1、Designation: D 7348 08Standard Test Methods forLoss on Ignition (LOI) of Solid Combustion Residues1This standard is issued under the fixed designation D 7348; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revisio
2、n. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 These test methods cover the determination of the massloss from solid combustion residues upon heating in an air oroxygen atmosphe
3、re to a prescribed temperature. The mass losscan be due to the loss of moisture, carbon, sulfur, and so forth,from the decomposition or combustion of the residue.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 stand
4、ard does not purport to address all of thesafety concerns, if any, 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 AS
5、TM Standards:2D 121 Terminology of Coal and CokeD 3174 Test Method forAsh in theAnalysis Sample of Coaland Coke from CoalD 3180 Practice for Calculating Coal and Coke Analysesfrom As-Determined to Different BasesD 3682 Test Method for Major and Minor Elements inCombustion Residues from Coal Utilizat
6、ion ProcessesD 3683 Test Method for Trace Elements in Coal and CokeAsh by Atomic AbsorptionD 4326 Test Method for Major and Minor Elements in Coaland Coke Ash By X-Ray FluorescenceD 5142 Test Methods for Proximate Analysis of the Analy-sis Sample of Coal and Coke by Instrumental ProceduresD 6316 Tes
7、t Method for Determination of Total, Combus-tible and Carbonate Carbon in Solid Residues from Coaland CokeD 6349 Test Method for Determination of Major and MinorElements in Coal, Coke, and Solid Residues from Com-bustion of Coal and Coke by Inductively CoupledPlasmaAtomic Emission SpectrometryD 6357
8、 Test Methods for Determination of Trace Elementsin Coal, Coke, C = mass of test specimen after drying in moisture test,g;D = mass of ash residue after heating at 750C or 950C,g; andLOI = percent loss on ignition as determined in the testspecimen.15. Report15.1 Report the temperature or method used,
9、 or both, todetermine the LOI vales. For reporting analyses to other thanthe as-determined basis, refer to Practice D 3180.16. Precision and Bias16.1 PrecisionThe precision data of these test method forthe determination of LOI for combustion residues are shown inD7348083Table 1. The precision charac
10、terized by the repeatability (Sr,r)and reproducibility (SR, R) is described in Tables A1.1-A1.4 inAnnex A1.16.1.1 Repeatability Limit (r)The value below which theabsolute difference between two test results of separate andconsecutive test determinations, carried out on the samesample in the same lab
11、oratory by the same operator using thesame apparatus on samples taken at random from a singlequantity of homogeneous 250 m (No. 60 USAStandard sieve)material, may be expected to occur with a probability ofapproximately 95 %.16.1.2 Reproducibility Limit (R)The value below whichthe absolute difference
12、 between two test results, carried out indifferent laboratories using samples taken at random from asingle quantity of 250 m (No. 60 USA Standard sieve)material that is as homogeneous as possible, may be expectedto occur with a probability of approximately 95 %.16.2 BiasA bias statement is not avail
13、able because asuitable Certified Reference Material with a certified value forthe LOI is not currently available. NIST Standard ReferenceMaterial 1880a, Portland Cement and NIST Standard Refer-ence Material 2696, Silica Fume provide a reference value forthe LOI, was included in the interlaboratory s
