“Tie interna stand was dele tn econdance with intently reogaoe precipi a sande forthe Devcapmeet i intraaunal Staaaeds Cuids t Recoendathns hse by th Ska Oxy Thal avers tn We (THT) Coe Y Designation: 01857/01857M - 17 Standard Test Method for Fusibility of Coal and Coke Ash’ ‘eappeosal A supersergt epsilon (e) indicates an eiorel change since the last revision or eagproval sur of igi adoption onthe Ws ound has bee erased forse Oy agentes of te 2S. Depavamen af Defers 1. Seope 1.1 This test method cavers the observation of the tempera tures at which trigmgular pyramids (cones) prepared from coal and coke ash attain and pass through certain defined stages of using and flow when heated at a specified rate in controlled mildly reducing, and whers desired, oxidizing, atmospheres 1.2 The test method is empirical, and strict observance of the requirements and conditions is necessary to obsain repeo- ducible temperatures and enable different laboratories to obtain ‘concordant results, 1.3 ‘The values stated in either St units or inch-pound units are to be regarded separately as standard. The values stated in each system may not be exact equivalents; therefore, each system shall be used independently of the other. Combining values from the to systems may result in non-conformance with the standard L3.1 All percentages aro percent’ mass fractions unless otherwise noted, LA This suemdard does not purport to auldress all of the safety concems, if any, associated with its use. It is the responsibility of the user of this standant to establish appro: priate safety and heatth practices and deiermine the applica bility of regulatory linizations prior 20 use. 2. Referenced Documents 21 ASTM Standards:* D346 Practice for Collection and Preparation of Coke Samples for Laboratory Analysis 12013 Practice for Preparing Coal Samples for Analysis 13174 Test Method for Ash in the Analysis Sample of Coal and Coke from Coal 13180 Practice for Calculating Coal and Coke Analyses from As-Determined to Different Bases "ws seth unde the juratcon of ASTM Corsi DOS on Coal approved 1961. Lat pons ction apposed i 2016 ay DI8S7 16. DOL usa 7217 Fe referenced ASTM stndan, wi the ASTM wei, wens. ‘onact ASTM Castor Serves at srvicciasm rg. Fa acs Boat of ASTM ‘Stands volar formation, reer so he sands Dost Sema Paso te ASTM weds, cov ©.7¢ heron 100 Br Ht rb PO Ro 7, nt Saco PAYER. Uri me 13682 Test Method for Major and Minor Elements in Combustion Residues from Coal Utilization Processes 14326 Test Method for Major and Minor Elements in Coal and Coke Ash By X-Ray Fluorescence 16349 ‘Test Method for Determination of Major and Minor Blements i Coal, Coke, and Solid Residues from Com bustion of Coal and Coke by Induetively Coupled Plasma—Atomic Emission Spectrometry D7582 Test Methods for Proximate Analysis of Coal and Coke by Macro Thermogravimetric Analysis, 3. Terminology 311 Definitions of Terms Specific to This Standart 3.11 The eriveal temperature points to be observed are as follows 3.1.2 flid temperature, FT—the vemperacure at which the fused” mass his spread out in a nearly fat layer with a maximom height of [6 mm {is in as shown hy the fifth cone, FT, in Fi. 3.1.3 hemispherical temperature, HTthe temperature at which the cane has fused down tos hemispherical lamp at ‘which point the height is onc hall the wih of the base as shown by the fourth coe, HT, in Fig. 1 314 initial deformation temperature, IT—the temperature fat which the first rounding of the apex of the cone occurs Shrinkage or warping of the cone ignored if the tip remains sharp. In Fig. 1, the first cone shown is an unheated one; the second cone IT is atypical cone atthe initial deformation stage 3.1.9 softening temperanure, ST—the temperature at which the cone has fused down w/a spherical lump ia which the height is equal to the width at the base as shown by the third cone, ST, in Fig. 1. (wWVSO") VIVSUIE VEILHVTaS ISvaadON ANIUN « IRUONEUIAIUT WASY !SUES!] YME IP NSE 4aIO IeNGIp IU! AdoD “YSN ‘EZHET Vd ‘UaYDOYOYSUOD 359M ‘AAUG INOqUEH Weg OT ‘TEUOHEWEILT WASY EdD 4H, 4, Summary of Test Method 4.1 Coal or coke ash, prepared by prescribed methods, is ‘mixed with a small amount of a dextrin solution to form a plastic mass. A cone mold is used to form triangular pyramids with the plastic mass, whieh are dried and mounted on a ceramic platform. The cones and platform are rapidly heated in clric furnace to 400 °C (750 °F). The cones and platform are then heated at a rate of 8°C & 3°C [15°F + 5°F]/min in{Wy 01857/01857M - 17 ole Meera fae a) ane 1m ost owt oT FIG. 1 Critical Temperature Points a reducing (CO/CO,) atmosphere, or an oxidizing (air) amo: sphere. The ash cones are carefully observed as they pass through certain defined stages of melting and flow. 5. Significance and Use 5.1 The design of most coal combustion and coal conver- sion equipment anticipates that the ash either remain solid or assume some degree of fluidity, depending on the particular design. Ash fusibility temperatures help prediet whether the ash will perform properly inthe process for whieh the coal was chosen, 5.2. Ash fusibility temperature values are used in various ‘equations to prediet the slagging tendency of ashes 6. Apparatus 6.1 Furnace—An electtie furnace coafoemi ing requirements may be used 6.1.1 Capable of maintaining a uniform temperature zone in which to heat the ash cones, 6.1.2 Capable of maintaining the desired atmosphere sur= rounding the cones during heating. The composition of the atmosphere, reducing or oxidizing, shall be raaintained within the limits specified in Seetion 7. The desired atmosphere is t0 be obtained by means of gases introduced into the heating, chamber. The fumace should be gas impervious. 6.1.3 Capable of regulation 90 that the rate of temperature rise shall be 8°C + 3°C [15°F + 5°F//min. 6.14 Providing means of observing the ash cones during the heating. Observation on the same horizontal plane as the ‘cane-support surface shall be possible, 6.2. Cone Moid—A commercially available cone mold, 1ypi- cally brass or made from a conosion-tesistant material with & low coeificient of friction, as shown in Fig, 2. The cone shall be 19 mm [4 in.] in height and 6.4 mm [4 in| in width at each side of the base. which is an equilateral triangle. A steel spatula, with a pointed tip, ground off to fit the cone depression ip the mold, is suitable for removal of the ash cone. 63 Refractory Teay Mold—A mold with fat top and bottom surfaces to provide a refractory tray of suitable thickness to minimize warping. A sidemold not over 6.4 mm [¥4 in. high of any convenient shape, placed on an iron plate so that the top ‘surface of the refractory mix can be struck off flat and parallel to the tray by means of a straight edge, is satisfactory. Logs not over 3.mm [¥% in] long may be provided on the eomers of the ‘cone way by suitable holes bored in the iron base plate of the old 64 Readout Device—A thermocouple of platinum and platinum-thodium, protected from the fumace gases by a ghved poreelain sheath, shall be used with an appropriate 3g tothe follow: 1 Unis, 7a 02 762 FIG, 2 Brass Cone Mold readout device accurate and readable 10 within 5.5 °C [10°F ‘The hot junction of the thermocouple shall touch the end of the sheath and shall he located in the center of the furnace and ‘immediately to the rear of the cones. The thermocouple protective sheath shall he checked periodically for cracks. The thermocouple and its meter shall meet the requirements of Section 10. 