Standard Test Method for Conradson Carbon …

1 Designation: D 189 06 2 Designation: 13/94An American National StandardBritish Standard 4380 Standard Test Method forConradson Carbon Residue of Petroleum Products1 This Standard is issued under the fixed designation D 189; the number immediately following the designation indicates the year oforiginal 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 Standard has been approved for use by agencies of the Department of Defense. 1 NOTE Removed asbestos reinstated original research report footnote editorially in October 2007. 2 NOTE Updated Summary of Changes and added to research report footnote editorially in December Scope* 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.

2 This test Method is generally ap-plicable to relatively nonvolatile petroleum products whichpartially decompose on distillation at atmospheric products containing ash-forming constituents asdetermined by Test MethodD 482or IP Method 4 will have anerroneously high Carbon residue, depending upon the amountof ash formed (Note 2andNote 4).NOTE1 The termcarbon residueis 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 . The termcarbon residueiscontinued in this test Method only in deference to its wide common Values obtained by this test Method are not numerically thesame as those obtained by Test MethodD 524. Approximate correlationshave been derived (seeFig. ), but need not apply to all materialswhich can be tested because the Carbon residue test is applied to a widevariety of petroleum The test results are equivalent to Test MethodD 4530, (seeFig.)

3 NOTE4 In diesel fuel, the presence of alkyl nitrates such as amylnitrate, hexyl nitrate, or octyl nitrate causes a higher 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 MethodD The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for 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 limitations prior to Referenced 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 Petroleum 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 133 Specification for Distillation Equipment3.

4 :1 This test Method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of on Analysis of edition approved Nov. 1, 2006. Published December 2006. Originallyapproved in 1924. Last previous edition approved in 2005 as D 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 joint ASTM IPstandard in procedure is a modification of the original Conradson Method and apparatusfor Carbon Test and Ash Residue in Petroleum Lubricating Oils. SeeProceedings,Eighth International Congress of Applied Chemistry, New York, Vol 1, p. 131,September 1912; alsoJournal of Industrial and Engineering Chemistry, IECHA,Vol 4, No. 11, December 1965, a new Fig. 2 on reproducibility and repeatability combining ASTM andIP precision data replaced old Fig.

5 2 andNote referenced ASTM standards, visit the ASTM website, , orcontact ASTM Customer Service at ForAnnual Book of ASTMS tandardsvolume information, refer to the Standard s Document Summary page onthe ASTM *A Summary of Changes section appears at the end of this ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United residue,n the residue formed by evaporationand thermal degradation of a Carbon containing The residue is not composed entirely ofcarbon but is a coke that can be further changed by carbonpyrolysis. The term Carbon residue is retained in deference toits wide common 41754. Summary of Test A weighed 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 period, the testcrucible containing the carbonaceous residue is cooled in adesiccator and weighed.

6 The residue remaining is calculated asa percentage of the original sample, and reported as Conradsoncarbon Significance and The Carbon residue value of burner fuel serves as arough approximation 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 withcombustion chamber 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. For example, anash-forming detergent additive may increase the Carbon residuevalue of an oil yet will generally reduce its tendency to 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, cylinder and bright stocks, areuseful in the manufacture of Apparatus(seeFig.)

7 1) Crucible, wide form, glazed throughout, or asilica crucible; 29- to 31-mL capacity, 46 to 49 mm in Crucible Skidmore iron crucible, flanged andringed, 65- to 82-mL capacity, 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 theFIG. 1 Apparatus for Determining Conradson Carbon ResidueD189 06 22vertical opening closed. The horizontal opening of about shall be kept clean. The outside diameter of the flat bottomshall be 30 to 32 Crucible Spun sheet-iron crucible with cover; 78to 82 mm in outside diameter at the top, 58 to 60 mm in height,and approximately mm in thickness. Place at the bottom ofthis crucible, and level before each test, a layer of about 25 mLof dry sand, or enough to bring the Skidmore crucible, withcover on, nearly to the top of the sheet-iron Support Triangle of bare Nichrome wire ofapproximately No.

8 13B&Sgage having an opening smallenough to support the bottom of the sheet-iron crucible at thesame level as the bottom of the heat-resistant block or hollowsheet-metal box ( ). Circular sheet-iron hood from 120 to 130 mm indiameter the height of the lower perpendicular side to be from50 to 53 mm; provided at the top with a chimney 50 to 60 mmin height and 50 to 56 mm in inside diameter, which is attachedto 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 bridgemade of approximately 3-mm iron or Nichrome wire, andhaving a height of 50 mm above the top of the chimney, shallbe Heat-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 with ametal-lined, inverted cone-shaped opening through the center;83 mm in diameter at the bottom, and 89 mm in diameter at thetop.

9 In the case of the refractory ring no metal lining isnecessary, providing the ring is of hard, heat-resistant It is not know what type of insulators were used in the roundrobin conducted for obtaining the precision given in , Meker type, having an orifice approximately 24mm in For sampling techniques see PracticesD 4057andD Shake thoroughly the sample to be tested, first heating to50 610 C for h when necessary to reduce its 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 cruciblecontaining two glass beads about 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 onthe latter fitting loosely to allow free exit to the vapors On a suitable stand or ring, place the bare Nichromewire triangle and on it the insulator.

10 Next center the sheet-ironcrucible in the insulator with its bottom resting on top of thetriangle, and cover the whole with the sheet-iron hood in orderto distribute the heat uniformly during the process (seeFig. 1). Apply heat with a high, strong flame from the Meker-type gas burner, so that the pre-ignition period will be (a shorter time can start the distillation so rapidly as tocause foaming or too high a flame). 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 vapors burn uniformly withthe flame above the chimney but not above the wire can be increased, if necessary, when the flame does notshow above the chimney. The period of burning the vaporsshall be 1361 min.