ENERGY EXPLORATION & EXPLOITATION · Volume 28 · Number 2 · 2010 pp.

105-115 105

Microwave Acid Digestion for the Determination of

Metals in Subbitumnious Coal Bottom Ash by ICP-OES
Abdurrahman Saydut
Dicle University, Engineering Faculty, Mining Engineering Department,
Diyarbakir TR-21280, Turkey
E-mail: saydut@dicle.edu.tr

(Received 22 October 2009; accepted 5 April 2010)

Abstract
The development of precise and easy determination method for the metals in
fossil fuel is the essential factor for the study of problems which are caused by
the existence of metals in fuel. Coal contains many kinds of mineral matter
elements including metals derived from its generation. The sample preparation
method developed for metal determination in coal by spectroanalytical
technique is dry ashing, and wet acid microwave digestion. Microwave-acid
digestion (MW-AD) followed by inductively coupled plasma-optical emission
spectrometry (ICP-OES) was examined for the determination of metals (Cd, Co,
Cr, Cu, Fe, Mn, Mo, Ni, Pb, Zn) in coal bottom ash (CBA). Subbitumnious coal
from Hazro deposits in SE Anatolia of Turkey has been used in this study.
Metals in coal gave good recoveries for their certified or reference values.

Keywords: Coal, Bottom ash, ICP-OES, Metal, Microwave acid digestion,

Trace elements

1. INTRODUCTION
Coal is mainly a cluster of organic high molecular compound which consists of C, H,
O, N, and S. However, coal is also one of the components of crust, so that it contains
many kinds of mineral matter elements including metals derived from its generation
(Xu et al., 2005; Ayhan et al., 2005; Zhao et al., 2009). Element flows between coal,
bottom ash, fly ash and flue gases are under study with the aim to refine coal
combustion technology. The inorganic chemical composition of coal shows
information about the depositional environment, as well as the sources and differential
fixation of elements during coalification processes (Rodushkin et al., 2000; Erdogan
et al., 2005; Zhao and Sun, 2008). The behavior of mineral matter elements during
coal combustion process is very important because they not only cause slugging and
fouling, but also gives great influence upon the combustion characteristics due to
positive or negative catalytic effect. Furthermore, the existence of hazardous trace
elements, such as heavy metals, in coal has been a considerable problem on the
viewpoint of environmental safety. Some of these hazardous elements will be released
into air while some of them are distributed in bottom and fly ash. The development of
precise and easy determination method for the metals in coal is the essential factor for
106 Microwave Acid Digestion for the Determination of Metals
in Subbitumnious Coal Bottom Ash by ICP-OES

the study of some problems which are caused by the existence of metals in coal
(Goodarzi, 2002; Hamamci et al., 2003; Xu et al., 2005; Duz et al., 2005; Dai et al.,
2006; Tang et al., 2009). Therefore, it is crucial to develop a precise and easy method
for determining the various elements present in coal bottom ash (CBA) (Iwashita et
al., 2006). The principal sample preparation methods used for metal determination in
coal and coal products by spectroanalytical techniques, besides direct analysis, are
dilution with organic solvents, dilution in three-component systems (emulsion or
micro-emulsion), dry ashing and wet acid digestion. Direct analysis using little or no
sample preparation is most suitable for ETAAS with a graphite tube furnace and XRF
(Hardaway and Sneddon, 2004; Bingol and Akcay, 2005; Felipe-Sotelo et al., 2005).
The main advantage of direct analysis is obviously the time saving and the minimum
risk of analyte loss. The main problem might be in calibration, as standards might
behave differently from the samples, an effect that cannot be compensated for by
matrix matching or the analyte addition technique. Dilution with organic solvents is an
attractive preparation method because it is rapid and simple; it can be used for all
analytical techniques mentioned in literature. This procedure does not minimize the
high organic load, which is mostly a problem for the ICP techniques, and necessarily
requires the use of expensive metal-organic calibration solutions prepared in the same
way. Alternatively, the coal sample might be modified by formation of an emulsion or
micro-emulsion (three-component system). Whenever two immiscible liquids are
stirred, a macro-emulsion is obtained, either oil-in-water (O/W, droplets of oil in
water) or water-in-oil (W/O, droplets of water in oil), depending on the dispersed
phase. The kind of emulsion that is formed is mainly related to the formulation and to
a lesser degree to the W/O ratio. In this case, a co-solvent allows the formation of a
homogeneous system containing both the aqueous and the organic phase, resulting in
a homogeneous and long-term stable three component solution (Gugum and
Hamamci, 1993; Tsai and Tsai, 1998). An emulsion, a cloudy mixture, is prepared
agitating a mixture of water, oil and one or more surfactants under controlled
experimental conditions. A microemulsion is kind of an emulsion in which the
droplets are much smaller, thus the light passes through without much scattering, i.e.,
it appears as a clear solution. Micro-emulsions are formed by a mixture of water, oil
and an organic co-solvent, such as a short-chain alcohol (i.e. propan-1-ol), because its
molecules (Aydin et al., 2009a; 2009b). Dry ashing is used for the almost complete
elimination of organic materials prior to analyte determination, and consists of the
ignition of the organic matrix in air or in a stream of oxygen, followed by dissolution
of the residue in an acid medium. The time required for this procedure is one of the
disadvantages of this method. Another one is the risk of losses of volatile elements and
their compounds. For wet digestion, oxidizing agents are used to decompose the
organic constituents prior to analyte determination. Normally concentrated acids are
applied under heating, and the important aspects to consider are the strength of the
acids, their oxidizing and complexing power, their boiling points, the solubility of the
resulting salts, safety in manipulation, and purity. Wet digestion procedures for coal
samples can be performed in closed or open vessels, using thermal energy or
microwave radiation. Microwave heating offers a considerable advantage in time over
thermal heating. Many microwave-assisted sample preparation systems offer multi-
ENERGY EXPLORATION & EXPLOITATION · Volume 28 · Number 2 · 2010 107

