Journal of Environmental Protection, 2011, 2, 489-501
doi:10.4236/jep.2011.25057 Published Online July 2011 (http://www.scirp.org/journal/jep)
Behavior of Cu, Pb, and Zn in Ash during the
Endothermic Burning of Mixed Industrial Wastes
Masafumi Tateda1, Seisou Suzuki1, Youngchul Kim2, Bandunee Champika Liyanage Athapattu3
1Department of Environmental Engineering, Toyama Prefectural University, Imizu, Japan; 2Department of Environmental Engineer-
ing, Hanseo University, Seosan-si, Korea; 3Department of Civil Engineering, The Open University of Sri Lanka, Nawala, Sri Lanka.
Received February 22nd, 2011; revised April 5th, 2011; accepted May 19th, 2011.
ABSTRACT
The behaviors of Cu, Pb, and Zn during the endothermic burning of heterogeneous wastes were investigated using a
variety of operational parameters, i.e., the mixed waste ra tio, burning temperature, and burning time , to obtain funda-
mental knowledge to generate an optimal burning operation and recycling strategy for bottom ash. Changing these
parameters had no impact on the Cu content of the ash, whereas the Pb content depended on the burning temperature
and the mixed ratio, and the Zn conten t was affected by all three parameters. It was found in this study that the optimal
burning conditions were a temperature of 1100˚C, a time of 15 minutes, and either the current waste conditions or
waste conditions with doub le the waste plastic and wood content.
Keywords: Heavy Metals, Endothermic Burning, Portioning Behavior, Industrial Waste, Ash
1. Introduction and Methods
Japan has two categories of waste: general waste mainly
from residential areas, and industrial waste. Industrial
waste accounts for almost 90% of the waste generated,
reaching about 400 million tons annually. For treatment
of both types of waste, Japan primarily uses incineration.
In fact, over 80% of the generated general waste, ap-
proximately 40 million tons annually, is incinerated. A
variety of metal elements are present in the resultant in-
cineration ashes, especially in the fly ash or fly and bot-
tom mixed ash; therefore, intermediate treatment meth-
ods to reduce their environmental impact are nationally
designated. The disposal of ashes treated by either solidi-
fication in cement or melting fu sion into landfills and the
recycling of those ashes as commercial materials have a
serious impact on health and economics due to the spread
of toxic materials (i.e., heavy metals) into the environ-
ment and the waste of non-recycled metal resources [1,2].
Burning is also one of the nation ally designated interme-
diate treatment options for ash recycling (Figure 1). This
method is commonly used by private companies that
generate a large amount of ash to avoid cost-prohibitive
ash disposal in landfill sites. Since ash burning is an en-
dothermic process, fuel is necessary to generate the heat
required. Normally a synthesized fuel or refused paper &
plastic fuel (RPF) is used instead of kerosene to reduce
the operating costs.
Alternatively, the ash is burned with other combustible
waste such as plastic and wood, which results in the
mixed burning of ash, plastics, and paper or wood. As
mentioned earlier, ash contains metal elements and the
effect of heterogeneous burning conditions on the be-
havior of those metal elements has not yet been investi-
gated. The purpose of this study is to investigate the be-
haviors of Cu, Pb, and Zn, as representative elements
with negative health and environmental impacts, under
heterogeneous waste burning with varying burning tem-
perature, burning time, and mixed waste ratio. Under-
standing the behaviors of metals in heterogeneous condi-
tions is essential in order to determine the appropriate
conditions for b urning operations and to op timize a recy-
cling strategy for the bottom ash from endothermic
burning.
2. Materials and Methods
2.1. Waste Samples
The following six samples were used as samples for
burning: automobile shredder residue (ASR) fly and bot-
tom ashes, fly and bottom ashes from the incineration of
waste plastics and woods, waste plastic residue from RPF

Behavior of Cu, Pb, and Zn in Ash during the Endothermic Burning of Mixed Industrial Wastes 490
Figure 1. Designated intermediate treatment methods for
fly ash or fly and bottom ash, as determined by the central
Japanese government.
production, and the benthic sludge of rivers. The ASR fly
and bottom ashes were obtained from the incineration of
ASR by a rotary kiln.
