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: D3682 − 21

Standard Test Method for

Major and Minor Elements in Combustion Residues from
Coal Utilization Processes by Atomic Spectrometry1
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 D3180 Practice for Calculating Coal and Coke Analyses

1.1 This test method covers the analysis of the commonly
determined major and minor elements in combustion residues
from coal utilization processes.
1.2 Use Test Method D5016 for determination of sulfur.
1.3 Units—The values stated in SI units are to be regarded
as standard. The values given in parentheses are provided for
information only and are not considered standard.
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
1.5 This international standard was developed in accor-
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:2
D121 Terminology of Coal and Coke
D346 Practice for Collection and Preparation of Coke
Samples for Laboratory Analysis
D1193 Specification for Reagent Water
D2013 Practice for Preparing Coal Samples for Analysis
D3173 Test Method for Moisture in the Analysis Sample of
Coal and Coke
D3174 Test Method for Ash in the Analysis Sample of Coal
and Coke from Coal
1
This test method is under the jurisdiction of ASTM Committee D05 on Coal
and Coke and is the direct responsibility of Subcommittee D05.29 on Major
Elements in Ash and Trace Elements of Coal.
Current edition approved Dec. 1, 2021. Published January 2022. Originally
approved in 1978. Last previous edition approved in 2013 as D3682 – 13. DOI:
10.1520/D3682-21.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
from As-Determined to Different Bases
D5016 Test Method for Total Sulfur in Coal and Coke
Combustion Residues Using a High-Temperature Tube
Furnace Combustion Method with Infrared Absorption
D7348 Test Methods for Loss on Ignition (LOI) of Solid
Combustion Residues
D7582 Test Methods for Proximate Analysis of Coal and
Coke by Macro Thermogravimetric Analysis
E691 Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method
3. Terminology
3.1 For definitions of terms used in this test method, refer to
Terminology D121.
4. Summary of Test Method
4.1 The combustion residue to be analyzed is ignited in air
at 750 °C to a constant mass. The ash is fused within lithium
tetraborate (Li2B4O7) followed by a final dissolution of the
melt in either dilute hydrochloric acid (HCl) or dilute nitric
acid (HNO3). The solution is analyzed by atomic absorption for
applicable elements.
5. Significance and Use
5.1 A compositional analysis of the ash in coal is often
useful in the total description of the quality of the coal.
Knowledge of ash composition is also useful in predicting the
behavior of ashes and slags in combustion chambers. Utiliza-
tion of the ash by-products of coal combustion sometimes
depends on the chemical composition of the ash.
5.2 Note that the chemical composition of laboratory-
prepared coal ash may not exactly represent the composition of
mineral matter in the coal or the composition of fly ash and slag
resulting from commercial-scale burning of the coal.
6. Apparatus
6.1 Ashing Furnace, with an adequate air circulation and
capable of having its temperature regulated at 500 °C and
750 °C.
6.2 Fusion Furnace, with an operating temperature of
1000 °C.

