Separation and Purification Technology 57 (2007) 513–518

Completely treating heavy metal laboratory waste

liquid by an improved ferrite process
Jie-Chung Lou ∗ , Chien-Kuei Chang
Institute of Environmental Engineering, National Sun Yat-Sen University, Kaohsiung,
Len-Hai Road No. 70, Kaohsiung 80424, Taiwan

Abstract
This work proposes a scheme for completely treating heavy metal laboratory waste liquid. Ten common heavy metals and various anions were
adopted to synthesize the simulated laboratory waste liquid. Experimental results demonstrated that although conventional ferrite process (FP)
could not be used to treat the simulated waste liquid completely, the enhanced FP, i.e., the extended reaction ferrite process (ERFP), could be used
to satisfy regulatory limits. FeSO4 can be added in the extended stage of ERFP intermittently rather than continuously. Elutriation was conducted
to reduce the cost of ERFP and ensure that the sludge met toxicity characteristic leaching procedure (TCLP) standards. The pH of the elutriation
liquid should be greater than 2.88. This work also establishes that FP or ERFP can be applied directly to treat dichromate and permanganate without
a prior reduction step.
© 2006 Elsevier B.V. All rights reserved.

Keywords: Laboratory waste liquid; Improved ferrite process; Elutriation; Heavy metal

1. Introduction Conventional technologies for treating heavy metals in

Laboratory waste liquid (LWL) refers to liquid waste gen-
erated in experiments performed for educational purposes,
research and examinations. The amount of LWL is minute,
explaining why it must be either collected over extended peri-
ods or derived from various sources to obtain an appropriately
operational amount. Therefore, LWL is highly complex and var-
ied. Treating LWL is more difficult than treating either industrial
waste liquid or wastewater owing to the inability to identify its
constituents.
Classified collection is critical to reducing the complexity of
LWL. “Heavy metal laboratory waste liquid (HMLWL)” is clas-
sified as such because it contains hazardous metals. These cannot
be eliminated by either physical or chemical means; at best, they
can merely be stabilized. According to the environmental laws
of Taiwan, the effluent may be discharged into a public water
body only when it fulfills effluent standards, and sludge can be
discharged into a landfill when it fulfills toxicity characteristic
leaching procedure (TCLP) standards. A treatment procedure
must satisfy these two conditions before it can be deemed to be
“complete”.
solution are based on chemical precipitation. Hydroxide,
carbonate and sulfide precipitations are the most common
methods. The sludge generated by chemical precipitation
has a loose structure, precipitates slowly, difficult to be fil-
tered, and dissolves easily in acid. Hence, it must be further
solidified before it can be deposited in a landfill. However,
solidification increases the volume of a landfill by a large
factor. It is particularly wasteful in areas where landfills are
scarce.
The ferrite process (FP), which is employed currently in
Japan, is another effective technique [1–4]. FP has many
advantages over chemical precipitation methods. It can be
applied directly to treat anions that contain heavy met-
als, such as Cr2 O7 2− , CrO4 2− , MnO4 − and others. It can
simultaneously remove various heavy metals, and the remain-
ing concentration is extremely low. The sludge produced
from this process is compact and easy to be separated and
it also fulfills TCLP standards without further solidifica-
tion.
FP was originally developed to produce magnetite (Fe3 O4 )
by wet-synthesis. The reaction equation is as follows:

∗ 1
Corresponding author. Tel.: +886 7 5254410; fax: +886 7 5254411. 3Fe2+ + 6OH− + O2 → Fe3 O4 + 3H2 O (1)
E-mail address: loujc@mail.nsysu.edu.tw (J.-C. Lou). 2

