1、Designation: D 524 09Designation: 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 () 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 tes
3、t 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 whichpartial
4、ly 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 resid
5、ue, 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 f
6、urther 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 derive
7、d (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 nit
8、rates 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 4
9、The 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 Sect
10、ion 10 for determining carbon residueon 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 This standard does not purport to address all of thesafety concerns, if a
11、ny, 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 use.2. Referenced Documents2.1 ASTM Standards:2D86 Test Method for Distillation of Petroleum Pro
12、ducts atAtmospheric PressureD 189 Test Method for Conradson Carbon Residue ofPetroleum ProductsD 482 Test Method for Ash from Petroleum ProductsD 4046 Test Method for Alkyl Nitrate in Diesel Fuels bySpectrophotometryD 4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD 4175 Termino
13、logy 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 Equipme
14、nt1This 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 June 1, 2009. Published June 2009. Originallyapproved in 1939. Last previous edition appro
15、ved in 2004 as D 52404.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 Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the sta
16、ndards 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.2.2 Energy Institute Standard:3Appendix AP-A SpecificationsIP Thermomet
17、ers3. Terminology3.1 Definitions:3.1.1 carbon residue, nthe residue formed by evaporationand thermal degradation of a carbon containing material.D 41753.1.1.1 DiscussionThe residue is not composed entirelyof carbon but is a coke that can be further changed by carbonpyrolysis. The term carbon residue
18、 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 heated to the point at which all volatile matter
19、 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 decomposition or slight oxidation due to the possibility
20、 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 residue.4.2 Provision is made for determining the
21、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 tendency of the fuel to formdeposits in vapor
22、izing 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 deposits.5.2 The carbon residue value of motor oil,
23、 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 can increase the c
24、arbon 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 stocks, areuseful in the manufacture of lubric
25、ants.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-mmdiameter drill rod through the capillary and
26、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 thermocoupleand conforming to the dimensions and t
27、olerances 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 polished bulb hasdifferent heating characteristics
28、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 serum needle (1.45 to 1.47 mm in outsidediamete
29、r) 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 are moresatisfactory, as the needle locks on th
30、e 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 to a uniform temperature of 550C. Thebottom
31、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 bulb wells, the internal dimensions ofwhich cor
32、respond to the internal dimensions of holes in thesolid metal furnace. The bulb wells shall be immersed in the3IP 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 mil
33、limetres.FIG. 1 Glass Coking BulbD524092molten 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 obtai
34、ned 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 X1.6.5 Temperature-Measuring DevicesA removable iron-constantan thermocouple with a sensitive pyrometer, or othersui
35、table temperature-indicating device, 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 me
36、talsheath when a molten bath is used.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 Pe
37、rformance of Apparatus7.1 Periodically 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 load
38、ing, when theoperating requirements 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 thecontro
39、l bulb, calibrate the thermocouple 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 te
40、mperature 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 and, within 15 s, insert in each of the other wells aglass coking bulb containing 4 6 0.1 g of a v
41、iscous neutralpetroleum lubricating 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
42、control bulbreaches 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 the fur
43、nace is used fullyloaded. Inspect 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
44、and routine operation) andwithin 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 th
45、e 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, 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 performa
46、nce well when only a single test 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 deg
47、ree of furnace loading which maybe 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 ins
48、pected 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 shortest possibletime
49、 to avoid segregation of the sediment. Samples containing sedimentwhich settles quickly after stirring can be placed 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 ca