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 D3682 − 21
6.3 Platinum Vessels (Dish or Crucible), 35 mL to 85 mL
capacity. Graphite crucibles with 10 mL to 15 mL capacity may
also be used (Note 1).
NOTE 1—The use of graphite crucibles and subsequent dissolution of
fused beads from them was not investigated; however, their successful use
in similar methods has been reported.3
6.4 Stirring Hotplate and Bars, operating temperature of
200 °C.
6.5 Flame Atomic Absorption Spectrophotometer—Any
dual-channel instrument using a deuterium (D2) arc back-
ground corrector or other comparable simultaneous back-
ground correction system equipped with air/acetylene and
nitrous oxide/acetylene burner heads.
6.6 Hollow Cathode or Electrodeless Discharge Lamp, for
each element to be defined.
6.7 Deuterium Continuum Lamp.
6.8 Compressed Air—Appropriate pressure reducing regu-
lator with base connections (see instrument manufacturer’s
instructions).
6.9 Acetylene Gas and Regulator—A cylinder of acetylene
equipped with a two-gauge, two-stage pressure-reducing regu-
lator (see instrument manufacturer’s instructions).
6.10 Nitrous Oxide Gas and Regulator—A cylinder of
nitrous oxide equipped with a two-gauge, two-stage pressure-
reducing regulator (see instrument manufacturer’s instruc-
tions).
7. Reagents
7.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. It is intended that all reagents shall conform to
the specifications of the Committee on Analytical Reagents of
the American Chemical Society, where such specifications are
available.4 Other grades may be used, provided it is first
ascertained that the reagent is of sufficiently high purity to
permit its use without lessening the accuracy of the determi-
nation. The lithium tetraborate and lanthanum chloride re-
agents in particular should be examined for alkali and alkaline
earth contamination.
7.2 Purity of Water—Unless otherwise indicated, references
to water shall be understood to mean Type II reagent water as
defined in Specification D1193.
7.3 Aluminum Stock Solution (1000 µg ⁄mL aluminum).
7.4 Calcium Stock Solution (1000 µg ⁄mL calcium).
7.5 Iron Stock Solution (1000 µg ⁄mL iron).
3
Muter, R. B., and Nice, L. L., “Major and Minor Constituents in Siliceous
Materials by Atomic Absorption Spectroscopy,” Advances in Chemistry Series 141,
Trace Elements in Fuels, American Chemical Society, Washington, DC, 1975, pp.
57–65.
4
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
MD.
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7.6 Lanthanum Chloride Solution (175 g ⁄L lanthanum chlo-
ride (LaCl3) or equivalent 10 % mass concentration lantha-
num).
7.7 Fluxing Agent - Lithium Tetraborate—(Li2B4O7), or
mixtures of lithium tetraborate (Li2B4O7) and anhydrous
lithium metaborate (LiBO2).
7.8 Magnesium Stock Solution (1000 µg ⁄mL magnesium).
7.9 Potassium Stock Solution (1000 µg ⁄mL potassium).
7.10 Silicon Stock Solution (200 µg ⁄mL silicon) (Note 2).
NOTE 2—A standard stock solution can be prepared by fusing 0.1070 g
of reignited spectrographic grade silica (SiO2) with 1 g of lithium
tetraborate, dissolving in solvent acid, and diluting to 250 mL as described
for sample preparation in 9.3.1 and 9.3.2. This solution is 200 µg ⁄mL
silicon. Preferable standard preparations for silica are made by fusion and
dilution of ash sample(s) of known composition in accordance with 9.3.1
and 9.3.2. The standard sample(s) should have a composition(s) similar to
the unknown.
7.11 Sodium Stock Solution (1000 µg ⁄mL sodium).
7.12 Titanium Stock Solution (1000 µg ⁄mL titanium).
7.13 Solvent Acid
7.13.1 Hydrochloric Acid (HCl)—Concentrated hydrochlo-
ric acid, 12 N, specific gravity (sp) 1.19.
7.13.2 Nitric Acid (HNO3)—Concentrated nitric acid, 16 N,
sp 1.42.
7.13.3 Dilute 50 mL of concentrated hydrochloric acid (sp
gr 1.19) or 50 mL of concentrated nitric acid (sp gr 1.42) to
1000 mL. Either acid solution may be used, but whichever is
chosen should be used throughout the subsequent solution
preparations.
8. Sample Preparation
8.1 Coal and Coke—Prepare the analysis sample in accor-
dance with Practice D2013 for coal or Practice D346 for coke
by pulverizing the material to pass a 250 µm (No. 60) U.S.A.
standard sieve.
8.1.1 Analyze separate test portions for moisture and ash
contents in accordance with Test Methods D3173, D3174, or
D7582, so that calculations to other bases can be made.
8.2 Laboratory Ashing of Coal and Coke Analysis Sample—
Prepare the ash from a thoroughly mixed analysis sample of
coal or coke (8.1). Spread the coal and coke in a layer not over
6 mm in depth in a porcelain, quartz, or fused silica roasting
dish. Place the dish in a cold muffle furnace and heat gradually
so that the temperature reaches 500 °C 6 10 °C at the end of
1 h. Continue the gradual heating until the temperature rises
from 500 °C 6 10 °C to 750 °C 6 15 °C at the end of 1 h.
Maintain the 750 °C temperature until the test specimen
reaches a constant mass or for an additional 2 h. Allow the dish
to cool, transfer to an agate mortar, and grind to pass a 75 µm
(No. 200) U.S.A. standard sieve. Reignite the ash at 750 °C for
1 h, cool rapidly, and determine the mass of portions for
analysis.
8.3 Solid Combustion Residue—Dry a representative por-
tion of the solid residue to constant mass at 107 °C 6 3 °C.
Determine the moisture loss during this drying step if it is
desirable to calculate results to an as-received basis. Crush the
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dried portion of the sample to pass a 75 µm (No. 200) U.S.A.
standard sieve. Use a mill that minimizes metal contamination.
8.4 Ashing Solid Combustion Residue—Spread an appropri-
ate amount of the prepared sample in a layer not over 2 mm in
a porcelain, quartz, or fused silica roasting dish. Place the dish
in a cold muffle furnace and heat gradually so that the
temperature reaches 500 °C 6 10 °C at the end of 1 h.
Continue the gradual heating until the temperature rises from
500 °C 6 10 °C to 750 °C 6 15 °C at the end of 1 h. Maintain
the 750 °C temperature until the combustion residue reaches a
constant mass or for an additional 2 h. Allow the test specimen
to cool, grind to pass a 75 µm (No. 200) U.S.A standard sieve,
and reignite at 750 °C for 1 h.
8.5 If previously ignited samples are stored and the absorp-
