Designation: D8010 − 16

Standard Practice for

Determination of Water Soluble Alkali Content in Coal1
This standard is issued under the fixed designation D8010; 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 3. Terminology
1.1 This practice describes a procedure for the determina- 3.1 For definitions of terms used in this practice, refer to
tion of water soluble sodium as sodium oxide (Na2O) and Terminology D121.
potassium as potassium oxide (K2O) in the analysis of coal
samples prepared in accordance with Practice D2013. 4. Summary of Practice
1.2 The values stated in SI units are to be regarded as 4.1 Sodium and potassium salts are leached from the sample
standard. No other units of measurement are included in this during a lengthy digestion with water and a wetting agent. The
standard. concentrations of sodium and potassium are measured in the
1.3 This practice is derived in part from the ASME proce- filtered liquid by an appropriate spectrometric technique for the
dure water soluble alkalis.2 elements sodium and potassium.
1.4 This standard does not purport to address all of the 5. Significance and Use
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 5.1 Results obtained from the practice are used to serve a
priate safety and health practices and determine the applica- number of interests, including the indication of possible boiler
bility of regulatory limitations prior to use. tube fouling and possible furnace corrosion problems.

2. Referenced Documents 6. Interferences

3
2.1 ASTM Standards: 6.1 Several types of interference effects may contribute to
D121 Terminology of Coal and Coke inaccuracies in the determination of sodium and potassium.
D1193 Specification for Reagent Water Follow the manufacturer’s operating guide to develop and
D2013 Practice for Preparing Coal Samples for Analysis apply correction factors to compensate for the interferences.
D3173 Test Method for Moisture in the Analysis Sample of
Coal and Coke 7. Apparatus
D3302 Test Method for Total Moisture in Coal 7.1 Analytical balance, with sensitivity of 0.1 mg.
D3180 Practice for Calculating Coal and Coke Analyses
from As-Determined to Different Bases 7.2 Digestion Apparatus
D7448 Practice for Establishing the Competence of Labora- 7.2.1 Stirring Hotplate and Bars, with operating tempera-
tories Using ASTM Procedures in the Sampling and ture up to 200 °C.
Analysis of Coal and Coke 7.2.1.1 Erlenmeyer flask with cover, 250 mL.
D7582 Test Methods for Proximate Analysis of Coal and 7.2.1.2 Refluxing column (optional).
Coke by Macro Thermogravimetric Analysis 7.2.2 Hot Block Digestion
E832 Specification for Laboratory Filter Papers 7.2.2.1 Polycarbonate Bottles, 250 mL capacity with an
O-ring seal and screw cap, capable of withstanding tempera-
tures up to 130 °C, the pressure that is developed during the
1
This test method is under the jurisdiction of ASTM Committee D05 on Coal digestion, and resistant to oxidation. Other types of bottles or
and Coke and is the direct responsibility of Subcommittee D05.21 on Methods of
Analysis. vials may be used provided they are capable of withstanding
Current edition approved Sept. 1, 2016. Published September 2016. Originally the temperatures and pressures developed during the digestion.
approved in 2015. Last previous edition approved in 2015 as D8010–15. DOI:
10.1520/D8010-16. 7.3 Filtering Apparatus
2
“Coal Fouling and Slagging Parameters.” ASME H-86. Editor E.C. 7.3.1 Filter Paper or 0.45 micron filter. The paper used must
Winegartner, 1974.
3
be ash-free, quantitative Type II filter paper, as described in
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Specification E832.
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 7.3.2 Filter (gravity or vacuum).
the ASTM website. 7.3.3 Volumetric flask, 250 mL.

