluesmoke can be observed, readjust the burner and hold the heatas at the beginning so as to make the bottom and lower part ofthe sheet-iron crucible a cherry red, and maintain for exactly 7min
38、. The total period of heating shall be 30 6 2 min, whichconstitutes an additional limitation on the tolerances for thepre-ignition and burning periods. There should be no difficultyin carrying out the test exactly as directed with the gas burnerof the type named, using city gas (20 to 40 MJ/m3), wit
39、h thetop of the burner about 50 mm below the bottom of thecrucible. The time periods shall be observed with whateverburner and gas is used.8.5 Remove the burner and allow the apparatus to cool untilno smoke appears, and then remove the cover of the Skidmorecrucible (about 15 min). Remove the porcela
40、in or silicacrucible with heated tongs, place in the desiccator, cool, andweigh. Calculate the percentage of carbon residue on theoriginal sample.9. Procedure for Residues Exceeding 5 %9.1 This procedure is applicable to such materials as heavycrude oils, residuums, heavy fuel oils, and heavy gas oi
41、ls.9.2 When the carbon residue as obtained by the proceduredescribed in Section 8 (using a 10-g sample) is in excess of5 %, difficulties can be experienced due to boiling over of thesample. Trouble also can be encountered with samples ofheavy products which are difficult to dehydrate.9.3 For samples
42、 showing more than 5.0 and less than 15.0 %carbon residue by the procedure described in Section 8, repeatthe test using a 5 6 0.5 g sample weighed to the nearest 5 mg.In event that a result greater than 15.0 % is obtained, repeat thetest, reducing the sample size to 3 6 0.1 g, weighed to thenearest
43、5 mg.9.4 If the sample boils over, reduce the sample size first to5 g and then to3gasnecessary to avoid the difficulty.9.5 When the 3-g sample is used, it can be impossible tocontrol the preignition and vapor burning times within thelimits specified in 8.3. However, in such cases, the results shallb
44、e considered as valid.10. Procedure for Carbon Residue on 10 % DistillationResidue10.1 This procedure is applicable to light distillate oils, suchas ASTM No. 1 and No. 2 fuel oils.D18906310.2 Assemble the distillation apparatus described in Speci-fication E 133 using flask D (250-mL bulb volume), fl
45、asksupport board with 50-mm diameter opening, and graduatedcylinder C (200-mL capacity). A thermometer is not requiredbut the use of the ASTM High Distillation Thermometer 8F or8C as prescribed in Specification E1or the IPHigh DistillationThermometer 6C, as prescribed in the IP Thermometer Speci-fic
46、ations is recommended.10.3 Place a volume of sample equivalent to 200 mL at 13to 18C in the flask. Maintain the condenser bath at 0 to 4C(for some oils it may be necessary to hold the temperaturebetween 38 and 60C to avoid solidification of waxy materialin the condenser tube). Use, without cleaning,
47、 the cylinderfrom which the sample was measured as the receiver and placeit so that the tip of the condenser does not touch the wall of thecylinder.10.4 Apply the heat to the flask at a uniform rate soregulated that the first drop of condensate exits from thecondenser between 10 and 15 min after ini
48、tial application ofheat. After the first drop falls, move the receiving cylinder sothat the tip of the condenser tube touches the wall of thecylinder. Then regulate the heat so that the distillation proceedsat a uniform rate of 8 to 10 mL/min. Continue the distillationuntil 178 mL of distillate has
49、been collected, then discontinueheating and allow the condenser to drain until 180 mL (90 % ofthe charge to the flask) has been collected in the cylinder.10.5 Immediately replace the cylinder with a small Erlen-meyer flask and catch any final drainage in the flask. Add tothis flask, while still warm, the distillation residue left in thedistilling flask, and mix well. The contents of the flask thenrepresents a 10 % distillation residue from the original product.10.6 While the distillation residue is warm enough to flowfreely, pour approximately 10 6 0.5 g of it in the p