tion of moisture or CO2, or both, is in question, reignite the ash
at 750 °C before use. Alternatively, determine loss on ignition
using Test Method D7348 on a separate sample whose mass is
determined out at the same time as the test portion and make
the necessary corrections. Thoroughly mix each sample before
weighing.
9. Procedure
9.1 The solutions and proportions described below are for
typical ash samples as represented by American coals of
bituminous rank. Therefore, stronger or weaker dilutions may
be required to establish suitable mass concentrations for those
elements of varying percentages outside the range of the
typical sample. Each analyst must determine the sensitivity and
linear range of calibration of their equipment and choose mass
concentration ranges for standards compatible with the samples
and instrument specific to their own work.
9.1.1 Calculations used in subsequent sections are devel-
oped from the following general formula for mass fraction of
element oxide, E, %, in moisture-free coal ash:
E 5 @ ~ C 2 B ! / ~ A 2 B ! # 3 ~ N/M ! 3 F 3 100
where:
A =absorbance of standard solution,
B =absorbance of blank solution,
C =absorbance of sample solution,
N =mass concentration of the element in the standard
solution, µg/mL,
M = mass concentration of the test portion mass in
solution, for example, 200 µg ⁄mL from 9.4.1 or
50 µg ⁄mL from 9.4.2,
F = conversion factor from element to oxide,
dimensionless, and
100 = conversion factor from a mass fraction to a
percentage, %.
9.1.1.1 Percent mass fractions in the ash may be converted
to the dry coal basis using the following expression:
w C 5 w A w B ⁄100
where:
wC = elemental oxide (dry basis) mass fraction in coal, %,
wA = elemental oxide mass fraction in ash, %,
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D3682 − 21
wB = ash (dry basis) mass fraction as determined in Test
Method D3174 or Test Method D7582, %, and calcu-
lated using Practice D3180, and
100 = factor to correct the product of two percent values to
a single percent value, %.
9.1.1.2 See Practice D3180 for procedures to convert values
to other bases.
9.2 To minimize the potential of contamination, the plati-
num ware, if used, must be prepared by boiling in solvent acid
(for example, HCl or HNO3 (7.12), but never a mixture of both
since the mixture would dissolve platinum) and rinsing thor-
oughly with reagent-grade water. After this initial cleaning, the
platinum ware must be handled with clean tongs and protected
from further contamination from table tops, and so forth. All
glassware used in analyses must be equally clean and equally
protected.
9.3 Sample Fusion and Solution:
9.3.1 Sample Fusion—Transfer 0.1 g 6 0.0002 g of the
sample as prepared in 8.2 – 8.5 into a platinum vessel (6.3)
(Note 3) and add 0.5 g of Li2B4O7. Mix the ash and lithium
tetraborate well, then add an additional 0.5 g of Li2B4O7 to
cover the mixture. Place the platinum vessel in a clean silica or
refractory tray and place in a muffle furnace preheated to
1000 °C; 15 min at 1000 °C is sufficient to fuse the mixture
completely. Remove the tray and dish and cool to room
temperature. Carefully rinse the bottom and outside of the
platinum vessel with the solvent acid (7.13.3) to remove
possible contamination, then place it in a clean 250 mL or
400 mL beaker.
NOTE 3—The use of graphite crucibles and subsequent dissolution of
fused beads from them was not investigated; however, their successful use
in similar methods has been reported.3
9.3.2 Solution—Place a clean polymer-coated stirring mag-
net inside the beaker, and immediately place the beaker on the
stirring hotplate. Heat the solution to just below boiling
(1)
temperature and maintain for not more than 30 min with
constant stirring. This time and temperature are sufficient to
completely dissolve the melt. If stirring is not maintained
constantly, some of the ash constituents are apt to precipitate
and the analysis must be repeated.
9.3.3 Remove the beaker from the hotplate and permit it to
cool to room temperature. Wash the platinum vessel, if used,
with small amounts of solvent acid into the beaker. Quantita-
tively transfer the solution to a 200 mL volumetric flask. Rinse
the beaker with small amounts of solvent acid, add the rinsings
to the flask, and dilute to the 200 mL mark with the solvent
acid. This solution is 500 µg ⁄mL with respect to the total
sample mass and contains 5 g ⁄L of Li2B4O7 solution.
9.4 Sample Dilution
9.4.1 Solution 1—Pipet 20 mL of the sample solution pre-
pared in 9.3.3 into a 50 mL volumetric flask and dilute to
(2) volume with solvent acid. This solution is 200 µg ⁄mL with
respect to the total sample mass and contains 2 g ⁄L of Li2B4O7.
9.4.2 Solution 2—Pipet 10 mL of the sample solution pre-
pared in 9.3.3 into a 100 mL volumetric flask, add 10 mL of
lanthanum solution (see 7.6), and dilute to volume with solvent
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acid. This solution is 50 µg ⁄mL with respect to the total sample 11.2 Blank Solution—Use the blank as prepared in 10.2.
mass and contains 0.5 g ⁄L of Li2B4O7.
11.3 Sample Dilution Solution 1—Use the 200 µg ⁄mL
9.4.3 Include lanthanum in the solution as a release agent in
sample mass dilution as prepared in 9.4.1.
those determinations that may require it (for example, cal-
cium). If this solution is to be used solely for the analysis of 11.4 Atomic Absorption Operating Conditions—Use an alu-
sodium or potassium, or both, lanthanum is not needed. minum hollow-cathode lamp and set the monochromator at
Alternative measures to using lanthanum, such as the use of 309.2 nm. Use a nitrous oxide-acetylene flame. Adjust other
nitrous oxide flame, are permissible. instrument parameters to optimum for the particular equipment
used.
10. Silicon Dioxide (SiO2)
11.5 Determination—Read out absorbance values for the
10.1 Preparation of Standards—Prepare a series of stan-
blank solution, standard solutions, and sample solution. Deter-
dards by combining the following volumes of the silicon (Si)
mine wAl2O3, the mass fraction of Al2O3, %, as follows:
stock solution (see 7.10) with 1 mL of the aluminum stock
solution (see 7.3) and diluting to 100 mL with the blank
solution (see 10.2) as outlined in Table 1. Only those standards
w Al2O3 5 F C2B
A2B GS D~ !
N
M
F 100 (4)

