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LOI Using TGA D7348 PDF
LOI Using TGA D7348 PDF
standard. No other units of measurement are included in this E 691 Practice for Conducting an Interlaboratory Study to
standard. Determine the Precision of a Test Method
1.3 This standard does not purport to address all of the 3. Terminology
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 3.1 Definitions—For definitions of terms used in these test
priate safety and health practices and determine the applica- methods, refer to Terminology D 121.
bility of regulatory limitations prior to use. 4. Summary of Test Method
2. Referenced Documents 4.1 Loss on ignition (LOI) is determined by measuring the
2.1 ASTM Standards: 2 loss in mass of the test specimen when heated under controlled
D 121 Terminology of Coal and Coke conditions of temperature, time, atmosphere, specimen mass,
D 3174 Test Method for Ash in the Analysis Sample of Coal and equipment specifications. The LOI can be determined by
and Coke from Coal measuring the mass loss in a single procedure or in a two-step
D 3180 Practice for Calculating Coal and Coke Analyses procedure in which mass losses, equivalent to the moisture and
from As-Determined to Different Bases ash values of the test specimen, are determined.
D 3682 Test Method for Major and Minor Elements in 5. Significance and Use
Combustion Residues from Coal Utilization Processes
D 3683 Test Method for Trace Elements in Coal and Coke 5.1 LOI refers to the mass loss of a combustion residue
Ash by Atomic Absorption whenever it is heated in an air or oxygen atmosphere to high
D 4326 Test Method for Major and Minor Elements in Coal temperatures. In the cement industry, use of the term LOI
and Coke Ash By X-Ray Fluorescence normally refers to a mass loss in a sample heated to 950°C. To
D 5142 Test Methods for Proximate Analysis of the Analy- combustion engineers, the term LOI normally refers to mass
sis Sample of Coal and Coke by Instrumental Procedures losses in samples heated to temperatures normally less than
D 6316 Test Method for Determination of Total, Combus- 950°C. These test methods establish a procedure for determin-
tible and Carbonate Carbon in Solid Residues from Coal ing LOI values for combustion residues heated to 750°C or
and Coke 950°C. LOI values from these test methods can be used by
D 6349 Test Method for Determination of Major and Minor industries that utilize combustion residues in various processes
Elements in Coal, Coke, and Solid Residues from Com- and products.
5.2 If the solid combustion residue is heated to estimate the
combustible or unburned carbon in the sample, it has been
shown that LOI and estimation of unburned carbon do not
1
These test methods are under the jurisdiction of ASTM Committee D05 on Coal necessarily agree well with each other and that LOI should not
and Coke and is the direct responsibility of Subcommittee D05.29 on Major
Elements in Ash and Trace Elements of Coal.
be used as an estimate of unburned carbon in all combustion
Current edition approved Oct. 15, 2008. Published October 2008. Originally
approved in 2007. Last previous edition approved in 2007 as D 7348–07.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service as service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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ash for the determination of the concentrations of trace balance is a separate piece of apparatus.
elements, use the heating procedure described in Test Methods 7.5 Operation of the instrumental system in its entirety shall
D 3683 and D 6357. be verified in accordance with the manufacturer’s operating
instructions.
NOTE 1—Combustion residues produced in furnace operations or other
combustion systems can differ from the ash yield, as determined in Test 7.6 Venting Equipment—Combustion and decomposition
Methods D 3174 and D 5142, because combustion conditions influence gases evolved during the test procedures shall be vented from
the chemistry and amount of ash. Combustion causes an expulsion of all the laboratory and suitable venting equipment shall be installed
water, the loss of carbon dioxide from carbonates, the conversion of metal in the vicinity of the apparatus.
sulfides into metal oxides, metal sulfates and sulfur oxides, and other
chemical reactions. Likewise, the “ash” obtained after igniting combustion 8. Reagents and Materials
residues can differ in composition and amount from Test Methods D 3174
8.1 Drying Gases—Air dried to a moisture content of 1.9
and D 5142 ash yields because of different heating procedures, combus-
tion of unburned carbon, and decomposition of materials in the residue. mg/L or less (dew point –10°C or less). Nitrogen (99.5 %
purity) is normally used with the macro TGA system. Argon
6. Interferences can also be used.
6.1 There are no known interferences for these test methods. 8.2 Oxidizing Gases—Oxygen (99.5 % purity) or air.
7. Apparatus 9. Hazards
7.1 Furnace—The apparatus shall consist of a furnace with 9.1 The user shall insure acceptable documented safety
a cavity large enough to accept multiple crucibles. The furnace procedures are in place for the handling of all reagents and test
shall be constructed so the cavity is surrounded by a suitable materials and for the operation of laboratory equipment speci-
refractory and insulated so as to develop a uniform temperature fied for these test methods.