sample preparation with temperature and pressure control features (Baysal et al., 2002;
Ozturk et al., 2010). For wet digestion procedures it is important to consider the time
consumption (several hours) and the amount of reagents used, in comparison to the
dilution methods (Sandroni et al., 2003; Xu et al., 2005; Wang et al., 2006; Duz et al.,
2009). Acid digestion assisted by microwave processing is popularly utilized for such
a pretreatment of the solid samples. (Iwashita et al., 2007)
In recent years, the acid-digestion assisted by microwave processing is popularly
utilized for such a pretreatment of solid matters. The microwave-assisted acid-
digestion (MW-AD) offers some advantages in short reaction time, the prevention of
vaporization, and the contamination control, compared to the conventional hot-plate
digestion methods (Xu et al., 2005). There have been many studies on the
determination of trace elements in coal and ash by use of the MW-AD (Iwashita et al.,
2007). For the microwave-assisted aciddigestion of coal samples, the combination of
HNO3 and HF is usually adopted because coal contains considerable amount of
inorganic matters (1-30 %), which mainly consists of aluminosilicate matrix
(Hatanpaa et al., 1997; Laban and Atkin, 1999; Rodushkin et al., 2002; Xu et al.,
2005). A variety of atomic spectrometric techniques have been used for the
determination of metals, among which are atomic absorption spectrometry (AAS) with
flame or graphite tube atomizers, inductively coupled plasma optical emission
spectrometry (ICP-OES) and XRF (Gumgum and Hamamci, 1991; Erdogan et al.,
2004; Akba et al., 2005; Sneddon et al., 2006; Iwashita et al., 2007).
The sample preparation method used in this study for metal determination in coal
by spectroanalytical technique is dry ashing, and wet acid microwave digestion. A
method is developed of the sample pretreatment and preparation procedures for metal
determination in CBA here. MW-AD followed by inductively coupled plasma-optical
emission spectrometry (ICP-OES) was examined for the determination of metals (Cd,
Co, Cr, Cu, Fe, Mn, Mo, Ni, Pb, Zn) in CBA.

2. EXPERIMENTAL
2.1. Sample preparation
Coal sample was obtained as lump from Hazro coalfield in SE Anatolia region of
Turkey. After oven drying at 105°C, sample was crushed by a jaw beaker (Retsch BB
1/A) and ground in a rotor beater mill (Retsch SRZ). The particle sizes of the samples
were less than 250 µm. Finely ground powdered coal samples, and the certified
reference standard materials, as received, were dried in an oven at 105°C until constant
weight was reached, and stored over silicagel in a desiccator. Heating value, ash and
sulfur content of samples were determined according to ASTM procedures. Elemental
analysis (C, H, N) for the coal sample was performed by a Carlo Erba elemental
analyzer EA 1108. Proximate and elemental analyses of the Hazro coal are shown in
Table 1. Samples were accurately weighed in a porcelain crucible and subject to a
calcination step in a muffle furnace at 650°C, for about 8 h.