need be prepared that bracket the expected SiO2 mass concen- where:
trations in the sample solutions.
A =absorbance of standard nearest C,
10.2 Blank Solution—Prepare a solution of 2 g ⁄L of B =absorbance of blank,
Li2B4O7 solution in solvent acid. C =absorbance of sample,
10.3 Sample Dilution Solution 1—Use the 200 µg ⁄mL N =aluminum in standard solution, µg/mL,
M =mass concentration of the test portion mass in
sample mass dilution solution as prepared in 9.4.1.
solution, µg/mL, for example, 200 µg ⁄mL,
10.4 Atomic Absorption Operating Conditions—Use a sili- F = conversion from element to oxide, for example, 1.889
con hollow-cathode lamp and set the monochromator at for Al2O3/2Al, dimensionless, and
251.6 nm. Use a nitrous oxide/acetylene flame. Adjust other 100 = factor to correct the product of two percent values to
instrument parameters to optimum for the particular equipment a single percent value, %.
used.
10.5 Determination—Read out absorbance values for the 12. Iron Oxide (Fe2O3)
blank solution, standard solutions, and sample solution. In this 12.1 Preparation of Standards—Prepare standard solutions
and all subsequent determinations, those instruments so containing from 2 µg ⁄mL to 10 µg ⁄mL iron and 10 mL of
equipped may be calibrated to read out “percent” directly. lanthanum solution per 100 mL. Dilute with blank solution
Determine wSiO2, the mass fraction of SiO2, %, as follows: (12.2).
w SiO2 5 F C2B
A2B GS D~ !
N
M
F 100 (3) 12.2 Blank Solution—Prepare a solution of solvent acid
containing 0.5 g ⁄L Li2B4O7.
where:
12.3 Sample Dilution Solution 2—Use the 50 µg ⁄mL sample
A =absorbance of standard solution nearest C, mass dilution as prepared in 9.4.2.
B =absorbance of blank solution,
C =absorbance of sample solution, 12.4 Atomic Absorption Operating Conditions—Use an iron
N =silicon in standard solution, µg/mL, hollow-cathode lamp and set the monochromator at 248.3 nm.
M =mass concentration of the test portion mass in Use an air-acetylene flame of stoichiometric composition.
solution, µg/mL, for example, 200 µg ⁄mL, Adjust other instrument parameters to optimum for the particu-
F = conversion from element to oxide, for example, 2.139 lar equipment used.
for SiO2/Si, dimensionless, and
100 = factor to correct the product of two percent values to 12.5 Determination—Read the absorbance values for the
a single percent value, %. blank solution, the standard solutions, and the sample solution.
Determine wFe2O3, the mass fraction of Fe2O3, %, as follows:
11. Aluminum Oxide (Al2O3)
11.1 Preparation of Standards—Prepare standard solutions
w Fe2O3 5 F C2B
A2B GS D
N
M
~ F ! 100 (5)
containing from 10 µg ⁄mL to 30 µg ⁄mL aluminum and dilute
where:
with blank solution (10.2).
A = absorbance of standard nearest C,
B = absorbance of blank,
TABLE 1 SiO2 Standards
C = absorbance of sample,
Silicon (Si), Stock Silicon Standard Series, Equivalent wSiO2, % N = iron in standard solution, µg/mL,
Solution (7.10), mL µg/mL
25 50 53.5
M = mass concentration of the test portion mass in
20 40 42.8 solution, µg/mL, for example, 50 µg ⁄mL,
15 30 32.1 F = conversion from element to oxide, for example, 1.430
10 20 21.4
for Fe2O3/2Fe, dimensionless, and

