1、Designation: D 524 04Designation: 14/94An American National StandardStandard Test Method forRamsbottom Carbon Residue of Petroleum Products1This standard is issued under the fixed designation D 524; the number immediately following the designation indicates the year oforiginal adoption or, in the ca
2、se 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.1. Scope*1.1 This te
3、st method covers the determination of the amountof carbon residue (Note 1) left after evaporation and pyrolysisof an oil, and it is intended to provide some indication ofrelative coke-forming propensity. This test method is generallyapplicable to relatively nonvolatile petroleum products whichpartia
4、lly decompose on distillation at atmospheric pressure.This test method also covers the determination of carbonresidue on 10% (V/V) distillation residues (see Section 10).Petroleum products containing ash-forming constituents asdetermined by Test Method D 482, will have an erroneouslyhigh carbon resi
5、due, depending upon the amount of ash formed(Notes 2 and 3).NOTE 1The term carbon residue is used throughout this test methodto designate the carbonaceous residue formed during evaporation andpyrolysis of a petroleum product. The residue is not composed entirely ofcarbon, but is a coke which can be
6、further changed by pyrolysis. The termcarbon residue is continued in this test method only in deference to itswide common usage.NOTE 2Values obtained by this test method are not numerically thesame as those obtained by Test Method D 189, or Test Method D 4530.Approximate correlations have been deriv
7、ed (see Fig. X2.1) but need notapply to all materials which can be tested because the carbon residue testis applicable to a wide variety of petroleum products. The RamsbottomCarbon Residue test method is limited to those samples that are mobilebelow 90C.NOTE 3In diesel fuel, the presence of alkyl ni
8、trates such as amylnitrate, hexyl nitrate, or octyl nitrate, causes a higher carbon residue valuethan observed in untreated fuel, which can lead to erroneous conclusionsas to the coke-forming propensity of the fuel. The presence of alkyl nitratein the fuel can be detected by Test Method D 4046.NOTE
9、4The test procedure in Section 10 is being modified to allowthe use of a 100mL volume automated distillation apparatus. Noprecision data is available for the procedure at this time, but a round robinis being planned to develop precision data. The 250mL volume bulbdistillation method described in Sec
10、tion 10 for determining carbon residueon a 10 % distillation residue is considered the referee test.1.2 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 heal
11、th practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 86 Test Method for Distillation of Petroleum Products atAtmospheric PressureD 189 Test Method for Conradson Carbon Residue ofPetroleum ProductsD 482 Test Method for Ash f
12、rom Petroleum 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 andPetrol
13、eum ProductsD 4530 Test Method for Determination of Carbon Residue(Micro Method)E 1 Specification for ASTM Liquid-in-Glass ThermometersE 133 Specification for Distillation Equipment2.2 Energy Institute Standards:Appendix AP-A SpecificationsIP Thermometers33. Terminology3.1 Definitions:3.1.1 carbon r
14、esidue, nthe residue formed 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 app
15、roved Nov. 1, 2004. Published November 2004. Originallyapproved in 1939. Last previous edition approved in 2003 as D 52403.In the IP, this test method is under the jurisdiction of the StandardizationCommittee.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Custom
16、er Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3IP Standard Methods for Analysis and Testing of Petroleum and RelatedProducts, 1998. Available from Energy Institute, 61 New Cavendish St., London,WIG
17、7AR, U.K.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.D 41753.1.1.1 DiscussionThe residue is not composed entirelyof carbon but is a coke that can be further change
18、d by carbonpyrolysis. The term carbon residue is retained in deference toits wide common usage.4. Summary of Test Method4.1 The sample, after being weighed into a special glassbulb having a capillary opening, is placed in a metal furnacemaintained at approximately 550C. The sample is thusquickly hea
