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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles

for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D7348 − 21

Standard Test Methods for


Loss on Ignition (LOI) of Solid Combustion Residues1
This standard is issued under the fixed designation D7348; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope D4326 Test Method for Major and Minor Elements in Coal
1.1 These test methods cover the determination of the mass Ash By X-Ray Fluorescence
loss from solid combustion residues upon heating in an air or D6316 Test Method for Determination of Total, Combustible
oxygen atmosphere to a prescribed temperature. The mass loss and Carbonate Carbon in Solid Residues from Coal and
can be due to the loss of moisture, carbon, sulfur, and so forth, Coke
from the decomposition or combustion of the residue. D6349 Test Method for Determination of Major and Minor
Elements in Coal, Coke, and Solid Residues from Com-
1.2 Units—The values stated in SI units are to be regarded bustion of Coal and Coke by Inductively Coupled
as standard. The values given in parentheses after SI units are Plasma—Atomic Emission Spectrometry
provided for information only and are not considered standard. D6357 Test Methods for Determination of Trace Elements in
1.3 This standard does not purport to address all of the Coal, Coke, and Combustion Residues from Coal Utiliza-
safety concerns, if any, associated with its use. It is the tion Processes by Inductively Coupled Plasma Atomic
responsibility of the user of this standard to establish appro- Emission Spectrometry, Inductively Coupled Plasma
priate safety, health, and environmental practices and deter- Mass Spectrometry, and Graphite Furnace Atomic Ab-
mine the applicability of regulatory limitations prior to use. sorption Spectro
1.4 This international standard was developed in accor- D7582 Test Methods for Proximate Analysis of Coal and
dance with internationally recognized principles on standard- Coke by Macro Thermogravimetric Analysis
ization established in the Decision on Principles for the D8146 Guide for Evaluating Test Method Capability and
Development of International Standards, Guides and Recom- Fitness for Use
mendations issued by the World Trade Organization Technical E177 Practice for Use of the Terms Precision and Bias in
Barriers to Trade (TBT) Committee. ASTM Test Methods
E691 Practice for Conducting an Interlaboratory Study to
2. Referenced Documents Determine the Precision of a Test Method
2.1 ASTM Standards:2
D121 Terminology of Coal and Coke 3. Terminology
D3174 Test Method for Ash in the Analysis Sample of Coal 3.1 Definitions—For definitions of terms used in these test
and Coke from Coal methods, refer to Terminology D121.
D3180 Practice for Calculating Coal and Coke Analyses
from As-Determined to Different Bases 4. Summary of Test Method
D3682 Test Method for Major and Minor Elements in 4.1 Loss on ignition (LOI) is determined by measuring the
Combustion Residues from Coal Utilization Processes loss in mass of the test specimen when heated under controlled
D3683 Test Method for Trace Elements in Coal and Coke conditions of temperature, time, atmosphere, specimen mass,
Ash by Atomic Absorption (Withdrawn 2018)3 and equipment specifications. The LOI can be determined by
measuring the mass loss in a single procedure or in a two-step
1
procedure in which mass losses, equivalent to the moisture and
These test methods are under the jurisdiction of ASTM Committee D05 on Coal
and Coke and are the direct responsibility of Subcommittee D05.29 on Major ash values of the test specimen, are determined.
Elements in Ash and Trace Elements of Coal.
Current edition approved Oct. 1, 2021. Published November 2021. Originally 5. Significance and Use
approved in 2007. Last previous edition approved in 2013 as D7348 – 13. DOI:
10.1520/D7348-21. 5.1 LOI refers to the mass loss of a combustion residue
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or whenever it is heated in an air or oxygen atmosphere to high
contact ASTM Customer Service as [email protected]. For Annual Book of ASTM temperatures. In the cement industry, use of the term LOI
Standards volume information, refer to the standard’s Document Summary page on
normally refers to a mass loss in a sample heated to 950 °C. To
the ASTM website.
3
The last approved version of this historical standard is referenced on combustion engineers, the term LOI normally refers to mass
www.astm.org. losses in samples heated to temperatures normally less than