2.2. Methods for the Analysis of the Total
Content of Elements in the Waste Samples
The conditions of the boiling extraction method for ele-
ment extraction [3], which is the standard Japanese me-
thod, were examined to d etermine the optimal conditio ns
for element extraction from the ash samples after incin-
eration of the mixed waste. The selected conditions are
shown in Table 1.
An inductively coupled plasma–mass spectrometer
(ICP-MS) was used for elemental analysis, and hydro-
chloric acid (conc. 35% - 37%, Kanto Kagaku), nitric
acid (60% - 61%, Kanto Kagaku) and deionized water
were used as solvents. The standard method for boiling
extraction was as follows: The ash sample (1 ± 0.01 g,
wet base) was placed in a beaker and mixed with hydro-
chloric acid (1:4 HCl:H2O) and nitric acid (1 + 1
HNO3:H2O) and boiled for 30 minutes. After cooling, the
solution was transferred to a 100 mL volumetric flask,
which was accurately filled with deionized water. Next,
the solution was filtered using a 1 µm cellulose acetate
filter (Advantec). A 10 mL aliquot was diluted to 50 mL
in a volumetric flask using deionized water. The solu tion
was then analyzed by ICP-MS (HP4500, Yokokawa).
2.3. Quantitative Analysis of Cu, Pb, and Zn
Content
Cu, Pb, and Zn heavy metals, which are present in rela-
tively high concentrations and cause considerable harm
to the environment and human health, were selected for
analysis using an atomic absorption spectrophotometer
(AAS; A-2000, Hitachi). The samples were pre-treated
Table 1. Pretreatment condition.
Altered conditions Details
Standard (SD) Boiling extraction using nitric a ci d
and hydrochlor i c acid
Altered condition 1 (AC1)Double concentration of hydrochlor ic
acid of SD
Altered condition 2 (AC2)Double concentration of nitric ac id o f
SD
Altered condition 3 (AC3)Double concentrations of
hydrochloric and nitric aci ds of SD
Altered condition 4 (AC4)Double boiling time of SD
Altered condition 5 (AC5)Double boiling time and concentration of
hydrochloric acid of SD
with AC1, which uses double the concentration of hy-
drochloric acid as compared to the standard (see Table 1).
For degradation of the waste samples, two methods were
tested: degradation at 600˚C combustion or drying at
105˚C. For the first method, the waste samples were
burned at 600˚C for 60 minutes and the ash was collected
for total content analysis for the metals. For the second
method, the sample was prepared by drying it at 105˚C
without burning and then analyzed for the total content of
the metals. The ash or dry samples (2 - 5 g) were trans-
ferred into a flask and hydrochloric (60 mL) and nitric
(30 mL) acids were added, and the solution was heated
until it reduced to about 5 mL. After cooling, 20 mL of
hydrochloric acid (1 + 5 HCl:H2O) was added to the so-
lution, which was further heated for 5 - 6 minutes. After
cooling again, the solution was diluted to 100 mL in a
volumetric flask using deionized water. The diluted solu-
tion was filtered through a 1 µm glass fiber filter and the
filtrate was analyzed using an AAS.
2.4. Quantitative Analysis of Cu, Pb, and Zn in
Ash
The content of heavy metals, i.e., Cu, Pb, and Zn, in
ashes burned under d ifferent conditions was analyzed v ia
the following procedure. The AC1 pretreatment, which
uses a double concentration of hydrochloric acid as
compared to the standard, was used. The parameters that
were investigated in this study w ere waste sample mixed
ratio, burning temperature, and burning time. Different
waste samples types were prepared with varying mixed
ratios, as summarized in Table 2. Burning temperatures
were either 900˚C, 1000˚C, or 1 100˚C and burning times
were either 15, 30, or 60 minutes in an electric furnace
(KDF S80, Eyela). All possible combinations of parame-
ters were performed and the sample descriptions are
shown in Table 3.
Ash samples (2 - 5 g) were transferred into a flask,
hydrochloric (60 mL) and nitric (30 mL) acids were added,
and the solution was h eated until it was reduced to about
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Behavior of Cu, Pb, and Zn in Ash during the Endothermic Burning of Mixed Industrial Wastes491
Table 2. Mixed status of burning samples for designing the
experimental preparation (%).