19、ted to the point at which all volatile matter isevaporated out of the bulb with or without decompositionwhile the heavier residue remaining in the bulb undergoescracking and coking reactions. In the latter portion of theheating period, the coke or carbon residue is subject to furtherslow decompositi
20、on or slight oxidation due to the possibility ofbreathing air into the bulb. After a specified heating period, thebulb is removed from the bath, cooled in a desiccator, andagain weighed. The residue remaining is calculated as apercentage of the original sample, and reported as Ramsbottomcarbon resid
21、ue.4.2 Provision is made for determining the proper operatingcharacteristics of the furnace with a control bulb containing athermocouple, which must give a specified time-temperaturerelationship.5. Significance and Use5.1 The carbon residue value of burner fuel serves as arough approximation of the
22、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 deposi
23、ts.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. For example, anash-
24、forming detergent additive can 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 residuum, cylinder and bright s
25、tocks, areuseful in the manufacture of lubricants.6. Apparatus6.1 Glass Coking Bulb, of heat-resistant glass conforming tothe dimensions and tolerances shown in Fig. 1. Prior to use,check the diameter of the capillary to see that the opening isgreater than 1.5 and not more than 2.0 mm. Pass a 1.5-mm
26、diameter drill rod through the capillary and into the bulb;attempt to pass a 2.0-mm diameter drill rod through thecapillary. Reject bulbs that do not permit the insertion of thesmaller rod and those whose capillaries are larger than thelarger rod.6.2 Control Bulb, stainless steel, containing a therm
27、ocoupleand conforming to the dimensions and tolerances shown in Fig.2, for use in determining compliance of furnace characteristicswith the performance requirements (Section 7). The controlbulb shall be provided with a dull finish, as specified in Fig. 2,and must not be polished thereafter. A polish
28、ed bulb hasdifferent heating characteristics from one with a dull finish. Asuitable thermocouple pyrometer for observing true tempera-ture within 61C is also required.6.3 Sample Charging Syringe, 5 or 10-mL glass hypodermic(Note 5), fitted with a No. 17 needle (1.5 mm in outsidediameter) or No. 0 se
29、rum needle (1.45 to 1.47 mm in outsidediameter) for transfer of the sample to the glass coking bulb.NOTE 5A syringe having a needle that fits on the ground-glass tip ofthe syringe is not recommended, as it may be blown off when pressure isapplied to the syringe plunger. The Luer-Lok type syringes ar
30、e moresatisfactory, as the needle locks on the bottom of the syringe barrel, andcannot be blown off by pressure.6.4 Metal Coking Furnace of solid metal, having cokingbulb wells 25.45 6 0.1 mm in internal diameter and 76 mmdeep to the center of the well bottom, with suitable arrange-ments for heating
31、 to a uniform temperature of 550C. Thebottom of the well shall be hemispherical to accommodate thebottom of the glass coking bulb. Do not cast or otherwise formthe furnace with unnecessary voids which will impede heattransfer. If a molten metal furnace is used, provide it with asuitable number of bu
32、lb wells, the internal dimensions ofwhich correspond to the internal dimensions of holes in thesolid metal furnace. The bulb wells shall be immersed in themolten metal to leave not more than 3 mm of the bulb wellexposed above the molten metal at operating temperatures.NOTE 6Ramsbottom coke furnaces
33、now in use can have dimensionaldifferences from those given in 6.4; however, it is essential that newfurnaces obtained after the adoption of this test method conform to therequirements outlined in 6.4. A description of one type of furnace whichhas been found to be satisfactory is given in Appendix X
34、1.6.5 Temperature-Measuring DevicesA removable iron-constantan thermocouple with a sensitive pyrometer, or othersuitable temperature-indicating device, located centrally nearthe bottom portion of the furnace and arranged to measure thetemperature of the furnace so that the performance testsNOTEAll d
35、imensions are in millimetres.FIG. 1 Glass Coking BulbD524042specified in Section 7 can be obtained. It is desirable to protectthe temperature-indicating device with a quartz or thin metalsheath when a molten bath is used.NOTE 7It is good practice to calibrate the thermocouple or othertemperature-mea