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

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D7348 − 21
950 °C. These test methods establish a procedure for determin- to a specific temperature and held at that temperature for a
ing LOI values for combustion residues heated to 750 °C or prescribed length of time. In thermogravimetric analysis, the
950 °C. LOI values from these test methods can be used by mass of a sample in a controlled atmosphere is recorded
industries that utilize combustion residues in various processes repeatedly as a function of temperature or time.
and products. 7.2 Drying Oven—For determining the moisture in solid
5.2 If the solid combustion residue is heated to estimate the combustion residue samples, use a drying oven with openings
combustible or unburned carbon in the sample, it has been for drying gas circulation and capable of temperature regula-
shown that LOI and estimation of unburned carbon do not tion between the limits of 104 °C and 110 °C. A drying gas
necessarily agree well with each other and that LOI should not flow rate of approximately one volume change per minute is
be used as an estimate of unburned carbon in all combustion recommended but higher flow rates, that is, two volume
residues.4 Direct determination of unburned (combustible) changes per minute, as in some other standard test methods for
carbon can be carried out using Test Method D6316. coal and coke, are acceptable.
5.3 If the solid combustion residue is heated to prepare an 7.3 Crucibles, use a crucible of a convenient form that
ash for the determination of the mass fractions of major and allows extensive contact between the specimen and reactant
minor elements, use the heating procedure described in Test gas. The crucibles can be made of porcelain, fused silica, or
Methods D3682, D4326, and D6349, or the procedures for the similar materials. The crucibles shall have the dimensions
750 °C LOI determination described in these test methods specified by the instrument manufacturer.
(Method A). 7.4 Balance, sensitive to 0.1 mg. In the macro TGA, the
5.4 If the solid combustion residue is heated to prepare an balance is an integral part of the system. For other systems, the
ash for the determination of the mass fractions 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
D3683 and D6357. be verified in accordance with the manufacturer’s operating
NOTE 1—Combustion residues produced in furnace operations or other instructions.
combustion systems can differ from the ash yield, as determined in Test
Methods D3174 and D7582, because combustion conditions influence the
7.6 Venting Equipment—Combustion and decomposition
chemistry and amount of ash. Combustion causes an expulsion of all gases evolved during the test procedures shall be vented from
water, the loss of carbon dioxide from carbonates, the conversion of metal the laboratory and suitable venting equipment shall be installed
sulfides into metal oxides, metal sulfates and sulfur oxides, and other in the vicinity of the apparatus.
chemical reactions. Likewise, the “ash” obtained after igniting combustion
residues can differ in composition and amount from Test Methods D3174 8. Reagents and Materials
and D7582 ash yields because of different heating procedures, combustion
of unburned carbon, and decomposition of materials in the residue. 8.1 Drying Gases—Air dried to a moisture content of
1.9 mg ⁄L or less (dew point –10 °C or less). Nitrogen (99.5 %
6. Interferences purity) is normally used with the macro TGA system. Argon
6.1 There are no known interferences for these test methods. can also be used.
8.2 Oxidizing Gases—Oxygen (99.5 % purity) or air.
7. Apparatus
7.1 Furnace—The apparatus shall consist of a furnace with 9. Hazards
a cavity large enough to accept multiple crucibles. The furnace 9.1 The user shall insure acceptable documented safety
shall be constructed so the cavity is surrounded by a suitable procedures are in place for the handling of all reagents and test
refractory and insulated so as to develop a uniform temperature materials and for the operation of laboratory equipment speci-
in all parts of the cavity but with a minimum free space. The fied for these test methods.
furnace shall be capable of being heated rapidly (10 °C ⁄min or
faster) from ambient to 950 °C. The temperature shall be 10. Sampling, Test Specimens, and Test Units
monitored and maintained at values specific to each of the 10.1 The sample used for analysis shall be thoroughly
determinations. Provisions shall be made to introduce drying mixed and of such fineness to pass through a 250 µm (No. 60)
and oxidizing gases and to remove products of drying, sieve. Pulverizing the sample to this fineness is required.
decomposition, and combustion. A recommended flow rate is
one furnace volume change per minute, but higher flow rates 11. Preparation of Apparatus
(that is, two furnace volumes per minute, as in some other 11.1 For LOI determinations using a macro TGA, follow the
standard test methods for coal and coke) are acceptable. The manufacturer’s recommended procedure for verifying system
furnace can be a stand alone muffle furnace or a computer- stability and for loading and taring the crucibles. Various
controlled macro thermogravimetric analyzer (macro TGA) modes of operation are possible depending on the instrument
system. In macro TGA, a sample size of 1 g (or larger) is used. used and the manner in which the determinations are com-
In a typical analysis, the temperature is ramped from ambient pleted. The instrument can be programmed to terminate the test
whenever the test specimens and crucibles have reached a
4
Burris S.C., Li, D., and Riley J.T, “Comparison of Heating Losses and Macro
constant mass. Typically, the mass of a crucible is determined
Thermogravimetric Analysis Procedures for Estimating Unburned Carbon in Com- automatically at specified intervals, and the analysis is com-
bustion Residues,” Energy Fuels Vol 19, 2005, pp. 1493–1502. plete whenever three successive mass determinations agree

