Designation: D3682 − 01 (Reapproved 2006)

Standard Test Method for

Major and Minor Elements in Combustion Residues from
Coal Utilization Processes1
This standard is issued under the fixed designation D3682; 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 Sample of Coal and Coke by Instrumental Procedures

1.1 This test method covers the analysis of the commonly (Withdrawn 2010)3
determined major and minor elements in combustion residues E691 Practice for Conducting an Interlaboratory Study to
from coal utilization processes. Determine the Precision of a Test Method
IEEE/ASTM SI 10 Standard for Use of the International
NOTE 1—Test Methods D1757 or D5016 shall be used for determina- System of Units (SI): The Modern Metric System
tion of sulfur.
1.2 The values stated in SI units ( IEEE/ASTM SI 10 ) shall 3. Summary of Test Method
to be regarded as the standard.
3.1 The combustion residue to be analyzed is ignited in air
1.3 This standard does not purport to address all of the at 750°C to a constant weight. The ash is fused within lithium
safety concerns, if any, associated with its use. It is the tetraborate (Li2B4O7) followed by a final dissolution of the
responsibility of the user of this standard to establish appro- melt in either dilute hydrochloric acid (HCl) or dilute nitric
priate safety and health practices and determine the applica- acid (HNO3). The solution is analyzed by atomic absorption/
bility of regulatory limitations prior to use. emission for applicable elements.
2. Referenced Documents
4. Significance and Use
2.1 ASTM Standards:2
D1193 Specification for Reagent Water 4.1 A compositional analysis of the ash in coal is often
D1757 Test Method for Sulfate Sulfur in Ash from Coal and useful in the total description of the quality of the coal.
Coke (Withdrawn 2009)3 Knowledge of ash composition is also useful in predicting the
D2013 Practice for Preparing Coal Samples for Analysis behavior of ashes and slags in combustion chambers. Utiliza-
D3173 Test Method for Moisture in the Analysis Sample of tion of the ash by-products of coal combustion sometimes
Coal and Coke depends on the chemical composition of the ash.
D3174 Test Method for Ash in the Analysis Sample of Coal 4.2 Note that the chemical composition of laboratory-
and Coke from Coal prepared coal ash may not exactly represent the composition of
D3180 Practice for Calculating Coal and Coke Analyses mineral matter in the coal or the composition of fly ash and slag
from As-Determined to Different Bases resulting from commercial-scale burning of the coal.
D5016 Test Method for Total Sulfur in Coal and Coke
Combustion Residues Using a High-Temperature Tube 5. Apparatus
Furnace Combustion Method with Infrared Absorption
D5142 Test Methods for Proximate Analysis of the Analysis 5.1 Ashing Furnace, with an adequate air circulation and
capable of having its temperature regulated between 700 and
750°C.
1
This test method is under the jurisdiction of ASTM Committee D05 on Coal 5.2 Fusion Furnace, with an operating temperature of
and Coke and is the direct responsibility of Subcommittee D05.29 on Major
Elements in Ash and Trace Elements of Coal.
1000°C.
Current edition approved April 1, 2006. Published April 2006. Originally 5.3 Platinum Dish, 35- to 85-mL capacity.
approved in 1978. Last previous edition approved in 2001 as D3682 – 01´1. DOI:
10.1520/D3682-01R06. 5.4 Stirring Hotplate and Bars, operating temperature of
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
200°C.
Standards volume information, refer to the standard’s Document Summary page on
5.5 Atomic Absorption Spectrometer—Any dual-channel in-
the ASTM website.
3
The last approved version of this historical standard is referenced on strument using a deuterium (D2) arc background corrector or
www.astm.org. other comparable simultaneous background correction system.

