1、Designation: D1857/D1857M 04 (Reapproved 2010)Standard Test Method forFusibility of Coal and Coke Ash1This standard is issued under the fixed designation D1857/D1857M; the number immediately following the designation indicates theyear of original adoption or, in the case of revision, the year of las
2、t revision. A number in parentheses indicates the year of lastreapproval. A superscript 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. Scope1.1 This test method covers the observation
3、of the tempera-tures at which triangular pyramids (cones) prepared from coaland coke ash attain and pass through certain defined stages offusing and flow when heated at a specified rate in controlled,mildly reducing, and where desired, oxidizing atmospheres.1.2 The test method is empirical, and stri
4、ct observance ofthe requirements and conditions is necessary to obtain repro-ducible temperatures and enable different laboratories to obtainconcordant results.1.3 The values stated in either SI units or inch-pound unitsare to be regarded separately as standard. The values stated ineach system may n
5、ot be exact equivalents; therefore, eachsystem shall be used independently of the other. Combiningvalues from the two systems may result in non-conformancewith the standard.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibili
6、ty 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:2D2013 Practice for Preparing Coal Samples for AnalysisD3174 Test Method for Ash in the Analysis Sam
7、ple of Coaland Coke from Coal3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 The critical temperature points to be observed are asfollows, denoting the atmosphere used:3.1.2 fluid temperature, FTthe temperature at which thefused mass has spread out in a nearly flat layer with
8、amaximum height of 1.6 mm 116 in. as shown by the fifthcone, FT, in Fig. 1.3.1.3 hemispherical temperature, HTthe temperature atwhich the cone has fused down to a hemispherical lump atwhich point the height is one half the width of the base asshown by the fourth cone, HT, in Fig. 1.3.1.4 initial def
9、ormation temperature, ITthe temperatureat which the first rounding of the apex of the cone occurs.Shrinkage or warping of the cone ignored if the tip remainssharp. In Fig. 1, the first cone shown is an unheated one; thesecond cone IT is a typical cone at the initial deformation stage.3.1.5 softening
10、 temperature, STthe temperature at whichthe cone has fused down to a spherical lump in which theheight is equal to the width at the base as shown by the thirdcone, ST, in Fig. 1.4. Significance and Use4.1 Design of most coal combustion and coal conversionequipment anticipates that the ash either rem
11、ain solid orassume some degree of fluidity, depending on the particulardesign.Ash fusibility temperatures predict whether the ash willperform properly in the process for which the coal was chosen.5. Apparatus and Materials5.1 FurnaceAny gas-fired or electric furnace conformingto the following requir
12、ements may be used:5.1.1 Capable of maintaining a uniform temperature zone inwhich to heat the ash cones. This zone shall be such that thedifference in the melting point of 12.7-mm 12-in. pieces ofpure gold wire when mounted in place of the ash cones on thecone support shall be not greater than 11C
13、20F in areducing atmosphere test run.5.1.2 Capable of maintaining the desired atmosphere sur-rounding the cones during heating. The composition of theatmosphere, reducing or oxidizing, shall be maintained withinthe limits specified in Section 6. The desired atmosphere in thegas-fired furnace surroun
14、ding the cones shall be obtained byregulation of the ratio of gas to air in the combustion mixture.The desired atmosphere in the electric furnace shall be ob-tained by means of gases introduced into the heating chamber.1This test method is under the jurisdiction of ASTM Committee D05 on Coaland Coke
15、 and is the direct responsibility of D05.21 on Methods of Analysis.Current edition approved Sept. 1, 2010. Published November 2010. Originallyapproved 1961. Last previous edition approved 2004 as D1857 04. DOI: 10.1520/D1857-04R10.2For referenced ASTM standards, visit the ASTM website, www.astm.org,
16、 orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.The muffle shal