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D7348 − 21
within a plateau deviation specified for the instrument. Con- 13.5 LOI can be determined in a single-step procedure using
stant mass is defined as a point where the mass change is a muffle furnace (see 7.1). Place approximately 1 g of com-
≤ 0.05 % of a 9 min period, either by using three successive bustion residue into a crucible of known mass and determine
mass determinations (for some TGAs) or a fixed 9 min period the mass of the test specimen to the nearest 0.1 mg. Place the
(for some TGAs). This mass change of 0.05 % is equivalent to crucible with the test specimen, without a cover, into the cold
0.0005 g for a 1.0000 g sample. Alternately, the instrument can furnace. Turn on the oxidizing gas (see 8.2) and adjust the flow
be programmed to allow for moisture determination by heating to approximately one furnace volume change per minute.
the test specimens for a specified time period (for example, 1 Gradually raise the temperature of the furnace at a rate such
h) at the prescribed temperature limits. that the furnace temperature reaches 500 °C 6 10 °C at the end
11.2 When using a muffle furnace for LOI determinations, of 1 h. For Method A, continue the gradual heating of the
always start the test with the muffle furnace at ambient samples until the temperature rises from 500 °C 6 10 °C to
temperature. 750 °C 6 15 °C at the end of 1 h. For Method B, continue the
gradual heating until the temperature rises from 500 °C 6
12. Conditioning 10 °C to 950 °C 6 20 °C at the end of 1 h. Maintain the higher
12.1 Heat new crucibles for use in these test methods under temperature until the combustion residue test specimens reach
the conditions of the test and cool before use. a constant mass or for an additional 2 h.
13. Procedure 13.6 LOI can be determined in a two-step procedure using a
muffle furnace and a drying oven (see 7.2). To determine
13.1 In these procedures Method A refers to LOI determi- moisture, place approximately 1 g of combustion residue into
nations at 750 °C whereas Method B refers to LOI determina- a crucible of known mass and determine the mass of the test
tions at 950 °C. specimen to the nearest 0.1 mg. Place the crucible with the test
13.2 For LOI determinations using a macro TGA, the specimen, without a cover, into the preheated drying oven
analyses are normally complete when the sample reaches a (104 °C to 110 °C) through which passes a current of preheated
constant mass as defined in the instrumental operating param- drying gas (see 8.1). Close the oven and heat for 1 h. Remove
eters. (See 11.1.) the test specimen crucibles, cover immediately, allow to cool to
13.3 For LOI determinations using a single-step procedure, ambient temperature in a desiccator, and determine the mass.
add approximately 1 g of solid combustion residue to each (Additional heatings and mass determinations may be neces-
successive crucible and determine the mass. Select oxygen or sary for some solid combustion residues if the 1 h time period
air as the furnace atmosphere and gradually raise the tempera- is insufficient to bring the test specimen to a constant mass.)