in all parts of the cavity but with a minimum free space. The 10. Sampling, Test Specimens, and Test Units
furnace shall be capable of being heated rapidly (10°C/min or
faster) from ambient to 950°C. The temperature shall be 10.1 The sample used for analysis shall be thoroughly
monitored and maintained at values specific to each of the mixed and of such fineness to pass through a 250-µm (No. 60)
determinations. Provisions shall be made to introduce drying sieve. Pulverizing the sample to this fineness is required.
and oxidizing gases and to remove products of drying, decom- 11. Preparation of Apparatus
position, and combustion. A recommended flow rate is one
furnace volume change per minute, but higher flow rates (that 11.1 For LOI determinations using a macro TGA, follow the
is, two furnace volumes per minute as in some other standard manufacturer’s recommended procedure for verifying system
test methods for coal and coke) are acceptable. The furnace can stability and for loading and taring the crucibles. Various
be a stand alone muffle furnace or a computer-controlled modes of operation are possible depending on the instrument
macrothermogravimetric analyzer (macro TGA) system. In used and the manner in which the determinations are com-
macro TGA, a sample size of 1 g (or larger) is used. In a typical pleted. The instrument can be programmed to terminate the test
analysis, the temperature is ramped from ambient to a specific whenever the test specimens and crucibles have reached a
temperature and held at that temperature for a prescribed length constant mass. Typically, crucibles are weighed automatically
of time. In thermogravimetric analysis, the mass of a sample in at specified intervals, and the analysis is complete whenever
a controlled atmosphere is recorded repeatedly as a function of three successive weighings agree within a plateau deviation
temperature or time. specified for the instrument. Constant mass is defined as a point
7.2 Drying Oven—For determining the moisture in solid where the mass change is # 0.05 % of a nine-minute period,
combustion residue samples, use a drying oven with openings either by using three successive weighings (for some TGAs) or
for drying gas circulation and capable of temperature regula- a fixed nine-minute period (for some TGAs). This mass change
tion between the limits of 104 and 110°C. A drying gas flow of 0.05% is equivalent to 0.0005 g for a 1.0000 g sample.
rate of approximately one volume change per minute is Alternately, the instrument can be programmed to allow for
recommended but higher flow rates, that is, two volume moisture determination by heating the test specimens for a
specified time period (for example, 1 h) at the prescribed
temperature limits.
3
Burris S.C. , Li, D., and Riley J.T, “Comparison of Heating Losses and Macro
11.2 When using a muffle furnace for LOI determinations,
Thermogravimetric Analysis Procedures for Estimating Unburned Carbon in Com- always start the test with the muffle furnace at ambient
bustion Residues,” Energy Fuels Vol 19 2005, pp. 1493-1502. temperature.
Table 1. The precision characterized by the repeatability (S r, r) the LOI is not currently available. NIST Standard Reference
and reproducibility (SR, R) is described in Tables A1.1-A1.4 in Material 1880a, Portland Cement and NIST Standard Refer-
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Annex A1. ence Material 2696, Silica Fume provide a reference value for
16.1.1 Repeatability Limit (r)—The value below which the the LOI, was included in the interlaboratory study with the
absolute difference between two test results of separate and results shown in Table 2.
consecutive test determinations, carried out on the same 16.3 An interlaboratory study, designed consistent with
sample in the same laboratory by the same operator using the Practice E 691, was conducted in 2006. Twenty labs partici-
same apparatus on samples taken at random from a single pated. The details of the study and supporting data are given in
quantity of homogeneous 250 µm (No. 60 USA Standard sieve) Research Reports RR:D05-1031 and RR:D05-1036.4
material, may be expected to occur with a probability of
approximately 95 %. 17. Keywords
16.1.2 Reproducibility Limit (R)—The value below which 17.1 ash; combustion residues; loss on ignition; LOI; macro
the absolute difference between two test results, carried out in thermogravimetric analysis; macro TGA
different laboratories using samples taken at random from a
single quantity of 250 µm (No. 60 USA Standard sieve)
material that is as homogeneous as possible, may be expected 4
Supporting data have been filed at ASTM International Headquarters and may
to occur with a probability of approximately 95 %. be obtained by requesting Research Report RR:D05-1031.