7. Reagents and Materials 7. Ash-Cone Refractory Trays—The ash cones shall be mounted on refractory trays. These trays are commercially available, or ean be prepared using a mixture of equal parts by weight of kaolin and alumina. Materials conforming to the following requirements are to be used in preparing the reirac~ tory trays: 7.2 Kaolin —NF-grade powder passing a 75 jum (USA. Standard No, 200) sieve, 7.3 Aluminum Ovide—Reagent grade ignited powder pass. ing a 150 ym (L7S.A. Standard No. 100) sieve. (viysom) vHVSUaE VUaLHYCas Isv¥adox MUA eUOReWIEIUT HLISY 15U9S1| YemeG Ip NSB YEIO YeNqIP IU! AdOD “YSN ‘EZHET Vd ‘UBPIOYOUSUOD ISOM ‘eAUUG noqeH Weg OOT ‘eUOREWAIUT MISV Ed) 42H, 7.4 Dextrin Solution—clear, filtered (if necessary) 10 % solution of dextrin containing 0.1 % salicylic acid as a preservative 75 Mold Release Agent-—petcoleum jelly, thinned with kerosene (if necessary), or a non-silicon-based mold release agent. 7.6 Gold Wire—0.51 mm diameter (twenty-four gage) or larger round wire of 99.98 % purity, but drawn from metal of 99.99 % purity, and having a melting point of 1063 °C [1945 °F 77 Nicket Wire—0.51 mm diameter (twenty-four gaye) or larger round wire of CP nickel, 99.98 % pure, fully annealed, and having a melting point of 1452 °C [2645 °Fily 01957/01857M - 17 8. Test Atmospheres 8.1 Redueing Atmosphere Test—A regulated flow of the nominal composition, volume fraction 60 % carbon ‘oxide and volume fraction 40 = 5 % carbon dioxide, shall be ‘maintained in the heating chamber throughout the test (Note 1) in the furnace. The gas stream shall be regulated by any ‘convenient means to provide a measured flow of 1.3 to 1.5 furnace volumes per minute. 82 Cylinders of COACO, Gus—To assure that the COCO, {gas remains mixed, maintain the temperature of the eylinder above the critical temperature at which CO, can liguety and separate, 82 Onidicing Atmosphere Test—A regulated stream of air ‘shall be maintained throughout the test in the furnace. The gas strcam shall be regulated by any convenient means to provide 4 measured flow of 13 (0 1.5 furnace volumes per minute 4. Sample and Test Specimen Preparation 9.1 Coal and Coke—Prepare the analysis sample in accor- dance with Practice D2013 for coal or Practice D346 for coke by pulverizing the material to pass a 250 yim (No. 60) US.A. standard sieve. 92 Laboratory Aching of Coal or Coke Analysis Seample— Prepare the ash from a thoroughly mixed analysis sample of coal or coke (see 9.1) To facilitate the ashing process, spread the coal or coke in a layer about 6 mm (¥% ia.) in depth in a porcelain, quartz. fused silica, or fireclay roasting dish. Place the dish in a mulfle furnace at ambient temperature and heat gradually so thatthe temperature reaches 500 °C = 10 °C at the end of Fh, For cals, eontinae heating te sample until the temperature rises from $00 °C + 10°C to 750°C = 15 °C in 1h, For cokes, continue beating the sample until the tempera- ture rises from 500°C 10°C to 950°C + 10°C in Lh. Continue to heat atthe fnal temperature (250 °C or 980 °C) until the test specimen reaches a constant mass or for an sxlitional 2h (Note 1), Allow the dish to cool, transfer to a agate moctar (Note 2), und grind 1 pass a 75 um (No. 200) USS.A. standard sieve. Reignit the ash at 750 °C or 950 °C for Teh to ensure complete and uniform oxidation of the ash 9.2.1 The tworstage ashing procedure allows pyrite sulfur to be oxidized and sulfur oxides expelled before most metal carbonates are decomposed. An ample supply of ait in the muffle furnace must be assured at all times to ensure complete oxidation of the pyitic sulfur and, more importantly, to efficiently remove the SO, formed. Because of tne possiblity (of SO product being sbsoched hy’ alkali and alkaline earth metal oxides (especially CaO), it is advisable to not ash high pyttic sulfur coals with coals that have high alkali or alkaline earth metal contems, or both. Noe 1—The D3I74 and D7S%2 ashing procedures used in the termination of ea from coal andr coke stmples and the D3682, 4326, and D639 ushing procedures use in prepering ash from coal or coke Samples. or both for-major and. minor element analysis are scceplable procedures for preparing esh for the fustbiity test. ‘None 2A mechanical agate mortar grind will save ime where many eterinatons are made 9.3. Preparation of