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

Copyright by ASTM Int'l (all rights reserved); 1

 D3682 − 01 (2006)
6. Reagents weighted out at the same time as the analysis sample and make
6.1 Purity of Reagents—Reagent grade chemicals shall be the necessary corrections. Thoroughly mix each sample before
used in all tests. It is intended that all reagents shall conform to weighing.
the specifications of the Committee on Analytical Reagents of 7.2 If the ash is to be prepared from a coal, prepare the coal
the American Chemical Society, where such specifications are analysis sample in accordance with Practice D2013 by pulver-
available.4 Other grades may be used, provided it is first izing the materials to pass a 250-µm (No. 60) sieve.
ascertained that the reagent is of sufficiently high purity to 7.2.1 Analyze separate test portions of the coal for moisture
permit its use without lessening the accuracy of the determi- and ash contents in accordance with Test Methods D3173,
nation. The lithium tetraborate and lanthanum chloride re- D3174, or D5142 so that calculations to other bases can be
agents in particular should be examined for alkali and alkaline made.
earth contamination.
7.2.2 Prepare the ash from a thoroughly mixed analysis
6.2 Purity of Water—Unless otherwise indicated, references sample of coal. Spread the coal in a layer not over 6 mm (1⁄4
to water shall be understood to mean Type II reagent water as in.) in depth in a fireclay or porcelain roasting dish. Place the
defined in Specification D1193. dish in a cold muffle furnace and heat gradually so that the
6.3 Aluminum Stock Solution (1000-ppm aluminum). temperature reaches 500°C in 1 h and 750°C in 2 h. Ignite at
750°C until all carbonaceous matter is removed. Proceed with
6.4 Calcium Stock Solution (1000-ppm calcium). the preparation of the ash in accordance with 7.1. If samples
6.5 Iron Stock Solution (1000-ppm iron). are stored and the absorption of moisture or CO2, or both, is in
6.6 Lanthanum Chloride Solution (175-g/L lanthanum chlo- question, reignite the ash using the 500-750°C staged combus-
ride (LaCl3) or equivalent 10 % lanthanum). tion before use. Alternatively, determine loss on ignition using
the 500-750°C staged combustion on a separate sample
6.7 Lithium Tetraborate—(Li2B4O7), powder. weighed out at the same time as the test portion and make the
6.8 Magnesium Stock Solution (1000-ppm magnesium). necessary corrections. Thoroughly mix each sample before
6.9 Potassium Stock Solution (1000-ppm potassium). weighing.
6.10 Silicon Stock Solution (200-ppm silicon) (Note 2). 8. Procedure
6.11 Sodium Stock Solution (1000-ppm sodium).
8.1 The solutions and proportions described below are for
6.12 Solvent Acid—Dilute 50 mL of concentrated hydro- typical ash samples as represented by American coals of
chloric acid (sp gr 1.19) or 50 mL of concentrated nitric acid bituminous rank. Therefore, stronger or weaker dilutions may
(sp gr 1.42) to 1000 mL. Either acid solution may be used, but be required to establish suitable concentrations for those
whichever is chosen should be used throughout the subsequent elements of varying percents outside the range of the typical
solution preparations. sample. Each analyst must determine the sensitivity and linear
6.13 Titanium Stock Solution (1000-ppm titanium). range of calibration of their equipment and choose concentra-
tion ranges for standards compatible with the samples and
NOTE 2—Commercial silicon standards prepared from sodium silicate
have not proved satisfactory. A standard stock solution can be prepared by
instrument specific to their own work.
fusing 0.1070 g of reignited spectrographic grade silica (SiO2) with 1 g of 8.1.1 Calculations used in subsequent sections are devel-
lithium tetraborate, dissolving in solvent acid, and diluting to 250 mL as oped from the following general formula for percent concen-
described for sample preparation in 8.3.1 and 8.3.2. This solution is tration of element oxide, E, in moisture-free coal ash:
200-ppm silicon. Preferable standard preparations for silica are made by
fusion and dilution of ash sample(s) of known composition in accordance E 5 @ ~ C 2 B ! / ~ A 2 B ! # 3 ~ N/M ! 3 F 3 100 (1)
with 8.3.1 and 8.3.2. The standard sample(s) should have a composition(s)
similar to the unknown. where:
A = absorbance of standard;
7. Sample Preparation B = absorbance of blank;
7.1 The combustion residue to be analyzed must first be C = absorbance of sample solution;
N = element in standard, ppm;
ignited in air at 750°C to a constant weight before analysis.
M = sample of solution, ppm; and
Allow the ash to cool, transfer to an agate mortar, and grind to F = conversion from element to oxide.
pass a 74-µm (No. 200) sieve. Reignite the ash at 750°C for 1
NOTE 3—Concentrations in the ash may be converted to the air-dried
h, cool rapidly, and immediately weigh portions for analysis. If coal basis using the following expression:
samples are stored, reignite the ash before weighing or deter-
mine the loss on ignition at 750°C on a separate sample C 5 ~ AB/100!