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100 = factor to correct the product of two percent values to B =

absorbance of blank,
a single percent value, %. C =
absorbance of sample,
N =
magnesium in standard solution, µg/mL,
13. Calcium Oxide (CaO) M =
mass concentration of the test portion mass in
13.1 Preparation of Standards—Prepare standard solutions solution, µg/mL, for example, 50 µg ⁄mL,
containing 1 µg ⁄mL to 10 µg ⁄mL calcium and 10 mL of lan- F = conversion from element to oxide, for example, 1.658
thanum solution per 100 mL. Dilute with the blank solution as for MgO/Mg, dimensionless, and
described in 12.2. 100 = factor to correct the product of two percent values to
a single percent value, %.
13.2 Blank Solution—Use blank solution as described in
12.2. 15. Sodium Oxide (Na2O)
13.3 Sample Dilution Solution 2—Use the 50 µg ⁄mL sample 15.1 Preparation of Standards—Prepare standard solutions
mass dilution as described in 9.4.2. containing 0.5 µg ⁄mL to 2 µg ⁄mL sodium and 10 mL of
13.4 Atomic Absorption Operating Conditions—Use a cal- lanthanum5 solution per 100 mL. Dilute with blank solution as
cium hallow-cathode lamp and set the monochromator at described in 12.2.
422.7 nm. Use an air-acetylene flame. Adjust other instrument 15.2 Blank Solution—Use blank solution as described in
parameters to optimum for the particular equipment used. 12.2.
13.5 Determination—Read the absorbance values for the 15.3 Sample Dilution Solution 2—Use the 50 µg ⁄mL sample
blank solution, the standard solutions, and the sample solution. mass dilution as described in 9.4.2.
Determine wCaO, the mass fraction of CaO, %, as follows:
15.4 Atomic Absorption Operating Conditions—Use a so-
w CaO 5
C2B
A2BF GS D N
M
~ F ! 100 (6)
dium hollow-cathode lamp and set the monochromator at
589.0 nm. Use an air-acetylene flame. Adjust other instrument
where: parameters to optimum for the particular equipment used.
A =absorbance of standard nearest C, 15.5 Determination—Read the absorbance values for the
B =absorbance of blank, blank solution, the standard solutions, and the sample solution.
C =absorbance of sample, Determine wNa2O, the mass fraction of Na2O, %, as follows:
N =calcium in standard solution, µg/mL,
M =mass concentration of the test portion mass in
solution, µg/mL, for example, 50 µg ⁄mL,
w Na2O 5 F C2B
A2B GS D~ !
N
M
F 100 (8)

