1、Designation: D524 10Designation: 14/94Standard Test Method forRamsbottom Carbon Residue of Petroleum Products1This standard is issued under the fixed designation D524; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of las
2、t revision. 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 Department of Defense.1. Scope*1.1 This test method covers the determinati
3、on 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 whichpartially decompose on distillation at
4、 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 D482, will have an erroneouslyhigh carbon residue, depending upon the amount of
5、 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 further changed by pyrolysis. The
6、 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 D189, or Test Method D4530.Approximate correlations have been derived (see Fig. X2.1) but need notappl
7、y 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 nitrates such as amylnitrate, hexyl n
8、itrate, 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 D4046.NOTE 4The test procedure in Section 10 is
9、 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 Section 10 for determining carbon resid
10、ueon a 10 % distillation residue is considered the referee test.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 WARNINGMercury has been designated by manyregulatory agencies as a hazardous material that can causecentral
11、nervous system, kidney and liver damage. Mercury, orits vapor, may be hazardous to health and corrosive tomaterials. Caution should be taken when handling mercury andmercury containing products. See the applicable product Ma-terial Safety Data Sheet (MSDS) for details and EPAswebsitehttp:/www.epa.go
12、v/mercury/faq.htmfor addi-tional information. Users should be aware that selling mercuryand/or mercury containing products into your state or countrymay be prohibited by law.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibil
13、ity of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D86 Test Method for Distillation of Petroleum Products atAtmospheric PressureD189 Test Method for
14、Conradson Carbon Residue of Pe-troleum ProductsD482 Test Method for Ash from Petroleum ProductsD4046 Test Method for Alkyl Nitrate in Diesel Fuels bySpectrophotometryD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4175 Terminology Relating to Petroleum, PetroleumProducts, and L
15、ubricants1This 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 July 1, 2010. Published July 2010. Originally approvedin 1939. Last previous editio
16、n approved in 2009 as D52409.In the IP, this test method is under the jurisdiction of the StandardizationCommittee. DOI: 10.1520/D0524-10.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume
17、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.D4177 Practice for Automatic Sampling of P
18、etroleum andPetroleum ProductsD4530 Test Method for Determination of Carbon Residue(Micro Method)E1 Specification for ASTM Liquid-in-Glass ThermometersE133 Specification for Distillation Equipment2.2 Energy Institute Standard:3Appendix AP-A SpecificationsIP Thermometers3. Terminology3.1 Definitions:
19、3.1.1 carbon residue, nthe residue formed by evaporationand thermal degradation of a carbon containing material.D41753.1.1.1 DiscussionThe residue is not composed entirelyof carbon but is a coke that can be further changed by carbonpyrolysis. The term carbon residue is retained in deference toits wi
20、de 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 heated to the point at which all volatile matter isevaporated out of the bulb with
21、 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 decomposition or slight oxidation due to the possibility ofbreathing air into the bulb. Af
22、ter 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 residue.4.2 Provision is made for determining the proper operatingcharacteristics of
23、 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 tendency of the fuel to formdeposits in vaporizing pot-type and sleeve-type bur
24、ners. 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 deposits.5.2 The carbon residue value of motor oil, while at one timeregarded as indi
25、cative 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 can increase the carbon residuevalue of an oil yet w
26、ill 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 stocks, areuseful in the manufacture of lubricants.6. Apparatus6.1 Glass Coking
27、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-mmdiameter drill rod through the capillary and into the bulb;attempt to pass a 2.
28、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 thermocoupleand conforming to the dimensions and tolerances shown in Fig.2, for use
29、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 polished bulb hasdifferent heating characteristics from one with a dull finish. Asuit
30、able 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 serum needle (1.45 to 1.47 mm in outsidediameter) for transfer of the sample to t
31、he 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 are moresatisfactory, as the needle locks on the bottom of the syringe barrel, an
32、dcannot 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 to a uniform temperature of 550C. Thebottom of the well shall be hemispherical
33、 to accommodate thebottom of the glass coking bulb. Do not cast or otherwise form3IP Standard Methods for Analysis and Testing of Petroleum and RelatedProducts, 1998. Available from Energy Institute, 61 New Cavendish St., London,WIG 7AR, U.K.NOTEAll dimensions are in millimetres.FIG. 1 Glass Coking
34、BulbD524 102the furnace with unnecessary voids which will impede heattransfer. If a molten metal furnace is used, provide it with asuitable number of bulb wells, the internal dimensions ofwhich correspond to the internal dimensions of holes in thesolid metal furnace. The bulb wells shall be immersed
35、 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 now in use can have dimensionaldifferences from those given in 6.4; however, it is essential that newfurnaces obtained after the adoption of this te
36、st 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 X1.6.5 Temperature-Measuring DevicesA removable iron-constantan thermocouple with a sensitive pyrometer, or othersuitable temperature-indicating devi
37、ce, located centrally nearthe bottom portion of the furnace and arranged to measure thetemperature of the furnace so that the performance testsspecified 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 u
38、sed.NOTE 7It is good practice to calibrate the thermocouple or othertemperature-measuring 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 Periodi
39、cally check the performance of the furnace andtemperature-measuring devices as described 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 requiremen
40、ts described for each coking bulb well aremet, while the bath is fully loaded as well 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 thermocoupl
41、e in the control bulbagainst a standard thermocouple.NOTE 8In use at the high temperature 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
42、 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 and, within 15 s, insert in each of the other wells aglass coking bulb containing 4 6 0.1 g of a viscous neutralpetroleum lubricati
43、ng oil with a viscosity within the SAE 30range or 60 to 100 mm2/s (cSt) at 40C. 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 l
44、ess than 4 and not more than 6 min fromthe instant of its insertion 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 the furnace is used fullyloaded. Inspect
45、 each well in similar fashion with the furnacefully loaded each time.7.1.3 Singly 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 routine operation) andwithin
46、the general range 550 6 5C, insert the control bulb inone well, with the remaining 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 bulb
47、reaches 547C in not less than 4 and not more than 6 min fromthe instant of its insertion 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
48、ismade. Inspect each well in similar fashion with the furnacesingly loaded each time.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 mayb
49、e used. For example, when not more than three wells of a six-wellfurnace can be used 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 no 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 shor