where:
4
Reagent Chemicals, American Chemical Society Specifications, American C = oxide in air-dried coal, %;
Chemical Society, Washington, DC. For suggestions on the testing of reagents not A = oxide in ash, %; and
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
B = ash as determined in Test Method D3174 or Test
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, Method D5142, %.
MD. See Practice D3180 for procedures to convert values to other bases.

Copyright by ASTM Int'l (all rights reserved); 2

 D3682 − 01 (2006)
8.2 To minimize the potential of contamination, the plati- solution (see 6.10) with 1 mL of the aluminum stock solution
numware must be prepared by boiling in solvent acid and (see 6.3) and diluting to 100 mL with the blank solution (see
rinsing thoroughly with reagent-grade water. After this initial 9.2). Only those standards need be prepared that bracket the
cleaning, the platinumware must be handled with clean tongs expected SiO2 concentrations in the samples.
and protected from further contamination from table tops, and Silicon, Stock
so forth. All glassware used in analyses must be equally clean Solution (6.12), mL Silicon, ppm Equivalent SiO2, %
and equally protected. 25 50 53.5
8.3 Sample Fusion and Solution: 20 40 42.8
15 30 32.1
8.3.1 Weigh 0.1 6 0.0002 g of the sample as prepared in 10 20 21.4
7.2.2 into a platinum dish (5.3) (Note 4) and add 0.5 g of
9.2 Blank Solution—Prepare a solution of 2 g/L of Li2B4O7
Li2B4O7. Mix the ash and lithium tetraborate well, then add an
solution in solvent acid.
additional 0.5 g of Li2B4O7 to cover the mixture. Place the dish
in a clean silica or refractory tray and place in a muffle furnace 9.3 Sample Solution—Use the 200-ppm sample solution as
preheated to 1000°C; 15 min at 1000°C is sufficient to fuse the prepared in 8.3.3.
mixture completely. Remove the tray and dish and cool to 9.4 Atomic Absorption Operating Conditions—Use a silicon
room temperature. Carefully rinse the bottom and outside of hollow-cathode lamp and set the monochromator at 251.6 nm.
the platinum dish to remove possible contamination, then place Use a nitrous oxide/acetylene flame. Adjust other instrument
it in a clean 250- or 400-mL beaker. Place a clean TFE- parameters to optimum for the particular equipment used.
fluorocarbon-coated stirring magnet inside the dish, add 150
9.5 Determination—Read out absorbance values for the
mL of solvent acid to the beaker and dish, and place immedi-
blank solution, standard solutions, and sample solution. In this
ately on the stirring hotplate. Heat the solution to just below
and all subsequent determinations, those instruments so
boiling temperature and maintain for not more than 30 min
equipped may be calibrated to read out “percent concentration”
with constant stirring. This time and temperature are sufficient
directly. Determine percent SiO2 as follows:
to completely dissolve the melt. If stirring is not maintained