17、l be gas impervious, free from cracks, and theclosure plug tight-fitting. The gas supply tube shall be sealed tothe back wall of the preheating chamber and shall not extend tothe front of the preheating chamber against the perforatedbaffle.5.1.3 Capable of regulation so that the rate of temperaturer
18、ise shall be 8 6 3C 15 6 5F/min.5.1.4 Providing means of observing the ash cones during theheating. Observation on the same horizontal plane as thecone-support surface shall be possible.5.2 Cone MoldA commercially available cone mold asshown in Fig. 2. The cone shall be 19 mm 34 in. in height and6.4
19、 mm 14 in. in width at each side of the base which is anequilateral triangle. A steel spatula with a pointed tip, groundoff to fit the cone depression in the mold, is suitable forremoval of the ash cone.5.3 Optical Pyrometer or Thermocouple, for temperaturemeasurements, conforming to the following r
20、equirements:5.3.1 Optical PyrometerAn optical pyrometer of the dis-appearing filament type shall be used. The instrument shallhave been calibrated to be accurate within 11C 20F up to1400C 2550F and within 16C 30F from 1400 to 1600C2550 to 2900F (Note 1). The pyrometer filament shall besighted on the
21、 cones until the softening point temperature C(Fig. 1) has been passed, and then sighted on the cone support.The pyrometer shall have readable graduations not larger than5.5C 10F.NOTE 1The pyrometer equipment shall be standardized periodicallyby a suitably equipped standardizing laboratory such as t
22、hat of theNational Bureau of Standards, or checked periodically against equipmentcertified by the Bureau of Standards.5.3.2 ThermocoupleA thermocouple of platinum andplatinum-rhodium, protected from the furnace gases by aglazed porcelain sheath, shall be used with a high-resistancemillivoltmeter or
23、potentiometer accurate and readable to within5.5C 10F. The sheath shall be sealed to the furnace wall byalundum cement. The hot junction of the thermocouple shalltouch the end of the sheath and shall be located in the center ofthe muffle and immediately to the rear of the cones. Thethermocouple prot
24、ective sheath shall be checked periodicallyfor cracks. The thermocouple and its meter shall meet therequirements of Section 9. The potentiometer or millivoltmetershall be so located or adequately shielded as to prevent radiantand convection heating of the cold junction. The room tem-perature compens
25、ator shall be adjusted to the existing tempera-ture.5.4 Ash-Cone Refractory SupportThe ash cones shall bemounted on a refractory base composed of a mixture of equalparts by weight of kaolin and alumina conforming to thefollowing requirements:5.4.1 KaolinNF-grade powder passing a 75-m (No. 200)sieve.
26、5.4.2 Aluminum OxideReagent grade ignited powderpassing a 150-m (No. 100) sieve.5.5 Refractory Support MoldA mold with flat top andbottom surfaces to provide a refractory support of suitablethickness to minimize warping. A sidemold not over 6.4 mm14 in. high of any convenient shape, placed on an iro
27、n plateso that the top surface of the refractory mix can be struck offflat and parallel to the base by means of a straightedge, issatisfactory. For electric furnace use, legs not over18 in. 3mm long may be provided on the corners of the cone supportby suitable holes bored in the iron base plate of t
28、he mold.5.6 Gold Wire30.51-mm diameter (twenty-four gage) orlarger round wire of 99.98 % purity, but drawn from metal of99.99 % purity, and having a melting point of 1063C1945F.5.7 Nickel Wire40.51-mm diameter (twenty-four gage) orlarger round wire of CP nickel, 99.98 % pure, fully annealed,and havi
29、ng a melting point of 1452C 2645F.6. Test Atmosphere6.1 Gas-Fired Furnace:6.1.1 Reducing Atmosphere TestA mildly reducing atmo-sphere surrounding the cones shall be maintained during thetest in the gas-fired furnace. Hydrogen, hydrocarbons, andcarbon monoxide shall be considered as reducing gases;ox
30、ygen, carbon dioxide, and water vapor shall be considered asoxidizing gases. Nitrogen is inert. The ratio by volume of3Gold wire of this purity can be purchased from the Baker Dental Division ofEngelhard Industries, Inc., 850 Passaic Ave., East Newark, NJ 07029 or from LeicoIndustries, Inc., 250 W.
