1、Designation: D524 10D524 15Designation: 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
2、 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 U.S. Department of Defense.1. Scope*1.1 This test method covers the
3、 determination of the amount of carbon residue (Note 1) left after evaporation and pyrolysis ofan oil, and it is intended to provide some indication of relative coke-forming propensity. This test method is generally applicableto relatively nonvolatile petroleum products which partially decompose on
4、distillation at atmospheric pressure. This test methodalso covers the determination of carbon residue on 10%10 % (V/V) distillation residues (see Section 10). Petroleum productscontaining ash-forming constituents as determined by Test Method D482, will have an erroneously high carbon residue, depend
5、ingupon the amount of ash formed (Notes 2 and 3).NOTE 1The term carbon residue is used throughout this test method to designate the carbonaceous residue formed during evaporation and pyrolysisof a petroleum product. The residue is not composed entirely of carbon, but is a coke which can be further c
6、hanged by pyrolysis. The term carbon residueis continued in this test method only in deference to its wide common usage.NOTE 2Values obtained by this test method are not numerically the same as those obtained by Test Method D189, or Test Method D4530.Approximate correlations have been derived (see F
7、ig. X2.1) but need not apply to all materials which can be tested because the carbon residue test isapplicable to a wide variety of petroleum products. The Ramsbottom Carbon Residue test method is limited to those samples that are mobile below90C.90 C.NOTE 3In diesel fuel, the presence of alkyl nitr
8、ates such as amyl nitrate, hexyl nitrate, or octyl nitrate, causes a higher carbon residue value thanobserved in untreated fuel, which can lead to erroneous conclusions as to the coke-forming propensity of the fuel. The presence of alkyl nitrate in thefuel can be detected by Test Method D4046.NOTE 4
9、The test procedure in Section 10 is being modified to allow the use of a 100mL100 mLvolume automated distillation apparatus. No precisiondata is available for the procedure at this time, but a round robin is being planned to develop precision data. The 250mL250 mL volume bulb distillationmethod desc
10、ribed in Section 10 for determining carbon residue on a 10 % distillation residue is considered the referee test.1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.3 WARNINGMercury has been designated by many regulatory age
11、ncies as a hazardous material that can cause centralnervous system, kidney and liver damage. Mercury, or its vapor, may be hazardous to health and corrosive to materials. Cautionshould be taken when handling mercury and mercury containing products. See the applicable product Material Safety Data She
12、et(MSDS) for details and EPAs websitehttp:/www.epa.gov/mercury/faq.htmfor additional information. Users should be awarethat selling mercury and/or mercury containing products into your state or country may be prohibited by law.1.4 This standard does not purport to address all of the safety concerns,
13、 if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D86 Test Method for Distillation of Petroleum P
14、roducts at Atmospheric PressureD189 Test Method for Conradson Carbon Residue of Petroleum ProductsD482 Test Method for Ash from Petroleum Products1 This test method is under the jurisdiction ofASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
15、SubcommitteeD02.06 on Analysis of Liquid Fuels and Lubricants.Current edition approved July 1, 2010June 1, 2015. Published July 2010June 2015. Originally approved in 1939. Last previous edition approved in 20092010 asD524D524 10.09.In the IP, this test method is under the jurisdiction of the Standar
16、dization Committee. DOI: 10.1520/D0524-10.10.1520/D0524-15.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.Th
17、is document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editi
18、ons as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959.