ture of the furnace at a rate such that the furnace temperature For ash determination, place the crucible, without covers, with
reaches 500 °C 6 10 °C at the end of 1 h. For Method A, the dry test specimen in a cold furnace. Gradually raise the
continue the gradual heating until the temperature rises from temperature of the furnace at a rate such that it reaches 500 °C
500 °C 6 10 °C to 750 °C 6 15 °C at the end of 1 h. For 6 10 °C at the end of 1 h. For Method A, continue the gradual
Method B, continue the gradual heating until the temperature heating until the temperature rises from 500 °C 6 10 °C to
rises from 500 °C 6 10 °C to 950 °C 6 20 °C at the end of 1 h. 750 °C 6 15 °C at the end of 1 h. For Method B, continue the
Maintain the higher temperature until the combustion residue gradual heating until the temperature rises from 500 °C 6
test specimens reach a constant mass or for an additional 2 h. 10 °C to 950 °C 6 20 °C at the end of 1 h. Maintain the higher
temperature until the combustion residue test specimens reach
13.4 For LOI determinations using a two-step procedure,
a constant mass or for an additional 2 h.
add approximately 1 g of solid combustion residue to each
successive crucible and determine the mass. For moisture 13.7 If the solid combustion residue is heated to prepare an
determinations with the macro TGA, turn on the drying gas ash for the determination of the mass fractions of major and
(see 8.1) and heat the test specimens of known mass in minor elements, use the heating procedure described in Test
crucibles without covers at 104 °C to 110 °C. A recommended Methods D3682, D4326, and D6349, or the 750 °C procedure
flow rate is one furnace volume change per minute, but higher (Method A) described previously.
flow rates (that is, two furnace volumes per minute, as in other 13.8 If the solid combustion residue is heated to prepare an
standard test methods for coal and coke) are acceptable. Ash ash for the determination of the mass fractions of trace
determinations on the residues (dried test specimens) from the elements, use the heating procedure described in Test Methods
moisture determination are made by changing the macro TGA D3683 and D6357.
furnace atmosphere to oxidizing gas (see 8.1), and gradually
raising the temperature of the furnace at a rate such that the 14. Calculation of Results
furnace temperature reaches 500 °C 6 10 °C at the end of 1 h. 14.1 With a computer-controlled macro TGA, the computer
For Method A, continue the gradual heating until the tempera- is normally programmed to perform calculations automatically.
ture rises from 500 °C 6 10 °C to 750 °C 6 15 °C at the end The equations used in the calculations are as listed in the
of 1 h. For Method B, continue the gradual heating until the following sections.
temperature rises from 500 °C 6 10 °C to 950 °C 6 20 °C at
the end of 1 h. Maintain the higher temperature until the 14.2 Calculate the LOI expressed as a percentage from the
combustion residue test specimens reach a constant mass or for single-step procedure as follows:
an additional 2 h. LOI 5 @ ~ W 2 B ! /W # 3 100 (1)