31、57th St., New York, NY 10019.4Nickel wire of this purity can be purchased with the additional specification ofhaving a minimum coefficient of resistance for 0 to 100C of 0.006 73 V/VC, fromLeico Industries, Inc., 250 W. 57th St., New York, NY 10019.FIG. 1 Critical Temperature PointsInch-poundUnits,i
32、n.SI Units,mm14 6.434 19.1112 38.12 50.23 76.2FIG. 2 Brass Cone MoldD1857/D1857M 04 (2010)2reducing gases to oxidizing gases in the atmosphere shall bebetween the limits of 20 to 80 and 80 to 20,5that is, on anitrogen-free basis, the total amount of reducing gases presentshall be between the limits
33、of 20 and 80 volume %. A flame152 to 203 mm 6 to 8 in. in height and tinged with yellowabove the furnace outlet has been found to provide anatmosphere within the specified limits.6.1.2 Oxidizing Atmosphere TestAn atmosphere contain-ing a minimum amount of reducing gases shall be maintainedsurroundin
34、g the cones during the test in the gas-fired furnace.On a nitrogen-free basis, the volume of reducing gases presentin the atmosphere shall not exceed volume 10 %. Combustionwith the maximum possible quantity of air with preservation ofthe specified rate of temperature increase has been found toprovi
35、de an atmosphere within the specified limits. A com-pletely blue flame, not over 50 mm 2 in. in height above theoutlet at the beginning of the test, provides the desiredatmosphere; and, by regulation of the combustion gas-air ratio,the specified atmosphere and temperature rise can be main-tained.6.2
36、 Electric Furnace:6.2.1 Reducing Atmosphere TestA regulated flow of gasof the nominal composition, 60 % carbon monoxide and 40 65 volume % carbon dioxide,6shall be maintained in the heatingchamber throughout the test (Note 2) in the electric furnace.The gas stream shall be regulated by any convenien
37、t means toprovide a measured flow of 1.3 to 1.5 furnace volumes perminute.6.2.2 Oxidizing Atmosphere TestA regulated stream of airshall be maintained throughout the test in the electric furnace.The gas stream shall be regulated by any convenient means toprovide a measured flow of 1.3 to 1.5 furnace
38、volumes perminute.NOTE 2Before using new cylinders of CO/CO2reducing gas, thecontents should be mixed according to the gas manufacturers recommen-dations. To assure that the gas remains mixed, the temperature of thecylinder contents should be maintained above the critical temperature atwhich CO2can
39、liquify and separate.7. Preparation of Ash7.1 Use coal or coke passing a 250-m (No. 60) sieveprepared in accordance with Method D2013, to obtain the ashby incineration in a well-ventilated muffle furnace. The quan-tity of coal or coke required will vary with the ash content;usually 3 to 5 g of ash w
40、ill be sufficient for cones for severalcheck determinations, if necessary. Spread out the coal or cokein a layer not over 6.4 mm 14 in. in depth in a fireclay orporcelain roasting dish. Place the dish in the cold muffle or onthe hearth at a low temperature and gradually heat to redness atsuch a rate
41、 as to avoid mechanical loss from too rapidexpulsion of volatile matter (Note 3). Complete the conversionto ash at a temperature of 800 to 900C 1470 to 1650F.Transfer the ash to an agate mortar (Note 4) and grind it so thatit will pass a 75-m (No. 200) sieve. Then spread the ash in athin layer in a
42、fireclay, silica, or porcelain dish and ignite it ina stream of oxygen for 112 h at 800 to 850C 1470 to 1560Fto ensure complete and uniform oxidation of the ash. Any tubeor muffle-type furnace which, when supplied with an oxygenflow of not less than one furnace volume in 5 min, willmaintain a highly
43、 oxidizing atmosphere and will be suitable.NOTE 3A heating rate conforming to that used for the ash determi-nation specified in Section 7 of Test Method D3174 is satisfactory.NOTE 4Amechanical agate mortar grinder will save time where manydeterminations are made. An iron mortar or pestle must not be
44、 used.8. Preparation of Cones8.1 Thoroughly mix the ignited ash in a mechanical mixeror on a sheet of glazed paper or oil cloth by raising first onecorner to roll the ash over and then raising each of the othercorners in rotation in the same manner until each corner hasbeen raised five times or more
45、.8.2 Take sufficient ash for the number of cones desired fromvarious parts of the bulk ash. Moisten the ash with a few dropsof a clear, filtered (if necessary) 10 % solution of dextrincontaining 0.1 % salicylic acid as a preservative and work itinto a stiff plastic mass with a spatula. Press the pla
46、stic materialfirmly with a spatula into the cone mold to form the triangularpyramids. Strike off the exposed surfaces of the materialsmooth and remove the cones from the mold by applyingpressure at the base with a suitably pointed spatula. Previouscoating of the mold with a thin layer of petroleum j
47、elly, thinnedwith kerosene (if necessary), aids in preventing adherence ofthe cones to the mold and in providing the sharp point andedges desired in the cone. With certain coal ashes, cones withsharp points and edges can be obtained using distilled water inplace of the dextrin solution and without t
48、he use of petroleumjelly.8.3 Place the cones in a suitable location to dry sufficientlyto permit handling without deformation. Mount the dried conevertically on a freshly prepared refractory base. Moisten aportion of the well-mixed kaolin-alumina mixture with theminimum amount of water to make a wor
49、kable, but stiff, plasticmass, and firmly press it into the support mold. Strike off thesurface of the mass flat and smooth with a steel spatula,moistening with one or two drops of water if necessary toobtain a smooth surface. A number of cones may be mountedon one base. Make shallow triangular depressions, not over 0.8mm 132 in. in depth, with a triangular file ground to thecorrect size to produce a depression to fit the base of the cone,and locate the cones sufficiently di