19、 United States1D4046 Test Method for Alkyl Nitrate in Diesel Fuels by SpectrophotometryD4057 Practice for Manual Sampling of Petroleum and Petroleum ProductsD4175 Terminology Relating to Petroleum, Petroleum Products, and LubricantsD4177 Practice for Automatic Sampling of Petroleum and Petroleum Pro
20、ductsD4530 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:3.1.1 carbon residue, nt
21、he residue formed by evaporation and thermal degradation of a carbon containing material. D41753.1.1.1 DiscussionThe residue is not composed entirely of carbon but is a coke that can be further changed by carbon pyrolysis. The term carbonresidue is retained in deference to its wide common usage.4. S
22、ummary of Test Method4.1 The sample, after being weighed into a special glass bulb having a capillary opening, is placed in a metal furnace maintainedat approximately 550C.550 C. The sample is thus quickly heated to the point at which all volatile matter is evaporated out ofthe bulb with or without
23、decomposition while the heavier residue remaining in the bulb undergoes cracking and coking reactions.In the latter portion of the heating period, the coke or carbon residue is subject to further slow decomposition or slight oxidationdue to the possibility of breathing air into the bulb. After a spe
24、cified heating period, the bulb is removed from the bath, cooled ina desiccator, and again weighed. The residue remaining is calculated as a percentage of the original sample, and reported asRamsbottom carbon residue.4.2 Provision is made for determining the proper operating characteristics of the f
25、urnace with a control bulb containing athermocouple, which must give a specified time-temperature relationship.5. Significance and Use5.1 The carbon residue value of burner fuel serves as a rough approximation of the tendency of the fuel to form deposits invaporizing pot-type and sleeve-type burners
26、. Similarly, provided alkyl nitrates are absent (or if present, provided the test isperformed on the base fuel without additive) the carbon residue of diesel fuel correlates approximately with combustion chamberdeposits.5.2 The carbon residue value of motor oil, while at one time regarded as indicat
27、ive of the amount of carbonaceous deposits amotor oil would form in the combustion chamber of an engine, is now considered to be of doubtful significance due to the presenceof additives in many oils. For example, an ash-forming detergent additive can increase the carbon residue value of an oil yet w
28、illgenerally reduce its tendency to form deposits.5.3 The carbon residue value of gas oil is useful as a guide in the manufacture of gas from gas oil, while carbon residue valuesof crude oil residuum, cylinder and bright stocks, are useful in the manufacture of lubricants.6. Apparatus6.1 Glass Cokin
29、g Bulb, of heat-resistant glass conforming to the dimensions and tolerances shown in Fig. 1. Prior to use, checkthe diameter of the capillary to see that the opening is greater than 1.51.5 mm and not more than 2.0 mm. 2.0 mm. Pass a1.5-mm1.5 mm diameter drill rod through the capillary and into the b
30、ulb; attempt to pass a 2.0-mm2.0 mm diameter drill rodthrough the capillary. Reject bulbs that do not permit the insertion of the smaller rod and those whose capillaries are larger thanthe larger rod.6.2 Control Bulb, stainless steel, containing a thermocouple and conforming to the dimensions and to
31、lerances shown in Fig. 2,for use in determining compliance of furnace characteristics with the performance requirements (Section 7). The control bulb shallbe provided with a dull finish, as specified in Fig. 2, and must not be polished thereafter. A polished bulb has different heatingcharacteristics
32、 from one with a dull finish. A suitable thermocouple pyrometer for observing true temperature within 61C61 Cis also required.3 IP Standard Methods for Analysis and Testing of Petroleum and Related Products, 1998. Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR,U.K.D524 1526.3
33、 Sample Charging Syringe, 55 mL or 10-mL10 mL glass hypodermic (Note 5), fitted with a No. 17 needle (1.5 mm (1.5 mmin outside diameter) or No. 0 serum needle (1.45(1.45 mm to 1.47 mm 1.47 mm in outside diameter) for transfer of the sampleto the glass coking bulb.NOTE 5Asyringe having a needle that
34、fits on the ground-glass tip of the syringe is not recommended, as it may be blown off when pressure is appliedto the syringe plunger. The Luer-Lok type syringes are more satisfactory, as the needle locks on the bottom of the syringe barrel, and cannot be blownoff by pressure.6.4 Metal Coking Furnac