16.2 Bias—A bias statement is not available because a Supporting data have been filed at ASTM International Headquarters and may be
suitable Certified Reference Material with a certified value for obtained by requesting Research Report RR:D05-1036.
ANNEX
(Mandatory Information)
A1.1 The precision of these test methods, characterized by determined for the following materials as listed in Tables
repeatability (Sr, r) and reproducibility (SR, R) has been A1.1-A1.4.
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TABLE A1.2 Repeatability (Sr, r) and Reproducibility (SR, R) Parameters Used for Calculation of Precision Statement for Macro-TGA,
Two-Step Procedure for Dry Basis LOI (750°C and 950°C)
Material Average % LOI Sr SR r R
750°C
EBIT 11.3225 0.0494 0.1057 0.1383 0.296
NDL 2.153 0.0532 0.0684 0.1488 0.1915
BB 2.3175 0.0529 0.054 0.1483 0.1512
CB 9.625 0.0392 0.0915 0.1097 0.2563
TXL 3.8755 0.0939 0.1297 0.2628 0.3631
BDPS 0.967 0.0637 0.0706 0.1785 0.1978
SHND 4.6285 0.0524 0.0661 0.1467 0.185
7FA 4.273 0.0561 0.058 0.157 0.1623
8FA 10.6325 0.0759 0.1105 0.2125 0.3094
NIST 2696 2.2687 0.1154 0.1471 0.323 0.4119
950°C
EBIT 11.3795 0.0827 0.1276 0.2315 0.3572
NDL 2.1886 0.0445 0.0539 0.1245 0.1508
BB 2.3932 0.0535 0.0624 0.1498 0.1748
CB 9.6830 0.0491 0.1078 0.1375 0.3017
TXL 3.9339 0.0669 0.0763 0.1874 0.2137
BDPS 0.9564 0.0335 0.0465 0.0938 0.1303
SHND 4.6620 0.0444 0.0565 0.1242 0.1582
7FA 4.2350 0.0861 0.0916 0.2412 0.2564
8FA 10.5536 0.1251 0.1487 0.3502 0.4164
NIST 1880a 1.0484 0.0689 0.0915 0.1930 0.2561
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TABLE A1.4 Repeatability (Sr, r) and Reproducibility (SR, R) Parameters Used for Calculation of Precision Statement for Muffle
Furnace, Two-Step Procedure for Dry Basis LOI (750°C and 950°C)
Material Average % LOI Sr SR r R
750°C
EBIT 11.4039 0.1071 0.1762 0.2998 0.4933
NDL 2.0889 0.081 0.1854 0.2268 0.5191
BB 2.3739 0.0526 0.1055 0.1472 0.2954
CB 9.705 0.0757 0.1164 0.212 0.3259
TXL 3.5261 0.0788 0.1588 0.2206 0.4446
BDPS 0.9068 0.0554 0.1019 0.1551 0.2852
SHND 4.5211 0.1126 0.1701 0.3154 0.4764
7FA 4.2629 0.0965 0.1435 0.2703 0.4019
8FA 10.7336 0.1301 0.2452 0.3643 0.6865
NIST 2696 2.1164 0.3207 0.3351 0.898 0.9384
950°C
EBIT 11.4738 0.0989 0.2104 0.2769 0.5891
NDL 2.4234 0.3403 0.6485 0.9529 1.8159
BB 2.4406 0.1309 0.1605 0.3665 0.4493
CB 9.8116 0.1055 0.1958 0.2955 0.5483
TXL 3.5737 0.1866 0.3659 0.5225 1.0246
BDPS 0.8663 0.1153 0.1914 0.3227 0.5359
SHND 4.7912 0.2520 0.4970 0.7057 1.3916
7FA 4.3513 0.1151 0.2462 0.3223 0.6894
8FA 10.6187 0.1165 0.2250 0.3263 0.6299
NIST 1880a 0.7931 0.1864 0.3862 0.5218 1.0813
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