Type AType B Type C
Sample type Current
condition
of waste
Double of
ASR
content
Double of waste
plastic & wood
content
bottom ash (BA) 11.22 22.44 11.22
ASR fly ash (FA) 6.12 12.24 6.12
bottom ash (BA) 2.04 2.04 4.08
Waste
plastic &
wood fly ash (FA) 1.02 1.02 2.04
Waste plastic residue from
RPF production (RPF-R) 67.34 50.02 64.36
Benthic sludge of rivers
(BSR) 12.24 12.24 12.24
Table 3. Combination of experimental conditions and sam-
ple IDs.
Burning
temperature (˚C) Burning time (minutes) Sample type in Table 2 Sample ID
A 915A
B 915B 15
C 915C
A 930A
B 930B
30
C 930C
A 960A
B 960B
900
60
C 960C
A 1015A
B 1015B
15
C 1015C
A 1030A
B 1030B
30
C 1030C
A 1060A
B 1060B
1000
60
C 1060C
A 1115A
B 1115B 15
C 1115C
A 1130A
B 1130B
30
C 1130C
A 1160A
B 1160B
1100
60
C 1160C
5 mL. After cooling, 20 mL of hydrochloric acid (1 + 5
HCl:H2O) was added to the solution, which was further
heated for 5 - 6 minutes. After cooling again, the solution
was diluted to 100 mL using deionized water in a volu-
metric flask. The diluted solutio n was filtered through a 1
µm glass fiber filter and the filtrate was analyzed using
an AAS (A-2000, Hitachi).
3. Results
3.1. Effect of the Chemical Pretreatment on the
Content Analysis
Figures 2(a)-(f) show the efficacy of each of the pre-
treatment methods and the amount of each selected ele-
ment. The heavy metals were almost undetectable in the
samples of waste plastic residue from RPF production
(RPF-R) and the benthic river sludge (BSR) using SD
and AC3 methods. The AC1 method resulted in the most
balanced detection of the Cu, Zn and Pb metals and other
elements, and is therefore considered to be the optimal
pretreatment method for analyzing heavy metals con-
tained in these samples. The amount of Cu, Zn, and Pb in
each sample after pretreatment using the AC1 method is
shown in Figure 3. The ASR bottom ash sample (ASR-
BA) contained the largest amount of Cu, Zn, and Pb.
3.2. Effect of Sample Preparation on the Cu, Pb,
and Zn Content
To optimize the detection of the selected heavy metals in
the samples, two methods of preparing the samples, i.e.,
burning at 600˚C or drying at 105˚C, were investigated.
Regardless of the waste sample types and the species of
heavy metal, the metal content of the burned samples
was always larger than that of the dried samples (Figures
4(a)-(i)). Therefore, it is evident that bu rning the samples
at 600˚C is a better method for degrading the waste sam-
ples for optimal detection of the heavy metals. The rea-
son for the lower detection of the metals in the dried
samples might be the remnant presence of organic mate-
rials. The initial reaction of the organic materials with
hydrochloric acid and altering the pH and oxidation-re-
duction potential (ORP) did not alter the environment
around the heavy metals enough to accelerate the metal
extraction from the samples.
3.3. Effect of Varying the Burning Conditions on
the Cu, Pb, and Zn Content
Figures 5(a)-(c), 6(a)-(c) and 7(a)-(c) show the behav-
iors of Zn, Pb and Cu, respectively, under different burn-
ing conditions, where Figures 5-7(a), Figures 5-7(b),
and Figures 5-7(c) display the effects of varying the tem-
perature, burning time and sample type, respectively.
4. Discussion
4.1. Optimal Chemical Pretreatment
The metal content of the samples were assessed employ-
ing the 6 different pretreatment methods described in
Table 1 and Figure 2. High amounts of all metals were
detected using both the AC1 and AC4 pretreatment me-
thods, although the metal levels detected after the AC4

Behavior of Cu, Pb, and Zn in Ash during the Endothermic Burning of Mixed Industrial Wastes 492
pretreatment were higher. However, to maximize time
efficiency, AC1 was used as the pretreatment for the fur-
ther analyses, as the boiling time was 30 and 60 minutes
for AC1 and AC4, respectively. Using the SD method,
the elements shown in Figure 2 could not be detected in
the WPW-FA, RPF-R, and BSR waste samples. These
results indicate that SD, which is especially useful for
heavy metal analysis in sewage sludge, was not suitable
for the waste samples focused on here. Since an accurate
measurement of the total heavy metal content in solid
samples is almost impossible using the acid solution ex-
traction method with ICP, it is more accurate to refer to
the results as the “maximum extracted element content”
instead of the “total content of heavy metals.” Al, Ca,
and Fe were detected in high levels in all of the waste
samples. The amount of the Zn, Pb and Cu detected in
each sample in Figure 3 was shown in Figure 4(a), Fig-
ure 4(d), and Figure 4(g), respectively, and was signifi-
cantly dependen t on the heat treatment. Therefore, it was
concluded that heat treatment is extremely important for
analyzing the elemental content of waste samples.