constantly, some of the ash constituents are apt to precipitate SiO2 , % 5 @ ~ C 2 B ! / ~ A 2 B ! # 3 N 3 1.07 (2)
and the analysis must be repeated. where:
NOTE 4—The use of graphite crucibles and subsequent dissolution of A = absorbance of standard nearest C,
fused beads from them was not investigated; however, their successful use B = absorbance of blank,
in similar methods has been reported.5 C = absorbance of sample, and
8.3.2 Remove the beaker from the hotplate and permit to N = silicon in standard, ppm.
cool to room temperature. Quantitatively transfer the solution
to a 200-mL volumetric flask, wash the platinum dish and 10. Aluminum Oxide (Al2O3)
beaker with small amounts of solvent acid and dilute to the 10.1 Preparation of Standards—Prepare standard solutions
200-mL mark with the solvent acid. This solution is 500 ppm containing from 10- to 30-ppm aluminum and dilute with blank
with respect to the total sample and contains 5 g/L of Li2B4O7 solution 9.2.
solution. 10.2 Blank Solution—Use the blank as prepared in 9.2.
8.3.3 Solution 1—Pipet 20 mL of the sample solution
prepared in 8.3.2 into a 50-mL volumetric flask and dilute to 10.3 Sample Solution—Use Solution 1 as prepared in 8.3.3.
volume with solvent acid. This solution is 200 ppm with 10.4 Atomic Absorption Operating Conditions—Use an alu-
respect to the total sample and contains 2 g/L of Li2B4O7 minum hollow-cathode lamp and set the monochromator at
solution. 309.2 nm. Use a nitrous oxide-acetylene flame. Adjust other
8.3.4 Solution 2—Pipet 10 mL of the sample solution instrument parameters to optimum for the particular equipment
prepared in 8.3.2 into a 100-mL volumetric flask, add 10 mL of used.
lanthanum solution (see 6.6), and dilute to volume with solvent 10.5 Determination—Read out absorbance values for the
acid. This solution is 50 ppm with respect to the total sample blank solution, standard solutions, and sample solution. Deter-
and contains 0.5 g/L of Li2B4O7 solution. mine percent Al2O3 as follows:
NOTE 5—Lanthanum was included in the solution as a release agent in Al2 O 3 , % 5 @ ~ C 2 B ! / ~ A 2 B ! # 3 N 3 0.94 (3)
those determinations that may require it (for example, calcium). Alterna-
tive measures, such as the use of nitrous oxide flame, are permissible. where:
A = absorbance of standard nearest C,
9. Silicon Dioxide (SiO2)
B = absorbance of blank,
9.1 Preparation of Standards—Prepare a series of standards C = absorbance of sample, and
by combining the following volumes of the silicon stock N = aluminum in standard, ppm.
11. Iron Oxide (Fe2O3)
5
Muter, R. B. and Nice, L. L., “Major and Minor Constituents in Siliceous
Materials by Atomic Absorption Spectroscopy,” Advances in Chemistry Series 141,
11.1 Preparation of Standards—Prepare standard solutions
Trace Elements in Fuels, American Chemical Society, Washington, DC, 1975, pp. containing from 2- to 10-ppm iron and 10 mL of lanthanum
57–65. solution per 100 mL. Dilute with blank solution (11.2).