35、e of solid metal, having coking bulb wells 25.4525.45 mm 6 0.1 mm 0.1 mm in internal diameter and76 mm 76 mm deep to the center of the well bottom, with suitable arrangements for heating to a uniform temperature of550C.550 C. The bottom of the well shall be hemispherical to accommodate the bottom of
36、 the glass coking bulb. Do not castor otherwise form the furnace with unnecessary voids which will impede heat transfer. If a molten metal furnace is used, provideit with a suitable number of bulb wells, the internal dimensions of which correspond to the internal dimensions of holes in the solidmeta
37、l furnace. The bulb wells shall be immersed in the molten metal to leave not more than 3 mm of the bulb well exposed abovethe molten metal at operating temperatures.NOTE 6Ramsbottom coke furnaces now in use can have dimensional differences from those given in 6.4; however, it is essential that new f
38、urnacesNOTE 1All dimensions are in millimetres.FIG. 1 Glass Coking BulbNOTE 1All dimensions are in millimetres.FIG. 2 Control BulbD524 153obtained after the adoption of this test method conform to the requirements outlined in 6.4. A description of one type of furnace which has been foundto be satisf
39、actory is given in Appendix X1.6.5 Temperature-Measuring DevicesA removable iron-constantan thermocouple with a sensitive pyrometer, or other suitabletemperature-indicating device, located centrally near the bottom portion of the furnace and arranged to measure the temperatureof the furnace so that
40、the performance tests specified in Section 7 can be obtained. It is desirable to protect thetemperature-indicating device with a quartz or thin metal sheath when a molten bath is used.NOTE 7It is good practice to calibrate the thermocouple or other temperature-measuring device against a standard the
41、rmocouple or referencestandards about once a week, when the furnace is in constant use, the actual frequency depending on experience.7. Checking Performance of Apparatus7.1 Periodically check the performance of the furnace and temperature-measuring devices as described in 7.1.1 7.1.3 to makecertain
42、that as used they conform to the requirements of the method. Consider the furnace as having standard performance, anduse it with any degree of loading, when the operating requirements described for each coking bulb well are met, while the bathis fully loaded as well as singly loaded. Use only a furn
43、ace that has successfully passed the performance or control tests given inthis section.7.1.1 ThermocoupleAt least once every 50 h 50 h of use of the control bulb, calibrate the thermocouple in the control bulbagainst a standard thermocouple.NOTE 8In use at the high temperature of the test, iron-cons
44、tantan thermocouples oxidize and their calibration curves change.7.1.2 Fully Loaded FurnaceWhen the furnace temperature is within a previously chosen 2C2 C temperature range (whichrange is to be used thereafter with that particular furnace for both standardization and routine operation) and within t
45、he generalrange 550550 C 6 5C, insert the control bulb in one well and, within 15 s, insert in each of the other wells a glass coking bulbcontaining 44g 6 0.1 g of a viscous neutral petroleum lubricating oil with a viscosity within the SAE 30 range or 6060 mm2 to100 mm100 mm2/s (cSt) at 40C.40 C. Wi
46、th a suitably accurate potentiometer or millivoltmeter (sensitive to 1C1 C or less),observe the temperature rise in the control bulb at 1-min1 min intervals for 20 min. 20 min. If the temperature in the control bulbreaches 547C547 C in not less than 44 min and not more than 6 min 6 min from the inst
47、ant of its insertion in the furnace, andremains within the range 550550 C 6 3C3 C for the remaining portion of the 20-min20 min test, consider that particular cokingbulb well suitable for use as a standard performance well when the furnace is used fully loaded. Inspect each well in similar fashionwi
48、th the furnace fully loaded each time.7.1.3 Singly Loaded FurnaceWhen the furnace temperature is within a previously chosen 2C2 C temperature range (whichrange is to be used thereafter with that particular furnace for both standardization and routine operation) and within the generalrange 550550 C 6
49、 5C,5 C, insert the control bulb in one well, with the remaining wells unoccupied. With a suitably accuratepotentiometer or millivoltmeter (sensitive to 1C1 C or less), observe the temperature rise in the control bulb at 1-min1 minintervals for 20 min. 20 min. If the temperature in the control bulb reaches 547C547 C in not less than 44 min and not more than6 min from the instant of its insertion in the furnace, and remains within the range 550550C 6 3C3 C for the remaining portionof the 20-min20 min test, consider that
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