14、tudy with theresults shown in Table 2.16.3 An interlaboratory study, designed consistent withPractice E 691, was conducted in 2006. Twenty labs partici-pated. The details of the study and supporting data are given inResearch Reports RR:D05-1031 and RR:D05-1036.417. Keywords17.1 ash; combustion resid
15、ues; loss on ignition; LOI; macrothermogravimetric analysis; macro TGA4Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D05-1031.Supporting data have been filed atASTM International Headquarters and may beobtained by requesting Re
16、search Report RR:D05-1036.TABLE 1 Concentration Range and Limits of Repeatability and Reproducibility for LOI (750C and 950C) Test MethodsConcentrationRange,PercentRepeatability Limit,rReproducibility Limit,R750CSingle-stepProcedureMacro-TGA 1.111.7 0.29 0.37Muffle Furnace 1.011.0 0.22 0.28Two-StepP
17、rocedure(drybasis)Macro-TGA 0.9711.3 0.19 0.27Muffle Furnace 0.911.4 0.37 0.52950CSingle-stepProcedureMacro-TGA 1.1-11.7 0.21 0.28Muffle Furnace 1.1-11.8 0.47 0.75Two-StepProcedureMacro-TGA 1.0-11.4 0.17 0.22Muffle Furnace 0.9-11.5 0.36 0.71D7348084ANNEX(Mandatory Information)A1. PRECISION STATISTIC
18、SA1.1 The precision of these test methods, characterized byrepeatability (Sr, r) and reproducibility (SR, R) has beendetermined for the following materials as listed in TablesA1.1-A1.4.TABLE 2 Comparison of the Percent LOI (750C and 950C)Value (Reference and Not Certified) for NIST 1880a and 2696 wi
19、ththe Interlaboratory Study Values750CNIST 2696Reference ValueMacro TGADryMuffle FurnaceDry% LOI (dry) 2.12 6 0.10 2.25 2.12Bias 0.14 0.00950CNIST 1880aReference ValueMacro TGATwo-stepMuffle FurnaceTwo-step% LOI (as-received) 1.320 1.345 1.084Bias 0.025 0.236D7348085TABLE A1.1 Repeatability (Sr, r)
20、and Reproducibility (SR, R) Parameters Used for Calculation of Precision Statement for Macro-TGA,One-Step Procedure for LOI (750C and 950C)Material Average % LOI SrSRrR750CEBIT 11.7025 0.1054 0.1186 0.2952 0.3321NDL 2.4303 0.0958 0.1082 0.2682 0.3029BB 2.495 0.0467 0.0624 0.1306 0.1748CB 9.8156 0.07
21、06 0.093 0.1977 0.2605TXL 4.0441 0.1604 0.1708 0.4491 0.4782BDPS 1.0722 0.038 0.0645 0.1064 0.1807SHND 4.8909 0.0852 0.096 0.2384 0.26887FA 4.4325 0.1477 0.1874 0.4135 0.52488FA 11.0131 0.118 0.2103 0.3303 0.5887950CEBIT 11.6509 0.0940 0.1549 0.2632 0.4336NDL 2.4157 0.1359 0.1415 0.3806 0.3961BB 2.5
22、407 0.0822 0.1119 0.2302 0.3132CB 9.8302 0.0851 0.1420 0.2382 0.3976TXL 4.0582 0.1005 0.1160 0.2814 0.3248BDPS 1.0714 0.0604 0.0604 0.1691 0.1691SHND 4.9136 0.0639 0.0680 0.1789 0.19057FA 4.4198 0.1091 0.1116 0.3054 0.31268FA 10.8991 0.0850 0.1613 0.2380 0.4516TABLE A1.2 Repeatability (Sr, r) and Re
23、producibility (SR, R) Parameters Used for Calculation of Precision Statement for Macro-TGA,Two-Step Procedure for Dry Basis LOI (750C and 950C)Material Average % LOI SrSRrR750CEBIT 11.3225 0.0494 0.1057 0.1383 0.296NDL 2.153 0.0532 0.0684 0.1488 0.1915BB 2.3175 0.0529 0.054 0.1483 0.1512CB 9.625 0.0
24、392 0.0915 0.1097 0.2563TXL 3.8755 0.0939 0.1297 0.2628 0.3631BDPS 0.967 0.0637 0.0706 0.1785 0.1978SHND 4.6285 0.0524 0.0661 0.1467 0.1857FA 4.273 0.0561 0.058 0.157 0.16238FA 10.6325 0.0759 0.1105 0.2125 0.3094NIST 2696 2.2687 0.1154 0.1471 0.323 0.4119950CEBIT 11.3795 0.0827 0.1276 0.2315 0.3572N
25、DL 2.1886 0.0445 0.0539 0.1245 0.1508BB 2.3932 0.0535 0.0624 0.1498 0.1748CB 9.6830 0.0491 0.1078 0.1375 0.3017TXL 3.9339 0.0669 0.0763 0.1874 0.2137BDPS 0.9564 0.0335 0.0465 0.0938 0.1303SHND 4.6620 0.0444 0.0565 0.1242 0.15827FA 4.2350 0.0861 0.0916 0.2412 0.25648FA 10.5536 0.1251 0.1487 0.3502 0.