Copyright by ASTM Int'l (all rights reserved); 3

 D3682 − 01 (2006)
11.2 Blank Solution—Prepare a solution of solvent acid 13.5 Determination—Read the absorbance values for the
containing 0.5-g/L Li2B4O7. blank solution, the standard solutions, and the sample solution.
11.3 Sample Solution—Use Solution 2 as prepared in 8.3.4. Determine percent MgO as follows:
MgO, % 5 @ ~ C 2 B ! / ~ A 2 B ! # 3 N 3 3.32 (6)
11.4 Atomic Absorption Operating Conditions—Use an iron
hollow-cathode lamp and set the monochromator at 248.3 nm. where:
Use an air-acetylene flame of stoichiometric composition. A = absorbance of standard nearest C,
Adjust other instrument parameters to optimum for the particu- B = absorbance of blank,
lar equipment used. C = absorbance of sample, and
11.5 Determination—Read the absorbance values for the N = magnesium in standard, ppm.
blank solution, the standard solutions, and the sample solution.
Determine percent Fe2O3 as follows: 14. Sodium Oxide (Na2O)
Fe2 O 3 , % 5 @ ~ C 2 B ! / ~ A 2 B ! # 3 N 3 2.86 (4) 14.1 Preparation of Standards—Prepare standard solutions
containing 0.5- to 2-ppm sodium and 10 mL of lanthanum6
where: solution per 100 mL. Dilute with blank solution as described in
A = absorbance of standard nearest C, 11.2.
B = absorbance of blank,
C = absorbance of sample, and 14.2 Blank Solution—Use blank solution as described in
N = iron in standard, ppm. 11.2.
14.3 Sample Solution—Use Solution 2 as described in 8.3.4.
12. Calcium Oxide (CaO)
14.4 Atomic Absorption Operating Conditions—Use a so-
12.1 Preparation of Standards—Prepare standard solutions dium hollow-cathode lamp and set the monochromator at 589.0
containing 1- to 10-ppm calcium and 10 mL of lanthanum nm. Use an air-acetylene flame. Adjust other instrument
solution per 100 mL. Dilute with the blank solution as parameters to optimum for the particular equipment used.
described in 11.2.
14.5 Determination—Read the absorbance values for the
12.2 Blank Solution—Use blank solution as described in blank solution, the standard solutions, and the sample solution.
11.2. Determine percent Na2O as follows:
12.3 Sample Solution—Use Solution 2 as described in 8.3.4. Na2 O, % 5 @ ~ C 2 B ! / ~ A 2 B ! # 3 N 3 2.70 (7)
12.4 Atomic Absorption Operating Conditions—Use a cal- where:
cium hallow-cathode lamp and set the monochromator at 422.7
A = absorbance of standard nearest C,
nm. Use an air-acetylene flame. Adjust other instrument B = absorbance of blank,
parameters to optimum for the particular equipment used. C = absorbance of sample, and
12.5 Determination—Read the absorbance values for the N = sodium in standard, ppm.
blank solution, the standard solutions, and the sample solution. NOTE 6—Alternatively, sodium may be determined by flame emission.
Determine percent CaO as follows:
15. Potassium Oxide (K2O)
CaO, % 5 @ ~ C 2 B ! / ~ A 2 B ! # 3 N 3 2.80 (5)
15.1 Standard Preparation—Prepare standard solutions
where: containing 0.5- to 2-ppm potassium and 10 mL of lanthanum6
A = absorbance of standard nearest C, solution per 100 mL. Dilute with blank solution as described in
B = absorbance of blank, 11.2.
C = absorbance of sample, and
N = calcium in standard, ppm. 15.2 Blank Solution—Use blank solution as described in
11.2.
13. Magnesium Oxide (MgO) 15.3 Sample Solution—Use Solution 2 as described in 8.3.4.
13.1 Preparation of Standards—Prepare standard solutions 15.4 Atomic Absorption Operating Conditions—Use a po-
containing 0.5- to 2-ppm magnesium and 10 mL of lanthanum tassium hollow-cathode lamp and set the monochromator at
solution per 100 mL. Dilute with blank solution as described in 766.5 nm. Use an air-acetylene flame. Adjust other instrument
11.2. parameters to optimum for the particular equipment used.
13.2 Blank Solution—Use blank solution as described in 15.5 Determination—Read the absorbance values for the
11.2. blank solution, the standard solution, and the sample solution.
13.3 Sample Solution—Use Solution 2 as described in 8.3.4. Determine percent K2O as follows:
13.4 Atomic Absorption Operating Conditions—Use a mag- K 2 O, % 5 @ ~ C 2 B ! / ~ A 2 B ! # 3 N 3 2.41 (8)
nesium hollow-cathode lamp and set the monochromator at
285.1 nm. Use an air-acetylene flame of stoichiometric com-
position. Adjust other instrument parameters to optimum for 6
Supporting data have been filed at ASTM International Headquarters and may
the particular equipment used. be obtained by requesting Research Report RR:RR:D05-1000..