36、suring device against a standard thermocouple or refer-ence standards about once a week, when the furnace is in constant use, theactual frequency depending on experience.7. Checking Performance of Apparatus7.1 Periodically check the performance of the furnace andtemperature-measuring devices as desc
37、ribed in 7.1.1-7.1.3 tomake certain that as used they conform to the requirements ofthe method. Consider the furnace as having standard perfor-mance, and use it with any degree of loading, when theoperating requirements described for each coking bulb well aremet, while the bath is fully loaded as we
38、ll as singly loaded. Useonly a furnace that has successfully passed the performance orcontrol tests given in this section.7.1.1 ThermocoupleAt least once every 50 h of use of thecontrol bulb, calibrate the thermocouple in the control bulbagainst a standard thermocouple.NOTE 8In use at the high tempe
39、rature of the test, iron-constantanthermocouples oxidize and their calibration curves change.7.1.2 Fully Loaded FurnaceWhen the furnace tempera-ture is within a previously chosen 2C temperature range(which range is to be used thereafter with that particularfurnace for both standardization and routin
40、e operation) andwithin the general range 550 6 5C, insert the control bulb inone well and, within 15 s, insert in each of the other wells aglass coking bulb containing 4 6 0.1 g of a viscous neutralpetroleum lubricating oil with a viscosity within the SAE 30range or 60 to 100 mm2/s (cSt) at 40C. Wit
41、h a suitablyaccurate potentiometer or millivoltmeter (sensitive to 1C orless), observe the temperature rise in the control bulb at 1-minintervals for 20 min. If the temperature in the control bulbreaches 547C in not less than 4 and not more than 6 min fromthe instant of its insertion in the furnace,
42、 and remains withinthe range 550 6 3C for the remaining portion of the 20-mintest, consider that particular coking bulb well suitable for useas a standard performance well when the furnace is used fullyloaded. Inspect each well in similar fashion with the furnacefully loaded each time.7.1.3 Singly L
43、oaded FurnaceWhen the furnace tempera-ture is within a previously chosen 2C temperature range(which range is to be used thereafter with that particularfurnace for both standardization and routine operation) andwithin the general range 550 6 5C, insert the control bulb inone well, with the remaining
44、wells unoccupied. With a suitablyaccurate potentiometer or millivoltmeter (sensitive to 1C orless), observe the temperature rise in the control bulb at 1-minintervals for 20 min. If the temperature in the control bulbreaches 547C in not less than 4 and not more than 6 min fromthe instant of its inse
45、rtion in the furnace, and remains withinthe range 550 6 3C for the remaining portion of the 20-mintest, consider that particular coking bulb well suitable for useas a standard performance well when only a single test ismade. Inspect each well in similar fashion with the furnacesingly loaded each tim
46、e.NOTE 9It is possible that not all of the wells in old furnaces will meetthe requirements when fully loaded and singly loaded; and, when this isthe case, inspect each well for any degree of furnace loading which maybe used. For example, when not more than three wells of a six-wellfurnace can be use
47、d at any one time, the three wells to be used should bechosen from the performance data obtained with fully loaded and singlyloaded furnaces. Then each of the three wells should be inspected for tripleloading, two of the wells for double loading, and one for single loading.Use the wells tested and n
48、o others in applying the test procedure.NOTE 10In sampling oils containing sediment (for example, usedoils), it is important to make the transfer of sample in the shortest possibletime to avoid segregation of the sediment. Samples containing sedimentwhich settles quickly after stirring can be placed
49、 in the coking bulbs moreexpeditiously by using an arrangement such as that shown in Fig. 3. Thissampling device consists of a three-way 2-mm stopcock to which havebeen fused two lengths of capillary tubing (1.5 mm in inside diameter).Connect the third leg of the stopcock by means of pressure tubing to avacuum line. Secure the glass coking bulb to the short arm of capillarytubing by a 25-mm length of rubber hose, taking care that the capillary ofthe glass bulb is butted up against the capillary tubing. Immerse the longend of the capillary tubing in th