2.2. Digestion procedures and measurement

Coal bottom ash samples were digested using Berghof MWS-3 model microwave
digestion system. The two-stage digestion was carried out as follows: 0.2 g portion of
108 Microwave Acid Digestion for the Determination of Metals
in Subbitumnious Coal Bottom Ash by ICP-OES

dried sample was weighed and transferred into a pressure-resistant PTFE

(polytetrafluoroethylene) vessel, and the mixture of acids (HNO3 +HF, 7:2 ml) was
added. The vessel was closed and heat in the microwave oven with the program as
described in Table 2. The vessels were removed and carefully vented in a fume hood
after cooling to room temperature in a water-bath. After the venting procedure
mentioned above, 15 ml of boric acid (H3BO3, saturated solution) was quickly added
to each sample. Crystallization of CaF2 is avoided by addition of boric acid. The
vessels were returned to the microwave oven and the second processing was applied
to the samples under the same temperature program above. The reaction mixture was
subjected to an evaporation procedure by use of the evaporation module in order to
remove the acids after the final digestion. Then the residue was dissolved in Milli-Q
water and filtrated, and the filtrate was diluted to 50 mL. The ICP-OES measurements
were performed for the diluted solutions. Coal bottom ash samples were evenly spaced
in the microwave oven carousel and procedure of MW-AD were applied.

Table 1. Roximate, elemental and sulfur analysis of Hazro coal.

Proximate Weight Sulfur Weight Elemental Weight

analysis (%) distribution (%) analysis (%)
Moisture 1.537 Total sulfur 7.540 Carbon 64.284
Ash 18.310 Pyritic sulfur 5.234 Nitrogen 1.020
Fixed Carbon 32.353 Sulphate sulfur 0.095 Hydrogen 4.708
Volatile mater 47.800 Organic sulfur 2.211
Heating value 6964.848
(k.cal.kg-1)

Table 2. Operating conditions for two-stage digestion by microwave oven.

Step 1 1 2 3
T 140 160 190
Ta (min)a 5 3 5
Time (min)b 5 10 20
Step 2 1 2
T°C 160 100
Ta (min)a 3 1
Time (min)b 15 15
a
Waiting time at desired temperature
b
The time between the two sequential temperatures

2.3. Reagents and instrumentation

Nitric acid (HNO3, 65%), hydrofluoric acid (HF, 40%) and boric acid (H3BO3,
saturated solution) were analytical grade reagents. Distilled water was further purified
by a Milli-Q system and used throughout the experiments. For the determination of
metal in CBA digested samples, MW-AD followed by ICP-OES (Perkin Elmer,
ENERGY EXPLORATION & EXPLOITATION · Volume 28 · Number 2 · 2010 109

Optima 2100 DV) were used. Instrumental conditions were optimized to obtain
sufficient sensitivity and precision (Table 3). Standard reference materials, SRM
1632c (Standard Reference Material), was used for evaluating the accuracy of the
present methods. SRM1632c was a bituminous coal certified by the National Institute
of Standards and Technology (NIST), USA. A certified reference material of coal,
NIST-1632c, was digested by MW-AD (Table 2) followed by the ICP-OES
measurement. The results are presented in Table 4 together with the certified or
reference values. The chosen wavelengths are shown in Table 5.

Table 3. Operating conditions for ICP-OES.

Parameter(Unit)
RF power (W) 1450
Plasma gas flow rate (L min–1) 15
Auxiliary gas flow rate (L min–1) 0.2
Nebulizer gas flow rate (L min–1) 0.8
Sample flow rate (L min–1) 1.5
View mode Axial-Radial
Read Peak area
Source equilibration time (s) 15
Read delay (s) 60
Replicates 3
Background correction 2-point (manual point correction)
Spray chamber Scott type spray chamber
Nebulizer Cross-Flow GemTip Nebulizer (HF resistant)
Detector CCD
Purge gas Nitrogen
Shear gas Air
Gas Argon

Table 4. Accuracy assessment through the analysis of the Coal Standard

Reference Material NIST SRM 1632c (µ µg g–1, dry wt.).