4.2. Optimal Thermal Pretreatment
Figures 4(a)-(i) show the results of the thermal destruc-
tion portion of the pretreatment. For all cases, the total
metal content was higher in the samples treated at 600˚C

Behavior of Cu, Pb, and Zn in Ash during the Endothermic Burning of Mixed Industrial Wastes493
Figure 2. Element contents in samples treated by (a) Standard method, (b) Double concentration of HCl (Altered condition 1),
(c) Double concentration of NH3 (Altered condition 2), (d) Double concentrations of HCl and NH3 (Altered condition 3), (e)
Double boiling time (Altered condition 4), and (f) Double boiling time and concentration of HCl (Altered condition 5).
Figure 3. Cu, Zn, and Pb contents in samples pretreated by Double concentration of HCl (Altered condition 1).

Behavior of Cu, Pb, and Zn in Ash during the Endothermic Burning of Mixed Industrial Wastes 494
Figure 4. Comparison of pretreatment (thermal treatment) on element content: (a)-(c):Type A-C on Zn, (d)-(f):Type A-C on
Pb, and (g)-(i):Type A-C on Cu.
than those that were dried at 105˚C. As it was established
that thermal pretreatment at 600˚C is better than at 105˚C,
the effect of thermal pretreatment at 900˚C, 1000˚C, and
1100˚C was also investigated. Since the time of burning
or drying was one hour for the results in Figure 4, a
comparison of Figure 4 and 960A–C, 1060A–C, and
1100A–C for the detection of Cu, Pb, and Zn (Figures 5-
7) was carried out. The amounts of the elements detected
after the 600˚C thermal pretreatment was highest in almost
all cases (Figures 8-10). There was the only one exception:
the amount of Pb detected after 960B pretreatment was
higher than that after 600˚C thermal pretreatment. There-
fore, it can be concluded that the 600˚C thermal pretreat-
ment was the best overall method to obtain the maximum
extraction content of elements from waste samples.
4.3. Behaviors of Cu, Pb, and Zn in Ash
Figures 5-7 show the behaviors of Zn, Pb, and Cu, re-
spectively, under different operating conditions; the re-
sults are summarized in Table 4.
The speciation of Cu, Pb, and Zn during municipal
solid waste combustion was described as follows [4,5]:
Cu, CuCl, CuH, CuO, CuS, Cu2, (CuCl)3, CuCl, CuO,
CuO-Al2O3, CuO-Fe2O3, CuS-FeS, CuSO4, Cu2O-Al2O3,
Cu2-Fe2O3, Cu2S, Cu5FeS4, Pb, PbCl, PbCl2, PbO, PbS,
Pb2, PbCl2, PbO-SiO2, 2Pb-SiO2, PbS, PbSO4, Pb2B2O4,
Pb3O4, Zn, ZnCl2 ZnS, ZnO, ZnO-SO2, ZnS, ZnSO4,
2ZnO-SiO2, Zn2SiO4, ZnFe2O4, ZnCr2O4, ZnAl2O4, and
ZnO-2ZnSO4. The metallic states (i.e., Zn, Pb, and Cu),
mono-oxidized species (i.e., ZnO, PbO, and CuO), and
chlorinated species (i.e., ZnCl2, PbCl2, and CuCl2) were
chosen as the representative compounds in this study;
their melting and boilin g points are listed in Figure 11.
According to Verhulst et al. [6], ZnCl2 (solid (s)) con-
verts to ZnO(s) at less than 300˚C and forms ZnCl2

Behavior of Cu, Pb, and Zn in Ash during the Endothermic Burning of Mixed Industrial Wastes495
Figure 5. The behavior of Zn depending on the (a) burning temperature, (b) burning time, and (c) sample types.