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D7348 − 21
TABLE 1 Mass Fraction Range and Limits of Repeatability (r), Reproducibility (R), and Precision Ratio (PR) for LOI (750°C and 950°C)
Test Methods
Mass Fraction Repeatability Limit, Reproducibility Limit, Precision Ratio,
Range, r R (PR)
Percent
750 °C
Single-step
Procedure
Macro-TGA 1.1 to 11.7 0.16 0.23 1.43
Muffle Furnace 1.0 to 11.0 0.19 0.26 1.35
Two-Step
Procedure (dry
basis)
Macro-TGA 2.2 to 11.3 0.18 0.26 1.55
Muffle Furnace 0.9 to 11.4 0.26 0.45 1.82
950 °C
Single-step
Procedure
Macro-TGA 1.1 to 11.7 0.21 0.30 1.42
Muffle Furnace 2.6 to 11.8 0.39 0.58 1.62
Two-Step
Procedure
Macro-TGA 1.0 to 11.4 0.16 0.24 1.45
Muffle Furnace 2.4 to 11.4 0.27 0.50 1.84

Where: sample in the same laboratory by the same operator using the
W = mass of test specimen used, g, same apparatus on samples taken at random from a single
B = mass of test specimen after heating at 750 °C or quantity of homogeneous 250 µm (No. 60 USA Standard sieve)
950 °C, g, and material, may be expected to occur with a probability of
100 = conversion factor from dimensionless mass fraction approximately 95 %.
to percent, %. 16.1.2 Reproducibility Limit (R)—The value below which
14.3 Calculate the LOI expressed as a percentage from the the absolute difference between two test results, carried out in
two-step procedure as follows: different laboratories using samples taken at random from a
single quantity of 250 µm (No. 60 USA Standard sieve)
M 5 @ ~ W 2 C ! /W # 3 100 (2)
material that is as homogeneous as possible, may be expected
Ash 5 @ D/W # 3 100 (3) to occur with a probability of approximately 95 %.
LOI 5 @ ~ C 2 D ! /W # 3 100 (4) 16.1.3 The above terms (repeatability limit and reproduc-
ibility limit) are used as specified in Practice E177.
Where:
M =percent moisture as determined in the test specimen; 16.2 Scope Limits for a Test Method—Guide D8146 offers
W =mass of test specimen used, g; techniques for evaluating the statistical capability and fitness
C =mass of test specimen after drying in moisture test, g; for use in standard test methods. Guide D8146 defines the
D =mass of ash residue after heating at 750 °C or 950 °C, analytical performance value (APVr) as a metric that assesses
g; and the precision of a test method relative to applicable specifica-
LOI = percent loss on ignition as determined in the test tion limits. APVr is the ratio of the repeatability (r) of a test
specimen. method to specific limits, expressed as a percent. Guide D8146,
subsection 5.3.2, states that it is generally expected that the
15. Report analytical performance value, or APVr, should be less than
15.1 Report the temperature or method used, or both, to 28 % for a capable test method at its lowest limit. Since the
determine the LOI vales. For reporting analyses to other than repeatability, r, is equal to 2.8 x Sr, this is equivalent to saying
the as-determined basis, refer to Practice D3180. that the ratio of the within laboratory standard deviation (Sr) to
a sample test level, expressed as a percentage, should be less
16. Precision and Bias than 10 %.
16.1 Precision—The precision data of these test methods for 16.2.1 The lower scope limit of a test method is the larger of
the determination of LOI for combustion residues are shown in [lowest sample mean tested in the Interlaboratory Study (ILS)]
Table 1. The precision characterized by the repeatability (Sr, r) or [the test level where the ratio of the repeatability, r, of a test
and reproducibility (SR, R), analytical performance value sample to the test sample value is 28 %.]. The lower scope
(APVr), and precision ratio (PR) is described in Tables A1.1- limits for all of the LOI test samples reported in Tables
A1.4 in Annex A1. A1.1-A1.4 had APVr values less than 28 %.
16.1.1 Repeatability Limit (r)—The value below which the 16.2.2 Additionally, the upper scope limit of a test method is
absolute difference between two test results of separate and set to a value that does not exceed the parameter value of the
consecutive test determinations, carried out on the same test material with the highest value used in the ILS. The upper

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D7348 − 21
scope limits for the LOI test methods in Table 1 are the highest 16.5 An interlaboratory study, designed consistent with
sample means in the ILS. Practice E691, was conducted in 2006. Twenty labs partici-
16.3 Precision Ratio (PR) is the ratio between the reproduc- pated. The details of the study and supporting data are given in
ibility and repeatability (R/r) and can be used to determine Research Reports RR:D05-1031 and RR:D05-1036.5
whether a test method is sufficiently robust. Generally, a PR
value between 2 and 4 indicates the test method appears to 17. Keywords
adequately control between-laboratory common cause variabil- 17.1 ash; combustion residues; loss on ignition; LOI; macro
ity. A PR in the range of 1 to 2 implies that the contribution of thermogravimetric analysis; macro TGA
between-laboratory bias towards reproducibility is small or
insignificant relative to the within-lab repeatability. The PR
values for the LOI test methods determined in this study are 5
Supporting data have been filed at ASTM International Headquarters and may
listed in Table 1. be obtained by requesting Research Report RR:D05-1031. Contact ASTM Customer
Service at [email protected].
16.4 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. Contact ASTM Customer
the LOI is not currently available. Service at [email protected].