F = conversion from element to oxide, for example, 1.399 where:

for CaO/Ca, dimensionless, and A =absorbance of standard nearest C,
100 = factor to correct the product of two percent values to B =absorbance of blank,
a single percent value, %. C =absorbance of sample,
N =sodium in standard solution, µg/mL,
14. Magnesium Oxide (MgO) M =mass concentration of the test portion mass in
14.1 Preparation of Standards—Prepare standard solutions solution, µg/mL, for example, 50 µg ⁄mL,
containing 0.5 µg ⁄mL to 2 µg ⁄mL magnesium and 10 mL of F = conversion from element to oxide, for example, 1.348
lanthanum solution per 100 mL. Dilute with blank solution as for Na2O/2Na, dimensionless, and
described in 12.2. 100 = factor to correct the product of two percent values to
a single percent value, %.
14.2 Blank Solution—Use blank solution as described in
NOTE 4—Alternatively, sodium may be determined by flame emission.
12.2.
14.3 Sample Dilution Solution 2—Use the 50 µg ⁄mL sample 16. Potassium Oxide (K2O)
mass dilution as described in 9.4.2. 16.1 Standard Preparation—Prepare standard solutions
14.4 Atomic Absorption Operating Conditions—Use a mag- containing 0.5 µg ⁄mL to 2 µg ⁄mL potassium and 10 mL of
nesium hollow-cathode lamp and set the monochromator at lanthanum5 solution per 100 mL. Dilute with blank solution as
285.1 nm. Use an air-acetylene flame of stoichiometric com- described in 12.2.
position. Adjust other instrument parameters to optimum for 16.2 Blank Solution—Use blank solution as described in
the particular equipment used. 12.2.
14.5 Determination—Read the absorbance values for the 16.3 Sample Dilution Solution 2—Use the 50 µg ⁄mL sample
blank solution, the standard solutions, and the sample solution. mass dilution as described in 9.4.2.
Determine wMgO, the mass fraction of MgO, %, as follows:
16.4 Atomic Absorption Operating Conditions—Use a po-
w MgO 5
C2B
A2BF GS D~ !
N
M
F 100 (7)
tassium hollow-cathode lamp and set the monochromator at

where: 5
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D05-1000. Contact ASTM Customer
A = absorbance of standard nearest C, Service at service@astm.org.

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 D3682 − 21
766.5 nm. Use an air-acetylene flame. Adjust other instrument 18. Report
parameters to optimum for the particular equipment used. 18.1 Report the percentages for the elemental oxides in the
16.5 Determination—Read the absorbance values for the ash as specified in 10.5, 11.5, 12.5, 13.5, 14.5, 15.5, 16.5, and
blank solution, the standard solution, and the sample solution. 17.5.
Determine wK2O, the mass fraction of K2O, %, as follows: 18.2 Report the method used for concurrent moisture and
w K2O 5
C2B
A2B F GS D~ !
N
M
F 100 (9)
ash determination, if applicable.
18.3 Use Practice D3180 for procedures to convert values to
where: other bases.
A =absorbance of standard nearest C, 19. Precision and Bias
B =absorbance of blank,
C =absorbance of sample, 19.1 Precision—The precision of this test method is in
N =potassium in standard solution, µg/mL, accordance with Table 2. The precision characterized by the
M =mass concentration of the test portion mass in repeatability (Sr, r) and reproducibility (SR, R) is in accordance
solution, µg/mL, for example, 50 µg ⁄mL, with Table A1.1.
F = conversion from element to oxide, for example, 1.205 19.1.1 Repeatability Limit (r)—The value below which the
for K2O/2K, dimensionless, and absolute difference between two test results of separate and
100 = factor to correct the product of two percent values to consecutive test determinations, carried out on the same
a single percent value, %. sample in the same laboratory by the same operator using the
NOTE 5—Alternatively, potassium may be determined by flame emis- same apparatus on samples taken at random from a single
sion. quantity of homogeneous material, may be expected to occur
NOTE 6—It may be found convenient to combine the standards for iron, with a probability of approximately 95 %.
calcium, magnesium, sodium, and potassium in one solution.
19.1.2 Reproducibility Limit (R)—The value below which
the absolute difference between two test results, carried out in
17. Titanium Dioxide (TiO2)
different laboratories using samples taken at random from a
17.1 Standard Preparation—Prepare a standard solution single quantity of material that is as nearly homogeneous as
containing 3 µg ⁄mL titanium and 5 g ⁄L of Li2B4O7 solution possible, may be expected to occur with a probability of
dissolved in solvent acid. If required, successive dilutions may approximately 95 %.
be made with the blank solution (see 17.2). 19.2 Bias—The NIST Standard Reference Material 1633b
17.2 Blank Solution—Prepare a solution containing 5 g/L of was included in the interlaboratory study to ascertain possible
Li2B4O7 solution dissolved in solvent acid. bias between reference material values and those determined
17.3 Sample Dilution Solution—Use the original undiluted by this test method. A comparison of the NIST values and those
500 µg ⁄mL sample mass solution as prepared in 9.3.3. obtained in the interlaboratory study are given in Table 3.