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

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 D8010 − 16
7.4 Spectrometer—Because of the differences between vari- dance with Test Method D3173, D3302, or D7582 to permit
ous makes and models of satisfactory instruments, no detailed calculations to other than as-determined bases.
operating instructions can be provided. Instead, follow the
instructions provided by the manufacturer of the particular 10. Procedure
instrument. Sensitivity, instrumental detection limit, precision,
10.1 The solutions and proportions described below are the
linear dynamic range, and interference effects must be inves-
typical samples as represented by American coals. Therefore,
tigated and established for each individual analyte line on that
stronger or weaker dilutions may be required to establish
particular instrument. All measurements must be within the
suitable concentrations for those elements of varying percents
instrument’s linear range in which correction factors are valid.
outside the range of the typical sample. Analysts must deter-
It is the responsibility of the analyst to verify that the
mine the sensitivity and linear range of calibration of their own
instrument configuration and operating conditions used satisfy
equipment and choose concentration ranges for standards
the analytical requirements of this method and to maintain
compatible with the samples and instrument specific to their
quality control data confirming instrument performance and
own work.
analytical results.
10.2 Sample Digestion
8. Reagents and Materials 10.2.1 Method A, Hot Plate—Accurately weigh 5 g of
8.1 Purity of Reagents—Use reagent grade chemicals in all sample to the nearest 0.1 mg into a 250 mL Erlenmeyer flask.
tests that conform to the specifications of the Committee on The sample may be wetted with 1 to 5 mL of wetting agent.
Analytical Reagents of the American Chemical Society,4 where Add 100 mL of water to the flask. Place the flask with sample
such specifications are available. onto the hot plate and cover. Allow to digest just under boiling
8.2 Purity of Water—Unless otherwise indicated, references for at least 16 h. Do not allow the sample to go to dryness (a
to water are understood to mean Type II reagent water as refluxing column may be used to prevent this). Allow to cool to
defined in Specification D1193. room temperature. Filter by either gravity filtration or vacuum
filtration into a 250 mL volumetric flask. Once filtration is
8.3 Wetting Agent—Approximately 1 to 5 mL of isopropyl complete, dilute the filtrate to volume (250 mL) with water and
alcohol, methanol or ethanol may be added to the sample. mix by inversion.
8.4 Calibration Standards—Standard stock solutions of 10.2.2 Method B, Hot Block—Accurately weigh 1 g of
1000 mg ⁄L for each element are needed for preparation of sample to the nearest 0.1 mg into a weighing dish and
dilute calibration standards in the nominal range from <0.1 to quantitatively transfer to a polycarbonate bottle. The sample
100 mg/L. Prepare calibration standard solutions from 99.99 % may be wetted with 1 to 5 mL of wetting agent. Add 25 mL of
(mass/mass) purity metals or salts. Alternatively, use commer- water to the tube. Place the sample on the hot block and digest
cially available standard stock solutions specifically prepared at 120 6 5 °C for 16 h. Do not allow the sample to go to
for the correct spectroscopy method. Dilute calibration stan- dryness. Allow to cool to room temperature. Filter by either
dard solutions are also used initially and periodically to verify gravity filtration or vacuum filtration into a 50 mL centrifuge
the baseline of the calibration has not changed significantly. tube. Once filtration is complete, dilute the filtrate to volume
8.5 Blank Solutions—Two types of blank solutions are (50 mL) with water and mix by inversion.
required: a calibration blank of water that is used to establish 10.3 Determination of Sodium and Potassium in the Test
the analytical calibration curve and a method blank which is Solution—Measure the concentrations of sodium and potas-
used to evaluate possible contamination and assess spectral sium in the test solution (filtrate from 10.2.1 or 10.2.2)
background. The calibration blank is also used initially and according to the selected spectrometric method.
periodically to verify the baseline of the calibration has not
changed significantly. 11. Instrument Operation
8.5.1 Calibration Blank—water.
11.1 Consult the manufacturer’s instructions for the chosen
8.5.2 Method Blank—Process the method blank through the
spectrometer. The present method assumes that good operating
same digestion procedure as the samples, using the same
procedures are followed. Design differences among instru-
volumes of water and wetting agent as used in preparing the
ments and different selected analytical wavelengths for indi-
samples.
vidual spectrometers make it impractical to list detailed con-
9. Analysis Sample ditions.
9.1 Prepare the analysis sample in accordance with Practice 11.2 Calibration Procedure—Calibrate the instrument ac-
D2013 for coal by pulverizing the material to pass a 250 µm cording to the procedure recommended by the manufacturer
(No. 60) U.S.A. standard sieve. Determine moisture in accor- using a calibration blank and calibration standards.
11.3 Initial Calibration Verification—Before analyzing test
4
Reagent Chemicals, American Chemical Society Specifications, American samples, analyze the method blank and verify the proper
Chemical Society, Washington, DC. For suggestions on the testing of reagents not calibration of the instrument by analyzing a reference material.
listed by the American Chemical Society, see Analar Standards for Laboratory
Results for the reference material must be within the stated
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, uncertainty limits or the calibration procedure must be re-
MD. peated.

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 D8010 − 16
11.4 Periodic Calibration Verification and 12.2.2
Recalibration—In accordance with Guide D7448, analyze a ~ A 2 B ! VC ~1 g K!
control sample on a periodic basis. Results obtained for the %K 2 O ~ as Det! 5 3 1.205 3 3 100 %
D ~ 1000 mg K !
control sample must be within 10 % of the stated value or all
(2)
results obtained since the last successful control check for that
element must be rejected and the calibration procedure re- where:
peated. A = as measured concentration of K, mg/L,
B = as measured concentration of blank, mg/L,
12. Report V = volume of solution, L
12.1 For reporting analyses to other than as-determined C = dilution factor, if applied, and
basis, refer to Practice D3180. D = sample mass, g (as determined).
12.2 For instruments that do not have calculation functions Note:
provided by the manufacturer for converting the concentration ~M W K2 O!
51.205
amount of the analyte as analyzed to the appropriate oxide, the 2~A W K!
following calculations can be used: where:
12.2.1
MW = molecular weight, and
~ A 2 B ! VC ~1 g N a! AW = atomic weight.
%Na 2 O ~ as Det! = D
3 1.348 3
~ 1000 mg Na!
3 100 % (1) 13. Keywords
where: 13.1 alkali; potassium oxide; sodium oxide; water soluble
A = as measured concentration of Na, mg/L,
B = as measured concentration of blank, mg/L,
V = volume of solution, L
C = dilution factor, if applied, and
D = sample mass, g (as determined basis).
Note:
~ MW Na 2 O !
51.348
2 ~ AW Na!
where:
MW = molecular weight, and
AW = atomic weight.

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