Behavior of Cu, Pb, and Zn in Ash during the Endothermic Burning of Mixed Industrial Wastes 496
Figure 6. The behavior of Pb depending on the (a) burning temperature, (b) burning time, and (c) sample types.
C opyright © 2011 SciRes. JEP

Behavior of Cu, Pb, and Zn in Ash during the Endothermic Burning of Mixed Industrial Wastes497
Figure 7. The behavior of Cu depending on the (a) bur ning temperature, (b) burning time, and (c) sample types.

Behavior of Cu, Pb, and Zn in Ash during the Endothermic Burning of Mixed Industrial Wastes 498
Figure 8. Content of Zn detected after burning at different
temperatures.
Figure 10. The content of Pb detected after burning at dif-
ferent temperatu re s .
Table 4. Summary of Zn, Pb, and Cu behaviors.
Influence byZn Pb Cu
Burning
temperature
Its detection became
small as temperature
goes up.
High detection
at 900˚C No significan t difference
Burning time
-No difference at 900˚C
-Its detection became
smaller as time
becomes longer.
-No significant
difference No significan t difference
Mixed ratio
-Mixed ratio B always
shows the highest.
-No significant
difference between
mixed ratios A and C .
Mixed ratio B
seemed high No significant difference
(gas (g)), whereas PbCl2(g) starts to volatilize around
300˚C and PbO(g) and PbCl(g) are predominant above
800˚C. In the case of Cu, CuCl2 is converted to CuO
around 700˚C and CuCl(g) is predominant around 900˚C
after Cu3Cl3(g) is formed. Generally, the presence of Cl
greatly influences the behavior of metals; the volatility of
heavy metals increases when they are chlorinated due to
their decreased boiling point.
Figure 9. The content of Cu detected after burning at dif-
ferent temperatu re s .

Behavior of Cu, Pb, and Zn in Ash during the Endothermic Burning of Mixed Industrial Wastes499
Figure 11. Melting and boiling properties of (a) metal, (b)
metal oxide, and (c) metal chloride species. The broken line
indicates 1100ºC, which was the highest burning tempera-
ture in this study. The temperature of ZnO is the sublima-
tion point.
The effect of Cl on heavy metals was discussed by
many researchers [7-10]. According to most studies, Cl
exerts a stronger influence on Zn than on Cu or Pb;
however, Pb was the most volatile chloride according to
a study by Trouvé et al. (1998). Also, Pb and Zn were
more likely than Cu to be transferred into th e combustio n
gas by forming compounds with chlorine [11]. All re-
ports agreed that chlorinated Cu was the most stable. In
the current study, the chlorine co ncentrations in the sam-
ples were not analyzed because, in reality, the chlorine
concentration in waste cannot be controlled. In addition
to the chlorine content, the combustion temperature also
greatly influences metal partitioning and speciation [12].
Heavy metal partitioning behaviors are also greatly af-
fected by the presence of alkaline metals such as Na and
K and moisture in the waste [13]. According to Wang et
al. (1999), the presence of Na and K increased the parti-
tioning of heavy metals into fly ash. All of the analyzed
samples contained Na and K (Figure 2), but the behavior
of Cu was not influenced by the changes in the mixed
ratio. In opposition to the trend reported by Wang et al.
(1999), Pb and Zn showed the highest con tents in the ash
under the mixed ratio B, which had the highest Na and K
concentration. Therefor e, it can be said that the influence
of Na and K was not supported by this study.
The behavior of Cu behavior has also been shown to
be affect by the presence of Ca; the detection level of Cu
in the gas phase drastically increased in the presence of
limestone with a Ca/S ratio of 1.3 [14]. However, the
increase in the detection level disappeared when the ratio
doubled to 2.5. From Figure 2, it is evident that the
ASR-FA, WPW-BA, and WPW-FA samples contain a
relatively large amount of Ca, which could influence Cu
detection in the ash analysis. It has also been reported
that the presence of organic chloride species decreases
the capture of Cu by limestone, while the presence of
inorganic chlorides increases it [15]. The influence of Ca
on Cu was not directly tested in this experiment. How-
ever, according to Table 2, there was no evident impact
of Ca on Cu as the Cu detection levels did not differ sig-
nificantly upon changes in the mixed ratio (Table 4) al-
though Type C did contain double the amount of WPW-
BA and WPW-FA, which contained a large amount of
Ca (Figure 2). From the results shown in Table 4, it was
determined that Cu was the most stable among the three
metals as it demonstrated no significant difference in the
Cu levels upon changing the burning temperature, burn-
ing time, and waste mixed ratio, which is in agreement
with the results of Williams [16] and Trouvé et al. (1998).