Element Found (Average) Certified (SRM 1632c)

Cd 0.071 (0.072 ± 0.007)
Co 3.42 3.48 ± 0.20
Cr 13.58 (13.73 ± 0.20)
Cu 5.92 (6.01 ± 0.25)
Fe 7355 (7350 ± 50)
Mn 12.90 (13.04 ± 0.53)
Ni 9.41 (9.32 ± 0.51)
Pb 3.50 (3.79 ± 0.07)
Zn 12.8 12.1 ± 0.7
110 Microwave Acid Digestion for the Determination of Metals
in Subbitumnious Coal Bottom Ash by ICP-OES

Table 5. Analytical wavelengths, detection limits and average concentration of

elements of coal bottom ash.

Element ICP-OES LOQ (µg/g) Concentration,

Wavelength (nm) (DF = 300) µg g–1
Cd 228.80 0.2 nda
Co 228.62 0.2 0.04±0.004
Cr 267.72 0.5 0.08±0.002
Cu 324.75 0.5 0.13±0.005
Fe 238.20 0.5 200.50±2.030
Mn 257.61 0.06 0.12±0.003
Ni 231.60 1.0 0.22±0.014
Pb 220.35 1.5 0.15±0.006
Zn 213.86 0.2 0.85±0.013
a
nd = not determined

3. RESULTS AND DISCUSSION

Coal sample was collected from Hazro deposites of SE Anatolia of Turkey for
determination of various (major and trace) elements in CBA. The global supply of
metal originates from primary sources such as ore feedstock, concentrates,
metallurgical slags, and petroleum residues. However, present primary resources are
insufficient to satisfy metal demand and in order to alleviate insufficient domestic
resources supply, many countries comprehensively utilize secondary resources
containing metal. The determination of metals in CBA is of economic concern but is
also of environmental concern. Metal mainly enters the environment from natural
sources and from the burning of fuel oils, asphaltites and coal. Indeed, uncontrolled
disposal of the ashes may cause a dispersion of fine particles containing products
hazardous to health. Exposure to metals may cause coughing, bronchial irritation,
gastrointestinal diseases and conjunctivitis (Isık et al., 2006; Erdogan et al., 2007).
The combustion of these a coal produces fly and bottom ashes that are characterized
by a high content of valuable elements such as vanadium, nickel, molybdenum,
uranium, thorium, sulfur and non-burnt carbon (Davydova, 2005; Erdogan et al.,
2007). Metal contamination is a significant problem in many manufacturing residues,
because it is well known that elements such as cadmium, chromium, lead, nickel, and
vanadium are potential risks in the environment even at low concentrations (Paul et
al., 2006; Ilander and Vaisanen, 2009; Mezhibor et al., 2009).
In the last few decades, ICP-OES and ICP-MS have popularly been applied to
analyze a wide range of samples including coal and coal ash by virtue of their
capability of simultaneous analysis of multi-elements with excellent reliability and
sensitivity. (Wang et al., 2004). The main advantages of inductively coupled plasma
optical emission spectrometry (ICP-OES) over atomic absorption techniques are
multi-element determination and high sample through-put with detection limits low
enough for most of the analyte elements in fly ash samples (Ilander and Vaisanen,
2009). Metals have strategic and industrial importance due to its applications in many
ENERGY EXPLORATION & EXPLOITATION · Volume 28 · Number 2 · 2010 111

technological fields. A certified reference material of coal, NIST-1632c, was digested