Copyright by ASTM Int'l (all rights reserved); 4

 D3682 − 01 (2006)
where: TABLE 1 Concentrations Ranges and Limits for Repeatability and
Reproducibility for Major and Minor Elemental Oxides in Ash
A = absorbance of standard nearest C, from Combustion Residues
B = absorbance of blank,
Elemental Concentration Repeatability Limit Reproducibility Limit
C = absorbance of sample, and Oxide Range, % r R
N = potassium in standard, ppm. SiO2 33.14 – 57.73 0.33 + 0.04 x̄A –1.21 + 0.14 x̄
NOTE 7—Alternatively, potassium may be determined by flame emis- Al2O3 11.32 – 31.83 0.80 –0.24 + 0.09 x̄
sion. Fe2O3 2.93 – 41.11 0.01 + 0.06 x̄ 0.36 + 0.06 x̄
NOTE 8—It may be found convenient to combine the standards for iron, MgO 0.45 – 7.12 0.04 + 0.03 x̄ 0.04 + 0.09 x̄
calcium, magnesium, sodium, and potassium in one solution. CaO 1.46 – 22.19 0.21 + 0.04 x̄ 0.15 + 0.11 x̄
TiO2 0.57 – 1.44 0.13 0.19
K2O 0.45 – 2.99 0.03 + 0.03 x̄ 0.05 + 0.05 x̄
16. Titanium Dioxide (TiO2) Na2O 0.14 – 7.15 0.06 + 0.03 x̄ 0.04 + 0.18 x̄
16.1 Standard Preparation—Prepare a standard solution A
Where x̄ is the average of two single test results.
containing 3-ppm titanium and 5 g/L of Li2B4O7 solution
dissolved in solvent acid. If required, successive dilutions may
be made with the blank solution (see 16.2). TABLE 2 Comparison of Certified Values for Standard Reference
Material 1633b with Interlaboratory Study Values for Major and
16.2 Blank Solution—Prepare a solution containing 5 g/L of Minor Elemental Oxides in Ash from Combustion Residues
Li2B4O7 solution dissolved in solvent acid. Elemental Significant (95 %
AA-RR Value NIST Value Bias, %
Oxide Confidence Level)
16.3 Sample Solution—Use the original sample solution as
SiO2 49.57 ± 0.96 49.25 ± 0.17 0.65 no
prepared in 8.3.2. Al2O3 28.16 ± 0.31 28.44 ± 0.51 –0.98 no
Fe2O3 10.96 ± 0.25 11.12 ± 0.33 –1.44 no
16.4 Atomic Absorption Operating Conditions—Use a tita- MgO 0.79 ± 0.02 0.80 ± 0.01 -1.25 no
nium hollow-cathode lamp and set the monochromator at 364.3 CaO 2.01 ± 0.12 2.11 ± 0.08 –4.74 no
nm. Use a nitrous oxide-acetylene flame. Adjust other instru- TiO2 1.30 ± 0.04 1.32 ± 0.02 –1.52 no
K2O 2.25 ± 0.04 2.35 ± 0.04 –4.25 yes
ment parameters to optimum for the particular equipment used. Na2O 0.26 ± 0.02 0.27 ± 0.004 –3.70 no
16.5 Determination—Read the absorbance for the blank
solution, the standard solution and the sample solution. Deter-
mine percent TiO2 as follows: quantity of homogeneous material, may be expected to occur
with a probability of approximately 95 %.
TiO2 , % 5 @ ~ C 2 B ! / ~ A 2 B ! # 3 1.00 (9)
18.1.2 Reproducibility Limit (R)—The value below which
where: the absolute difference between two test results, carried out in
A = absorbance of standard, different laboratories using samples taken at random from a
B = absorbance of blank, and single quantity of material that is as nearly homogeneous as
C = absorbance of sample. possible, may be expected to occur with a probability of
approximately 95 %.
17. Report
18.2 Bias—The NIST Standard Reference Material 1633b
17.1 Report the percentages for the elemental oxides in the was included in the interlaboratory study to ascertain possible
ash as specified in 9.5, 10.5, 11.5, 12.5, 13.5, 14.5, 15.5, and bias between reference material values and those determined
16.5. by this test method. A comparison of the NIST values and those
17.2 Report the method used for concurrent moisture and obtained in the interlaboratory study are given in Table 2.
ash determination, if applicable. 18.3 An interlaboratory study, designed in accordance with
17.3 Use Practice D3180 for procedures to convert values to Practice E691, was conducted in 1999. Six laboratories par-
other bases. ticipated.7