Cones—Thoroughly mix the ignited ash ina mechanical mixer or on a sheet of glazed paper or oil cloth by raising first one comer to roll the ash over and then raising. ‘each of the other corners in rotation in the same manner until ‘each comer hus been raised five times or more 9.3.1 Take sufficient ash for the number of cones desired orn varies parts of the bulk ash, Moisten the ash with a few ‘drops of a dextrin solution and work it into a stiff plastic mass with a spatula, Press the plastic material firmly with a spatula into the cone mold to form the triangular pyramids. Strike off the exposed surfaces of the matcrial smooth and remove the ‘cones from the mold by applying slight pressure at the base with a suitably pointed spatula, Previous coating of the mold with a very thin layer of petroleum jelly, thinned with kerosene Gt necessary), or a very thin coating of a non-silicon-based mold release agent, aids in preventing adherence of the conos to the mold and in providing the sharp point and edges desired in the cone. With certain coal ashes, cones with sharp points and edges ean be obisined using distilled water in place of the extrin solution and without the use of petroleum jelly 9.3.2. Place the cones ina suitable location 1o dry sufficiently to permit handling without deformation. Mount she dried cones ‘vertically on a refractory tray. 9.32.1 Follow the manufacturer's recommendations for mounting the dry cones on commercially available support trays. 9.3.2.2 To prepare fresh support trays, moisten a portion of the well-mixed kaolin-alumina mixture with the minimum amount of water fo-make a workable, but stiff, plastic mass, and firmly press it into the support mold (Section 7.4). Strike fff the surface of the mass flat and smooth with astcel spal moistening with one or two drops of water if necessary to ‘obtain a smooth surface. A number of cones may be mounted fon one hase. Make shallow triangular depressions, not over 0.8 mm [42 in.] in depth, with a triangular file ground te the ccortect size to produce a depression to fit the base of the cone, and locate the cones sufficiently distant from adjacent cones so that oo merging of the fusing material of the cones shall occur during the test. Mount the cones vertically in the depressions ‘while the base is still wet without the use of ash or retmaciory as 4 mounting aid (Note 3 and Note 4), Non: 3—The tent of the na to be mounted in sulcenly sta prepared support with canes. "Nore Gold wires ean be mounted om each sone support beside the ash cones, and the gold melting point observed concurent with the ash fons i both oxizing and reducing stops, 94 Before running the test in a reducing atmosphere, dry the mounted cones and ignite (750 °C) for 1 h to remove all carbonaceous material. If'no organie material has been used in the preparation of the mounted coaes, this iguition step dhat follows the drying step may be omitted. The drying step must be retained, oar depression i to enable the comes manner to pennit handling of the 10, Furnace Temperature Check 10.1 It is recommended that the furnace temperature be checked after seven days of operation, This eleck is 40 be under routine test conditions using a reducing atmosphere and observing the melting point of gold. At the same time, check the quality of the reducing atmosphere by observing the melting point of nickel (WWYSON) VVSuaa VUaLHVEaS Isvuado™ ymUN 1» IUOMEUIEIUT WLSY ISUBSH YeMed IP NSA 4/0 IeNaIp Jul AdoD “YSN ‘ESTHET Wd ‘UAYDOYOYSUOD ISOM ‘OALIG INOGIH eG OOT ‘IEUORELUAIUT WASY BGI eH,ly 01857/01857M - 17 10.1.1 Insert a support with mounted pieces of gold and nickel wire (12.7 mm [' in.] lengths) into the test furnace Locate at the position used for tests of ash cones. 