by MW-AD followed by the ICP-OES measurement. The results are presented in
Table 4 together with the certified or reference values.
The limits of quantification (LOQ) of the ICP-OES instruments are calculated as
the concentration equal to 10 times the standard deviation of the background signal
(the signal of the blank solution), multiplied by the dilution factor. The LOQs
represent the lowest concentrations of trace elements in coal (µg/g) that can be
quantified with the referred instruments (Wang et al., 2004). It has become evidence
that complete dissolution of metals in CBA and accurate results in subsequent analysis
can be obtained by means of applying pressurized digestion under microwave heating.
A combination of HNO3 and HF is conventionally employed in the MW-AD of coal
because coal contains an appreciable amount of inorganic matters, which mainly
consist of aluminosilicate matrix (Iwashita et al., 2006). The combination of HNO3
(conc.) and HF (conc.) in the volume ratio of 7:2 attacked the sample well enough, and
good recoveries for all the metals studied were obtained.
The sample preparation method developed in this study for element determination
in coal by spectroanalytical technique is dry ashing, and wet acid microwave
digestion. The particle sizes of the samples were below than 250 µm. The burning
temperature of 650˚C was found to be the best as a result of the trade-off between the
overall metal recovery yield. The inductively coupled plasma-optical emission
spectrometry (ICP-OES) functions best when the samples are in aqueous or solution
phase. Coal samples were prepared for the analysis of element to be collected in an
aqueous phase (Hardaway and Sneddon 2004). Generally, coal contain a greater
concentration of heteroatoms and metals than the crude oil and are an extremely
abundant source of trace-metal compounds (Saydut et al., 2007; 2008). A number of
the heavy metals such as nickel, copper, and iron can be effectively bound in large
organic molecules characteristic of those found in the coal. It is necessary to use an
appropriate sample preparation in order to avoid measurement errors. The selected
sample preparation procedure involves the task to obtain the best results in the shortest
time, with minimum contamination, using the smallest quantities of reagents and
samples, and having little residue and waste generation. In addition it is of importance
to maintain the integrity of the sample and the traceability of the results, to have
quality and confidence in the measurements (Amorim et al., 2007).
Inductively coupled plasma optical emission spectrometry ICP-OES has been used
for the determination of elements in CBA. Instrumental parameters are listed in Table
3. The inductively coupled plasma-optical emission spectrometry (ICP-OES)
functions best when the samples are in aqueous or solution phase. Analytical
wavelengths, detection limits and average concentration of elements of CBA are
shown in Table 5. ICP-OES offers a wider linear dynamic range and has multielement
detection capability. The method was validated through the analysis of an SRM with
good recoveries (Table 4). Dry ash and microwave acid digestion method had clear
advantages in terms of simplicity of sample preparation, overall analysis time, and the
use of inorganic standards for calibration instead of expensive metalorganic standards.
The samples digested with HNO3 alone were not analysed for Zn. In order to obtain
a recovery close to 100% for all the metals studied, the use of HF was necessary. This
112 Microwave Acid Digestion for the Determination of Metals
in Subbitumnious Coal Bottom Ash by ICP-OES

indicated that part of the metals in the reference materials are bound to silicate-based
compounds. However, very small volumes of HF seemed to be sufficient. The
combination of HNO3 and HF in the volume ratio of 7:2 attacked the sample well
enough, and highly satisfactory recoveries for all the metals, including Zn, were
obtained. (Ikavalko et al., 1999) The inductively coupled plasma-optical emission
spectrometry (ICP-OES) functions best when the samples are in aqueous or solution
phase.

4. CONCLUSIONS
Sample preparation method was developed for element determination in coal by
spectroanalytical techniques, dry ashing (at 650°C) and wet acid digestion
(HF+HNO3+H3BO3). For the determination of various elements in CBA, MW-AD
followed by ICP-OES was carried out. The results are in good agreement with the
reference values.

REFERENCES
Akba O., Baysal A., Merdivan M., Hamamci C. and Gumgum.B., 2005. Matrix effects
of concomitant species on the determination of nickel by inductively coupled
plasma atomic emission spectrometry. Asian Journal of Chemistry 17(3), 1518-
1526.
Amorim F.A.C., Welz B., Costa A.C.S., Lepri F.G., Goreti M., Vale R. and Ferreira
S.L.C., 2007. Determination of vanadium in petroleum and petroleum products
using atomic spectrometric techniques. Talanta 72, 349-359.
Aydin I., Aydin F., Saydut A. and Hamamci C., 2009a. A sequential extraction to
determine the distribution of phosphorus in the seawater and marine surface
sediment. Journal of Hazardous Materials 168, 664-669.
Aydin I., Imamoglu S., Aydin F., Saydut A. and Hamamci C., 2009b. Determination
of mineral phosphate species in sedimentary phosphate rock in Mardin, Turkey
by sequential extraction. Microchemical Journal 91(1), 63-69.
Ayhan F.D., Abakay H. and Saydut A., 2005. Desulfurization and deashing of Hazro
coal via a flotation method. Energy & Fuels 19, 1003-1007.
Baysal A., Akba O., Merdivan M., Hamamci C. and Gumgum B., 2002. Comparison
of microwave digestion procedures for the determination of some elements in
asphaltite ash using ICP-AES. Annali Di Chimica 92, 1127-1133.
Bingol D. and Akcay M., 2005. Determination of trace elements in fly ash samples by
FAAS after applying different digestion procedure. Talanta 66, 600-604.
Dai S.F., Sun Y.Z. and Zeng R.S., 2006. Enrichment of arsenic, antimony, mercury,
and thallium in a Late Permian anthracite from Xingren, Guizhou, Southwest
China. International Journal of Coal Geology 66, 217-226.
Davydova S., 2005. Heavy metals as toxicants in big cities. Microchemical Journal
79, 133-136.
Duz M.Z., Saydut A., Erdogan S. and Hamamci C., 2009. Removal of sulfur and ash
from coal using molten caustic leaching, a case study from Hazro fields, Turkey.
Energy Exploration & Exploitation 27(6), 391-400.
ENERGY EXPLORATION & EXPLOITATION · Volume 28 · Number 2 · 2010 113