18. Precision and Bias 19. Keywords

18.1 Precision—The precision of this test method is in 19.1 aluminum oxide (A12O3); ash analysis; atomic absorp-
accordance with Table 1. The precision characterized by the tion spectroscopy; calcium oxide (CaO); elemental ash com-
repeatability (Sr, r) and reproducibility (SR, R) is in accordance position; ferric oxide (Fe2O3); magnesium oxide (MgO); po-
with Table A1.1. tassium oxide (K2O); silicon dioxide (SiO2); sodium oxide
18.1.1 Repeatability Limit (r)—The value below which the (Na2O); titanium dioxide (TiO2)
absolute difference between two test results of separate and
consecutive test determinations, carried out on the same
sample in the same laboratory by the same operator using the 7
Supporting data have been filed at ASTM International Headquarters and may
same apparatus on samples taken at random from a single be obtained by requesting Research Report RR:RR:D05-1000.

Copyright by ASTM Int'l (all rights reserved); 5

 D3682 − 01 (2006)
ANNEX

(Mandatory Information)

A1. PRECISION STATISTICS

A1.1 The precision of this test method, characterized by A1.3 Reproducibility Standard Deviation (SR)—The stan-
repeatability (Sr, r) and reproducibility (SR, R) has been dard deviation of test results obtained under reproducibility
determined for the following materials as listed in Table A1.1. conditions.
A1.2 Repeatability Standard Deviation (Sr)—The standard
deviation of test results obtained under repeatability condi-
tions.