17.4 Atomic Absorption Operating Conditions—Use a tita- 19.3 An interlaboratory study, designed in accordance with
nium hollow-cathode lamp and set the monochromator at Practice E691, was conducted in 1999. Six laboratories par-
364.3 nm. Use a nitrous oxide-acetylene flame. Adjust other ticipated.5
instrument parameters to optimum for the particular equipment 20. Keywords
used.
20.1 aluminum oxide (A12O3); ash analysis; atomic absorp-
17.5 Determination—Read the absorbance for the blank tion spectroscopy; calcium oxide (CaO); elemental ash com-
solution, the standard solution, and the sample solution. De- position; ferric oxide (Fe2O3); magnesium oxide (MgO); po-
termine wTiO2, the mass fraction of TiO2, %, as follows: tassium oxide (K2O); silicon dioxide (SiO2); sodium oxide
(Na2O); titanium dioxide (TiO2)
w TiO2 5 F C2B
A2B GS D~ !
N
M
F 100 (10)

where: TABLE 2 Mass Fraction Ranges and Limits for Repeatability and
Reproducibility for Major and Minor Elemental Oxides in Ash
A =absorbance of standard, from Combustion Residues
B =absorbance of blank,
Elemental Mass Fraction Range, Repeatability Limit Reproducibility Limit
C =absorbance of sample, Oxide % r R
N =titanium in standard solution, µg/mL, for example, SiO2 29.75 to 58.45 -0.140 + 0.031x̄A 0.146 + 0.093x̄A
3 µg ⁄mL, Al2O3 11.32 to 31.71 0.298 + 0.013x̄A 0.126 + 0.063x̄A
M = mass concentration of the test portion mass in Fe2O3 2.97 to 41.12 0.166 + 0.015x̄A 0.274 + 0.066x̄A
MgO 0.45 to 7.12 0.043 + 0.016x̄A 0.082 + 0.110x̄A
solution, µg/mL, for example, 500 µg ⁄mL, CaO 1.44 to 22.14 0.136 + 0.028x̄A 0.091 + 0.078x̄A
F = conversion from element to oxide, for example, 1.668 TiO2 0.58 to 1.44 -0.006 + 0.087x̄A 0.023 + 0.169x̄A
for TiO2/Ti, dimensionless, and K2O 0.46 to 3.00 0.011 + 0.041x̄A 0.050 + 0.064x̄A
Na2O 0.14 to 7.15 0.023 + 0.025x̄A 0.060 + 0.123x̄A
100 = factor to correct the product of two percent values to
A
a single percent value, %. Where x̄ is the average of two single test results.

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TABLE 3 Comparison of Certified Values for Standard Reference
Material 1633b with Interlaboratory Study Values for Major and
Minor Elemental Oxides in Ash from Combustion Residues
Elemental Significant (95 %
AA-RR Value, % NIST Value, % Bias, %
Oxide Confidence Level)
SiO2 49.57 ± 1.04 49.25 ± 0.17 0.65 no
Al2O3 28.22 ± 0.44 28.44 ± 0.51 –0.79 no
Fe2O3 10.89 ± 0.14 11.12 ± 0.33 –2.10 no
MgO 0.787 ± 0.030 0.799 ± 0.013 –1.49 no
CaO 2.015 ± 0.092 2.11 ± 0.08 –4.48 no
TiO2 1.279 ± 0.048 1.32 ± 0.02 –3.09 no
K2O 2.251 ± 0.041 2.35 ± 0.04 –4.20 yes
Na2O 0.255 ± 0.019 0.271 ± 0.004 –5.90 no