26、4164NIST 1880a 1.0484 0.0689 0.0915 0.1930 0.2561D7348086ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such paten
27、t rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited eithe
28、r for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair he
29、aring you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standar
30、d may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).TABLE A1.3 Repeatability (Sr, r) and Reproducibility (SR, R) Parameters Used for Calculation of Precision Statement for Muff
31、leFurnace, One-Step Procedure for LOI (750C and 950C)Material Average % LOI SrSRrR750CEBIT 11.64 0.0709 0.0924 0.1986 0.2587NDL 2.2763 0.123 0.1306 0.3443 0.3657BB 2.4925 0.0608 0.0612 0.1702 0.1714CB 9.8129 0.0395 0.0588 0.1105 0.1647TXL 3.5796 0.0713 0.1111 0.1998 0.3111BDPS 1.0208 0.0571 0.0664 0
32、.1598 0.186SHND 4.6871 0.081 0.0986 0.2267 0.27627FA 4.4367 0.1041 0.1047 0.2914 0.29328FA 10.9746 0.0843 0.1343 0.236 0.3759950CEBIT 11.7936 0.1086 0.2246 0.3041 0.6289NDL 2.6050 0.1494 0.1684 0.4184 0.4716CB 9.9729 0.2084 0.2572 0.5835 0.7202TXL 3.7696 0.1714 0.4017 0.4798 1.1248BDPS 1.0718 0.1665
33、 0.2397 0.4663 0.6711SHND 4.8404 0.2258 0.3418 0.6323 0.95697FA 4.4568 0.1221 0.1625 0.3418 0.4551TABLE A1.4 Repeatability (Sr, r) and Reproducibility (SR, R) Parameters Used for Calculation of Precision Statement for MuffleFurnace, Two-Step Procedure for Dry Basis LOI (750C and 950C)Material Averag
34、e % LOI SrSRrR750CEBIT 11.4039 0.1071 0.1762 0.2998 0.4933NDL 2.0889 0.081 0.1854 0.2268 0.5191BB 2.3739 0.0526 0.1055 0.1472 0.2954CB 9.705 0.0757 0.1164 0.212 0.3259TXL 3.5261 0.0788 0.1588 0.2206 0.4446BDPS 0.9068 0.0554 0.1019 0.1551 0.2852SHND 4.5211 0.1126 0.1701 0.3154 0.47647FA 4.2629 0.0965
35、 0.1435 0.2703 0.40198FA 10.7336 0.1301 0.2452 0.3643 0.6865NIST 2696 2.1164 0.3207 0.3351 0.898 0.9384950CEBIT 11.4738 0.0989 0.2104 0.2769 0.5891NDL 2.4234 0.3403 0.6485 0.9529 1.8159BB 2.4406 0.1309 0.1605 0.3665 0.4493CB 9.8116 0.1055 0.1958 0.2955 0.5483TXL 3.5737 0.1866 0.3659 0.5225 1.0246BDPS 0.8663 0.1153 0.1914 0.3227 0.5359SHND 4.7912 0.2520 0.4970 0.7057 1.39167FA 4.3513 0.1151 0.2462 0.3223 0.68948FA 10.6187 0.1165 0.2250 0.3263 0.6299NIST 1880a 0.7931 0.1864 0.3862 0.5218 1.0813D7348087