TABLE A1.1 Repeatability (Sr, r) and Reproducibility (SR, R) Parameters Used for Calculation of Precision Statement
SiO2 CaO
Materials Average Sr SR r R Materials Average Sr SR r R
CAN 33.1437 0.6687 1.3581 1.8725 3.8026 CAN 4.4988 0.1446 0.169 0.4049 0.4732
FPA 57.7325 0.8709 2.7464 2.4386 7.69 FPA 1.4646 0.103 0.1536 0.2883 0.4301
IL 48.7917 0.604 2.1085 1.6912 5.9037 IL 4.4004 0.1224 0.1993 0.3427 0.5581
JO 40.1846 0.5457 1.1898 1.5279 3.3316 JO 7.4804 0.1686 0.3083 0.472 0.8633
WDK 34.6421 0.5795 0.9385 1.6227 2.6279 WDK 17.5079 0.5356 0.7637 1.4998 2.1384
95-1 29.8767 0.4486 1.4572 1.256 4.0801 95-1 22.1937 0.3805 0.8789 1.0653 2.4609
95-6 29.7379 0.5258 1.2832 1.4724 3.593 95-6 19.6621 0.307 0.7844 0.8597 2.1962
NIST 1633B 49.5717 0.9622 1.856 2.6941 5.1969 NIST 1633B 2.0154 0.1196 0.1579 0.335 0.4422
Al2O3 TiO2
Materials Average Sr SR r R Materials Average Sr SR r R
CAN 11.3254 0.185 0.3371 0.518 0.9438 CAN 0.574 58 0.054 28 0.091 09 0.151 97 0.255 06
FPA 29.0638 0.2896 1.1124 0.8109 3.1146 FPA 1.439 58 0.051 76 0.089 63 0.144 93 0.250 95
IL 19.2546 0.3629 0.597 1.0162 1.6715 IL 0.925 00 0.036 55 0.054 40 0.102 35 0.152 33
JO 31.8275 0.2288 0.8521 0.6406 2.386 JO 1.172 5 0.042 26 0.042 26 0.118 33 0.118 33
WDK 15.825 0.2908 0.4738 0.8142 1.3267 WDK 0.913 33 0.029 63 0.032 79 0.082 96 0.091 8
95-1 18.9821 0.2141 0.5738 0.5994 1.6066 95-1 1.140 83 0.038 73 0.069 46 0.108 44 0.194 48
95-6 19.7283 0.3554 0.3554 0.9951 0.9951 95-6 1.303 75 0.051 87 0.065 0.145 23 0.181 99
NIST 1633b 28.1637 0.3148 0.794 0.8815 2.2231 NIST 1633b 1.279 17 0.048 13 0.085 68 0.134 77 0.239 91
K2O Na2O
Materials Average Sr SR r R Materials Average Sr SR r R
CAN 1.367 92 0.026 33 0.054 73 0.073 71 0.153 26 CAN 0.140 83 0.028 63 0.031 08 0.080 15 0.087 04
FPA 2.991 67 0.050 94 0.080 55 0.142 62 0.225 53 FPA 0.254 58 0.016 71 0.035 18 0.046 78 0.098 52
IL 2.175 0.029 3 0.030 19 0.082 03 0.084 52 IL 1.366 25 0.028 16 0.075 69 0.078 85 0.211 94
JO 0.523 75 0.017 52 0.029 19 0.049 06 0.081 73 JO 0.251 67 0.024 49 0.033 86 0.068 59 0.094 81
WDK 0.54 0.019 44 0.026 14 0.054 42 0.073 19 WDK 1.067 08 0.026 54 0.059 91 0.074 3 0.167 75
95-1 0.451 67 0.022 67 0.027 74 0.063 47 0.077 68 95-1 3.488 33 0.109 19 0.278 28 0.305 73 0.779 18
95-6 0.648 75 0.017 52 0.032 97 0.049 06 0.092 32 95-6 7.149 58 0.086 87 0.459 96 0.243 23 1.287 89
NIST 1633b 2.251 25 0.044 33 0.071 96 0.124 13 0.201 49 NIST 1633b 0.258 75 0.024 41 0.034 7 0.068 35 0.097 15
Fe2O3 MgO
Materials Average Sr SR r R Materials Average Sr SR r R
CAN 41.1154 0.8321 1.0852 2.3299 3.0385 CAN 0.448 33 0.019 79 0.037 79 0.055 41 0.105 81
FPA 2.9279 0.0505 0.1685 0.1414 0.4719 FPA 1.049 17 0.011 9 0.050 77 0.033 33 0.142 16
IL 15.86 0.2502 0.4939 0.7005 1.383 IL 0.951 25 0.036 8 0.065 73 0.103 04 0.184 03
JO 4.6396 0.1449 0.2774 0.4058 0.7768 JO 1.315 83 0.034 8 0.065 25 0.097 44 0.182 7
WDK 6.5746 0.1445 0.3407 0.4045 0.9539 WDK 4.313 75 0.060 79 0.175 91 0.170 22 0.492 54
95-1 6.535 0.1482 0.1995 0.415 0.5587 95-1 7.122 5 0.084 93 0.224 3 0.237 82 0.628 04
95-6 5.3317 0.0833 0.2662 0.2332 0.7454 95-6 6.197 08 0.114 17 0.272 78 0.319 68 0.763 79
NIST 1633b 10.9625 0.2547 0.3576 0.7131 1.0012 NIST 1633b 0.787 08 0.024 12 0.052 03 0.067 55 0.145 69

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of 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 and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make 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 standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or [email protected] (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/
COPYRIGHT/).

Copyright by ASTM Int'l (all rights reserved); 6