Duz M.Z., Tonbul Y., Baysal A., Akba O., Saydut A. and Hamamci C., 2005.
Pyrolysis kinetics and chemical composition of Hazro coal according to the
particle size. Journal of Thermal Analysis and Calorimetry 81, 395-398.
Erdogan S., Baysal A., Akba O. and Hamamci C., 2007. Interaction of metals with
humic acid isolated from oxidized coal. Polish Journal of Environmental Studies
16(5), 671-675.
Erdogan S., Baysal A., Akba O., Merdivan M. and Hamamci C., 2007. Relationship
between wintertime atmospheric particulate matter and meteorological
conditions in Diyarbakir (Turkey). Asian Journal of Chemistry 19(3), 1703-
1708.
Erdogan S., Duz M.Z., Merdivan M. and Hamamcı C., 2005. Formation and
characterization of humic acids from low rank Anatolian coals by air oxidation.
Energy Sources 27(5), 423-430.
Erdogan S., Merdivan M., Hamamcı C., Akba O. and Baysal A., 2004. Polymer
supported humic acid for separation and preconcentration of thorium(IV).
Analytical Letters 37(12), 2565-2575.
Felipe-Sotelo M., Carlosena A., Andrade J.M., Cal-Prieto M.J., Fernandez E. and
Prada D., 2005. Slurry-based procedures to determine chromium, nickel and
vanadium in complex matrices by ETAAS. Microchemical Journal 81, 217-224.
Goodarzi F., 2002. Mineralogy, elemental composition and modes of occurrence of
elements in Canadian feed-coals. Fuel 81, 1199-1213.
Gumgum B. and Hamamci C. 1991. Determination of some rare elements in
phosphate rocks by ICP-AES. Spectroscopy Letters 24(9), 1229-1236.
Hamamci C., Duz M.Z., Saydut A. and Merdivan M., 2003. Elemental composition of
Southeastern Anatolia asphaltites (Turkey) as a function of particle size. Oil
Shale 20, 161-166.
Hardaway C. and Sneddon J., 2004. Determination of metals in crude oil by atomic
spectrometry-a review. Analytical Letters 37, 2881-2899.
Hatanpaa E., Kajander K., Laitinen T., Piepponen S. and Revitzer H., 1997. A study
of trace element behavior in two modern coal-fired power plants I. Development
and optimization of trace element analysis using reference materials. Fuel
Processing Technology 51, 205-217.
Ikavalko E., Laitinen T. and Tzer H., 1999. Optimised method of coal digestion for
trace metal determination by atomic absorption spectroscopy. Fresenius’
Journal of Analytical Chemistry 363, 314-316.
Ilander A. and Vaisanen A., 2009. The determination of trace element concentrations
in fly ash samples using ultrasound-assisted digestion followed with inductively
coupled plasma optical emission spectrometry. Ultrasonics Sonochemistry 16,
763-768.
Isık B., Hamamci C. and Isık R., 2006. Effect of winter air pollution on lipid
peroxidation product levels of patients with chronic obstructive pulmonary
disease. Asian Journal of Chemistry 18(2), 1433-1436.
114 Microwave Acid Digestion for the Determination of Metals
in Subbitumnious Coal Bottom Ash by ICP-OES