10.1.2 Establish the reducing gas atmosphere and heat the fumnace chamber in accordance with Hl. 10.1.3 Observe the temperatures shown on the meter when the pieces of wire melt 10.14 The indicated melting points should be within £5.5°C [10°F] of the followi 0 toes¢ 1848 -F) Neket 452°C [2685 °F] 10.15 IF the indicated melting point for gold wire falls putside of the desired range. readjust or recalibrate the readout device so that the average temperature from several observa tions of the gold melting point is within the specified range. 10.1.6 If the indicated melting point for nickel wire falls outside the desired range, after applying the comections as described in 10.1.5, the consisteney of indicated temperatures ‘and the subsequent appearance of the specimen should be examined closely. Erratic readings or failures to obtain melting at 1452 °C [2645 *F] can be duc to nickel oxidation caused by fan insufficiently reducing atmosphere. If a consistent error of ‘more than 14 °C [25 °F] is found, the furnace atmosphere and the temperature measurement equipment should be suspected of having faults; nocessary corrections should be made. U1, Procedure MAL Reducing Atmosphere Test: ILI Place the mounted test cones in the furnace at a temperature of not over 400°C [73°F] for the funace to provide sufficient time to purge the air from the uniform temperature zone and establish the desired atmosphere, 11.1.2 Ii the furnace temperature is below the temperature specified in 1.1.1, raise it rapicly to the specified temperature before intreclucing a reducing gas atmosphere. Then control the rate of heating to give @ rate of temperature inerease of 8 + 3°C [15 + 5°F]énin, Maintain this rate throughout the test. ng Atmosphere Test: 1.1.3.1 Place the mounted test cones in the furnace at a ‘temperature of net over 400 °C [750 °F] for the furnace. If the jumace temperature is below the temperature specified, raise it rapidly to the specified (emperature, then control the rate of heating to give a rate of temperature increase of 8 + 3.°C [15 = 5°F]fmin, Maintain this rate throughout the test. 1.1.3.2 Establish the oxidizing atmosphere surrounding the cones, a8 specified in 8.3 at the temperature specified in 1.1.3.1 for the respective furnace type, Maintain this atmo- sphete throughout the test. 12. Precision 12.1 The precision data for the determination of the fusion temperatures of eval and coke ash are shown Table 1 ‘TABLE 1 Repeatability and Reproducibility for Fusion ‘Temperatures of Coal and Coke Ash F c Repeninty Lim sD eproacty Lr (8) For eaucing smosorere: Ina esfomatontampertire. rr ms 7 Soteningforpertare ST 0S Nemgphercal temperature, MT mss Fue fomperatir, FT ry For ong amcepher: Ina! determatontperstue, TT wo 55 Sofening taroerature ST ce? Nemiseneres temperature, HT 1 8 Fae tonperatre FT 10088 12.1.1. Repearabitity (r} the value below which the absolute difference between two test results of soparate and consecutive test determinations, carried out on the same sample in the same laboratory by the same operator using the same apparatus on samples laken at random from a single quantity of homoxe- ‘neous material, may be expected to oceur with a probability of approximately 95 %. 12.1.2 Reproducibitity (R) the value below which the abso lute difference hetween two test results calculated 0 a dry basis, (Practice D3IS0) carried out in different laboratories using ‘samples taken at random from a single quantity of material is as homogeneous as possible, may be expected to oceur with 4 probability of approximately 95 %. (wWvSoy) VWSua VaaLHVCas ISvwadoN IMUN 13. Keywords 13.1 ash; coal; coke ASTAt Inrnasont takes no palin eapoctng the vay tary patent hts tered n concn win any Ro eaten nhs stra Users of Oe serdarecuprnsly sed ta oan 2 Ox wal ay sch pant hs, nd the sk (fanaa of suc ahs, ao only to own scons. ‘Th sane sutjctto anion at any te Bye raspons etal cormtoe ana must bo reviewed every ve years and \tncerviaoy eae raspproiegcrwindran, Your ammonite are mites her fer rasa" ays tenda's e coatona Sardar ‘and shows be adstesae w& ASTM inermaenal Mosier. 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