ANNEX

(Mandatory Information)

A1. PRECISION STATISTICS

A1.1 The precision of these test methods, characterized by determined for the following materials as listed in Tables
repeatability (Sr, r), reproducibility (SR, R), Analytical Perfor- A1.1-A1.4.
mance Value (APVr), and Precision Ratio (PR) has been

TABLE A1.1 Repeatability (Sr, r), Reproducibility (SR, R), Analytical Performance Value (APVr), and Precision Ratio (PR) Parameters
Used for Calculation of Precision Statement for Macro-TGA, One-Step Procedure for LOI (750 °C and 950 °C)
Material Average % LOI Sr SR r R APVr PR
750 °C
EBIT 11.6658 0.0622 0.0882 0.1742 0.2469 1.5 1.42
NDL 2.4303 0.0538 0.0684 0.1507 0.1915 6.3 1.27
BB 2.4911 0.0521 0.0620 0.1459 0.1736 5.9 1.19
CB 9.8186 0.0689 0.0865 0.1930 0.2421 2.0 1.25
TXL 4.0450 0.0616 0.1120 0.1725 0.3135 4.3 1.82
BDPS 1.0835 0.0273 0.0425 0.0763 0.1191 7.1 1.56
SHND 4.9025 0.0518 0.0589 0.1451 0.1649 3.0 1.14
7FA 4.4603 0.0425 0.0574 0.1191 0.1606 2.7 1.35
8FA 11.0510 0.0711 0.1217 0.1990 0.3406 1.8 1.71
950 °C
EBIT 11.6772 0.0962 0.1553 0.2695 0.4349 2.3 1.61
NDL 2.4200 0.0727 0.0787 0.2035 0.2204 8.4 1.08
BB 2.5603 0.0637 0.0981 0.1784 0.2747 7.0 1.54
CB 9.8631 0.0808 0.1249 0.2263 0.3497 2.3 1.55
TXL 4.0633 0.0585 0.0733 0.1637 0.2051 4.0 1.25
BDPS 1.0708 0.0283 0.0359 0.0793 0.1006 7.4 1.27
SHND 4.9075 0.0427 0.0534 0.1195 0.1495 2.4 1.25
7FA 4.4244 0.1114 0.1161 0.3119 0.3251 7.0 1.04
8FA 10.9314 0.0784 0.1531 0.2194 0.4286 2.0 1.95

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D7348 − 21
TABLE A1.2 Repeatability (Sr, r), Reproducibility (SR, R), Analytical Performance Value (APVr), and Precision Ratio (PR) 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 APVr PR
750 °C
EBIT 11.3225 0.0494 0.1057 0.1383 0.296 1.2 2.14
NDL 2.153 0.0532 0.0684 0.1488 0.1915 6.9 1.29
BB 2.3175 0.0529 0.054 0.1483 0.1512 6.4 1.02
CB 9.625 0.0392 0.0915 0.1097 0.2563 1.1 2.34
SHND 4.6285 0.0524 0.0661 0.1467 0.185 3.2 1.26
7FA 4.273 0.0561 0.058 0.157 0.1623 3.7 1.03
8FA 10.6325 0.0759 0.1105 0.2125 0.3094 2.0 1.46
NIST SRM 2696 2.2687 0.1154 0.1471 0.323 0.4119 14.2 1.28
950 °C
EBIT 11.3675 0.0698 0.1194 0.1955 0.3344 1.7 1.71
NDL 2.1708 0.0534 0.0849 0.1496 0.2376 6.9 1.59
BB 2.3905 0.0552 0.0644 0.1546 0.1803 6.5 1.17
CB 9.6633 0.0510 0.0900 0.1429 0.2519 1.5 1.76
TXL 3.9363 0.0687 0.0788 0.1923 0.2206 4.9 1.15
BDPS 0.9585 0.0306 0.0460 0.0858 0.1289 8.9 1.50
SHND 4.6653 0.0424 0.0559 0.1187 0.1566 2.5 1.32
7FA 4.2235 0.0446 0.0548 0.1247 0.1535 3.0 1.23
8FA 10.5600 0.0814 0.1265 0.2279 0.3543 2.2 1.55
NIST SRM 1880a 1.0488 0.0640 0.0917 0.1792 0.2568 17.1 1.43