Zn, on the other hand, was the most unstable metal
among the three: the content of Zn in the ash decreased
with increasing temperature and was also influenced by
the burning time at 1000˚C and 1100˚C. Changes to the
mixed ratio resulted in a higher Zn content in the ash
from sample type B. In contrast, the amount of Pb de-
tected was not influenced by th e burning time (Table 4).
Weight percentages of 89% - 96% of Cu, 58% - 94% of
Pb, and 37% - 86% of Zn remained in the bottom ash [4].
These ranges are consistent with the results of this study.
4.4. Comparison to Environmental Criteria
After burning, ash either goes to a lan dfill site or to recy-
cling after clearing the criteria for the heavy metal ex-
traction test; lower heavy metal conten t in the ash is bet-
ter for both purposes. According to the results, the sam-
ples with the lowest conten t of heavy metals were 1115A
and 1115C. The content of Zn, Pb, and Cu was 3,384 ±
434 mg/kg, 4,013 ± 2228 mg/kg, and 23,570 ± 8,210
mg/kg, respectively, for 1115A, and 5219 ± 58 mg/kg,
4455 ± 414 mg/kg , and 18,271 ± 434 mg/k g, respectiv ely,
for 1115C. The heavy metal content in samples 1115A
and 1115C were compared to standards related to envi-
ronmental issues such as landfill, sea dumping, and com-
posting (Table 5). The experimental values were 7.5
to11.6, 261 to 337, and 803 to 891 times larger than the

Behavior of Cu, Pb, and Zn in Ash during the Endothermic Burning of Mixed Industrial Wastes 500
Table 5. Environmental values.
Heavy
metals Landfill standard (Japan) Sea dumping (Japan) Soil (Japan) Compost standard (mg/kg) This study (Mean) (mg/kg)
(mg/l) (mg/kg) (mg/kg) JapanIndia†USEPA†Canada†Germany† 1115A 1115C
Zn - 450 - - 1000 2800 500 400 3,3845,219
Cu - 70 125 - 300 1500 60 100 23,57018,271
Pb 0.3 5 0.01* - 100 300 150 150 4,0134,455
note†:Reference [17].
sea dumping standards for Zn, Cu, and Pb, respectively.
When compared with the United States Environmental
Protection Agency (USEPA) compost standards, which
are relatively high, the experimental values were ap-
proximately 1.2 to 1.9, 12 to 16, and 13 to 15 times
higher for Zn, Cu, and Pb, respectively. Therefore, al-
though the content of heavy metals in ash is greatly re-
duced by tuning the burning temperature and time for Zn
and Pb, it is still far higher than that allowed by any of
the standards described here.
5. Conclusions
The behaviors of Cu, Pb, and Zn under the endothermic
burning of heterogeneous wastes were investigated by
changing the operational parameters, i.e., the mixed
waste ratio, burning temperature, and burning time, to
obtain fundamental knowledge to generate an approp riate
burning operation and recycling strategy for bottom ash.
Changing these parameters yielded no significant effect
on the Cu content of the ash, whereas the Pb content was
influenced by the burning temperature and mixed ratio,
and the Zn content was influence by all three parameters.
The burning conditions not only influence the partition-
ing behavior of metals in thermal treatment reactors, such
as incinerators, but also the characteristics of the metals
in the ash. Therefore, it is important to understand these
effects to plan an effective recycling strategy for incin-
eration ash. In this study, the optimal operation condi-
tions were 1115A and 1115C, which correspond to a
burning temperature of 1100˚C, a burning time of 15
minutes, and either the current waste conditions or the
waste condition with double the waste plastic & wood
content. It is also important that managers in charge of
thermal treatment reactors conduct their own investiga-
tion into the partitioning behavior of heavy metals at
their plants based on the academic results that have been
reported in order to optimize the operations for their re-
actors.
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