Iwashita A., Nakajima T., Takanashi H., Ohki A., Fujita Y. and Yamashita T., 2007.
Determination of trace elements in coal and coal fly ash by joint-use of ICP-AES
and atomic absorption spectrometry. Talanta 71, 251-257.
Iwashita A., Nakajima T., Takanashi H., Ohki A., Fujita Y. and Yamashita T., 2006.
Effect of pretreatment conditions on the determination of major and trace
elements in coal fly ash using ICP-AES. Fuel 85, 257-263.
Laban K.L. and Atkin B.P., 1999. The determination of minor and trace element
associations in coal using a sequential microwave digestion procedure.
International Journal of Coal Geology 41, 351-369.
Mezhibor A.M., Arbuzov S.I. and Rikhvanov L.P., 2009. Accumulation and average
contents of trace elements in the high-moor peat of Tomsk region (Western
Siberia, Russia). Energy Exploration & Exploitation 27(6), 401-410.
Ozturk G., Kafadar A.B., Duz M.Z., Saydut A. and Hamamci C., 2010. Microwave
assisted transesterification of maize (Zea mays L.) oil as a biodiesel fuel. Energy
Exploration & Exploitation 28(1), 47-57.
Paul M., Seferinoglu M., Aycik G.A., Sandstrom A, Smith M.L. and Paul J., 2006.
Acid leaching of ash and coal: Time dependence and trace element occurrences.
International Journal of Mineral Processing 79(1), 27-41.
Rodushkin I., Axelsson M.D. and Burman E., 2000. Multielement analysis of coal by
ICP techniques using solution nebulization and laser ablation. Talanta 51, 743-
759.
Sandroni V., Smith C.M.M. and Donovan A., 2003. Microwave digestion of sediment,
soils and urban particulate matter for trace metal analysis. Talanta 60, 715-723.
Saydut A., Duz M.Z., Aydin I. and Hamamci C., 2008. Desulfurization and
demineralization of asphaltite using combination of froth flotation and aqueous
caustic leaching. Energy Exploration & Exploitation 26, 133-142.
Saydut A., Tonbul, Y., Baysal A., Duz M.Z. and Hamamci C., 2007. Froth flotation
pretreatment for enhancing desulfurization of coal with sodium hydroxide.
Journal of Scientific & Industrial Research 66(1), 72-74.
Sneddon J., Hardaway C., Bobbadi K. and Reddy A. 2006. Sample preparation of
solid samples for metal determination by atomic spectroscopy-An overview and
selected recent applications. Applied Spectroscopy Reviews 41(1), 1-14.
Tang Y.G., Chang C.X., Zhang Y.Z. and Li W.W., 2009. Migration and distribution
of fifteen toxic trace elements during the coal washing of the Kailuan Coalfield,
Hebei Province, China. Energy Exploration & Exploitation 27(2), 143-152.
Tsai S.L. and Tsai M., 1998. A study of the extraction of vanadium and nickel in oil-
fired fly ash. Resources, Conservation and Recycling 22, 163-176.
Wang A.J., Nakazato T., Sakanishi K., Yamadaa O., Tao H. and Saito I., 2004.
Microwave digestion with HNO3/H2O2 mixture at high temperatures for
determination of trace elements in coal by ICP-OES and ICP-MS. Analytica
Chimica Acta 514, 115-124.
ENERGY EXPLORATION & EXPLOITATION · Volume 28 · Number 2 · 2010 115

Wang J., Nakazato T., Sakanishi K., Yamada O., Tao H. and Saito I., 2006. Single-
step microwave digestion with HNO3 alone for determination of trace elements
in coal by ICP spectrometry. Talanta 68, 1584-1590.
Xu. A., Iwashita A., Nakajima T., Yamashita H., Takanashi H. and Ohki A., 2005.
Effect of HF addition on the microwave-assisted acid-digestion for the
determination of metals in coal by inductively coupled plasma-atomic emission
spectrometry. Talanta 66, 58-64.
Zhao C.L. and Sun Y.Z., 2008. Rare earth elements of Coal Seam 5 from Gequan
Mine, Xingtai Coalfield. World Journal of Engineering 5(1), 90-94.
Zhao C.L., Qin S.J., Yang Y.C., Li Y.H. and Lin M.Y., 2009. Concentration of
Gallium in the Permo-Carboniferous Coals of China. Energy Exploration &
Exploitation 27(5), 333-343.