TABLE A1.3 Repeatability (Sr, r), Reproducibility (SR, R), Analytical Performance Value (APVr), and Precision Ratio (PR) Parameters
Used for Calculation of Precision Statement for Muffle Furnace, One-Step Procedure for LOI (750 °C and 950 °C)
Material Average % LOI Sr SR r R APVr PR
750 °C
EBIT 11.64 0.0709 0.0924 0.1986 0.2587 1.7 1.30
BB 2.4925 0.0608 0.0612 0.1702 0.1714 6.8 1.01
CB 9.8129 0.0395 0.0588 0.1105 0.1647 1.1 1.49
TXL 3.5796 0.0713 0.1111 0.1998 0.3111 5.6 1.56
BDPS 1.0208 0.0571 0.0664 0.1598 0.186 15.7 1.16
SHND 4.6871 0.081 0.0986 0.2267 0.2762 4.8 1.22
8FA 10.9746 0.0843 0.1343 0.236 0.3759 2.2 1.59
950 °C
EBIT 11.7538 0.1046 0.2117 0.2928 0.5927 2.5 2.02
NDL 2.6146 0.0755 0.1321 0.2113 0.3699 8.1 1.75
CB 9.9296 0.1005 0.1794 0.2815 0.5022 2.8 1.78
TXL 3.6904 0.1170 0.3532 0.3276 0.9890 8.9 3.02
SHND 4.8404 0.2439 0.3727 0.6829 1.0434 14.1 1.53
7FA 4.4563 0.1318 0.1770 0.3692 0.4956 8.3 1.34

TABLE A1.4 Repeatability (Sr, r), Reproducibility (SR, R), Analytical Performance Value (APVr), and Precision Ratio (PR) 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 APVr PR
750 °C
EBIT 11.4039 0.1071 0.1762 0.2998 0.4933 2.7 1.65
NDL 2.0889 0.081 0.1854 0.2268 0.5191 5.2 2.29
BB 2.3739 0.0526 0.1055 0.1472 0.2954 4.0 2.01
CB 9.705 0.0757 0.1164 0.212 0.3259 2.4 1.54
TXL 3.5261 0.0788 0.1588 0.2206 0.4446 4.1 2.02
BDPS 0.9068 0.0554 0.1019 0.1551 0.2852 3.4 1.84
SHND 4.5211 0.1126 0.1701 0.3154 0.4764 2.3 1.51
7FA 4.2629 0.0965 0.1435 0.2703 0.4019 2.2 1.49
8FA 10.7336 0.1301 0.2452 0.3643 0.6865 3.6 1.88
950 °C
EBIT 11.4246 0.0916 0.2154 0.2566 0.6031 2.3 2.35
BB 2.4304 0.0707 0.1166 0.1980 0.3266 8.2 1.65
CB 9.7538 0.1187 0.1809 0.3323 0.5065 3.4 1.52
SHND 4.5763 0.1107 0.1850 0.3100 0.5180 6.8 1.67
7FA 4.2642 0.0941 0.1574 0.2634 0.4408 6.2 1.67
8FA 10.5542 0.0971 0.1975 0.2718 0.5531 2.6 2.04

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D7348 − 21
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