ANNEX

(Mandatory Information)

A1. PRECISION STATISTICS

A1.1 The precision of this test method, characterized by

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

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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 33.24 0.399 1.371 1.12 3.84 CAN 4.50 0.079 0.170 0.22 0.48
FPA 58.45 0.859 1.762 2.41 4.93 FPA 1.44 0.043 0.090 0.12 0.25
IL 48.28 0.132 2.014 0.37 5.64 IL 4.40 0.077 0.195 0.22 0.55
JO 40.17 0.242 1.271 0.68 3.56 JO 7.48 0.170 0.298 0.48 0.84
WDK 34.64 0.290 0.920 0.81 2.58 WDK 17.51 0.349 0.758 0.98 2.12
95-1 30.38 0.355 0.823 0.99 2.30 95-1 22.14 0.221 0.927 0.62 2.59
95-6 29.74 0.401 1.236 1.12 3.46 95-6 19.66 0.176 0.755 0.49 2.12
SRM 1633b 49.57 0.540 1.801 1.51 5.04 SRM 1633b 2.02 0.059 0.159 0.17 0.45
Al2O3 TiO2
Materials Average Sr SR r R Materials Average Sr SR r R
CAN 11.32 0.131 0.330 0.37 0.92 CAN 0.58 0.015 0.042 0.04 0.12
FPA 29.48 0.206 0.552 0.58 1.55 FPA 1.44 0.050 0.093 0.14 0.26
IL 19.20 0.173 0.588 0.48 1.65 IL 0.93 0.039 0.058 0.11 0.16
JO 31.71 0.209 0.867 0.59 2.43 JO 1.16 0.045 0.064 0.13 0.18
WDK 15.86 0.148 0.465 0.41 1.30 WDK 0.88 0.017 0.079 0.05 0.22
95-1 19.21 0.200 0.312 0.56 0.87 95-1 1.15 0.026 0.068 0.07 0.19
95-6 19.51 0.284 0.590 0.79 1.65 95-6 1.30 0.034 0.066 0.09 0.18
SRM 1633b 28.22 0.297 0.770 0.83 2.16 SRM 1633b 1.28 0.027 0.084 0.07 0.24
K2O Na2O
Materials Average Sr SR r R Materials Average Sr SR r R
CAN 1.37 0.023 0.053 0.07 0.15 CAN 0.14 0.007 0.021 0.02 0.06
FPA 3.00 0.052 0.080 0.15 0.23 FPA 0.26 0.009 0.027 0.03 0.08
IL 2.19 0.027 0.071 0.08 0.20 IL 1.37 0.016 0.073 0.05 0.20
JO 0.52 0.013 0.029 0.04 0.08 JO 0.25 0.007 0.028 0.02 0.08
WDK 0.54 0.016 0.027 0.04 0.08 WDK 1.07 0.020 0.058 0.06 0.16
95-1 0.46 0.010 0.027 0.03 0.08 95-1 3.56 0.044 0.233 0.12 0.65
95-6 0.65 0.012 0.033 0.03 0.09 95-6 7.15 0.071 0.440 0.20 1.23
SRM 1633b 2.25 0.041 0.072 0.11 0.20 SRM 1633b 0.26 0.016 0.034 0.04 0.09
Fe2O3 MgO
Materials Average Sr SR r R Materials Average Sr SR r R
CAN 41.12 0.296 1.079 0.83 3.02 CAN 0.45 0.015 0.038 0.04 0.11
FPA 2.97 0.044 0.137 0.12 0.38 FPA 1.05 0.015 0.053 0.04 0.15
IL 15.86 0.128 0.480 0.36 1.34 IL 0.95 0.024 0.065 0.07 0.18
JO 4.64 0.172 0.275 0.48 0.77 JO 1.32 0.028 0.064 0.08 0.18
WDK 6.57 0.047 0.341 0.13 0.95 WDK 4.31 0.044 0.169 0.12 0.47
95-1 6.54 0.128 0.181 0.36 0.51 95-1 7.21 0.042 0.173 0.12 0.49
95-6 5.33 0.086 0.256 0.24 0.72 95-6 6.20 0.065 0.263 0.18 0.74
SRM 1633b 10.89 0.092 0.247 0.26 0.69 SRM 1633b 0.79 0.016 0.051 0.05 0.14

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