1383-5866/$ – see front matter © 2006 Elsevier B.V. All rights reserved.
doi:10.1016/j.seppur.2006.11.005
514 J.-C. Lou, C.-K. Chang / Separation and Purification Technology 57 (2007) 513–518
The reaction equation becomes Eq. (2) when the solution
contains other metal ions (for example with divalent cations):
1
xM2+ + (3 − x)Fe2+ + 6OH− + O2
2
→ Mx Fe(3−x) O4 + 3H2 O (2)
Treating heavy metal wastewater by FP involves the reaction
of Eq. (2) by inserting heavy metal ions into the spinel structure
formed from iron and oxygen.
Various studies indicated that three important factors deter-
mine the performance of FP [5–7]. First, the range of commonly
used pH is 9–11 because FP must be conducted under basic con-
ditions. Second, the reaction temperature must exceed 70 ◦ C to
ensure that the spinel crystal of ferrite is large and includes no
other mixed crystal phase. Third, the dosage of Fe2+ is typically
5–10 times the total metal content to ensure the quality of ferrite.
Aeration was used to provide oxygen for chemical oxidation. It
has ascertained that the air supply rate of 1 L/min is enough to
support the reaction by previous research [8].
As well as offering the advantages elucidated above, the FP-
treated sludge is stable and exhibits soft magnetism; it can be
recycled as a magnetic material, such as used in blind guide
bricks, magnetic symbols and electric wave absorbents. Also, it
can be resourced as catalyst to treat isopropyl alcohol and carbon
monoxide in waste gas [9]. Accordingly, this approach has great
potential. FP will interfere with chelating agent. This problem
has been solved by Fenton method [10].
This work develops a procedure for completely treating
HMLWL that improves upon the FP. Although various past
studies have claimed that FP can be adopted to treat heavy
metal-containing wastewater, all treatment targets have simple
compositions and low concentration, and exist only in the liq-
uid phase [11–15]. HMLWL is obviously more complex than
such wastewater. Its composition is difficult to anticipate, and
heavy metal precipitates or complex compounds may be present.
Although Tamura1 [1] reported the treatment of HMLWL by
FP, they considered only the effluent. Therefore, whether FP
can be adopted to treat completely HMLWL must be verified.
Besides, to establish an assistant procedure to improve treatment
efficiency of FP is worthy.
2. Materials and methods
2.1. Preparing simulated laboratory waste liquid
This study attempts to develop a procedure for effectively
treating almost all HMLWL, hence an extremely difficult
treating target-simulated waste liquid was designed. The total
concentration of heavy metals of the simulated waste liquid is
0.02 M. It contains 10 heavy metals—Cd, Pb, Cu, Cr, Zn, Ag,
Hg, Ni, Sn and Mn, each at a concentration of 0.002 M. Various
anions are adopted to elucidate their interactions (precipitation,
complexation, redox and others). Table 1 presents the chemi-
cals that were used. The 0.1 M solution of each heavy metal
reagent was prepared in advance; 20 mL was mixed with each
of the other solutions. Then, the mixture was diluted to 1 L by
Table 1
Chemicals to synthesize simulated heavy metal laboratory waste liquid
Metal Chemical Metal Chemical
Cd Cd(NO3 )2 ·4H2 O Ag AgNO3
Cu CuSO4 ·5H2 O Hg Hg(NO3 )2
Pb Pb(NO3 )2 Ni NiSO4 ·6H2 O
Cr K2 Cr2 O7 Sn SnCl2 ·2H2 O
Zn Zn(NO3 )2 ·6H2 O Mn KMnO4
adding deionized water. K2 Cr2 O7 and KMnO4 , which are highly
toxic and often used in laboratories, were adopted as sources of
Cr and Mn. These two compounds must be reduced before the
heavy metals can be placed into the spinel structure of ferrite.
Therefore, they can be used to test the reductive power of FP.
2.2. Analytical methods and instruments
Heavy metal concentrations were determined by induc-
tively coupled plasma atomic emission spectrometry (ICP-AES)
(ELAN5000, Perkin-Elmer, Germany). Although the TCLP test
corresponded to the regulations on methods allowed the Envi-
ronmental Protection Administration of the Republic of China
(NIEA R201.13C), the volume of the sludge was modified. The
extraction agent was prepared by adding 5.7 mL of glacial acetic
acid and 64.3 mL of 1 M NaOH to a 1 L volumetric flask that con-
tained 500 mL deionized water; then, the solution was diluted to
1 L by adding deionized water. The pH of the extraction agent
was 4.93 ± 0.05 and it should be checked before testing. About
4 g of dry sludge was placed in a 100 mL extraction bottle, and
80 g of extraction agent was added. The extraction bottle was
placed on the rotator and the bottle rotated at a frequency of
30 ± 2 rpm for 18 ± 2 h. Following this procedure, the concen-
tration of the heavy metals in the extraction liquid was measured.
2.3. Reaction equipment
The FP reactor is a 2 L stainless steel tank. The temperature
of the system is automatically controlled and a pH monitor is
used. An agitator is used to mix the solution thoroughly. An air
supply tube provides oxygen to the reaction from the bottom
of the reactor. The maximum air supply rate is 4 L/min. The
pH value is maintained in the range ±0.2 by adding NaOH or
HNO3 .
2.4. Treating HMLWL by conventional FP
About 1 L of the simulated waste liquid was poured into the
reactor. FeSO4 was added, the solution was agitated and it was
mixed uniformly. The pH of the solution was adjusted in advance
by adding NaOH or HNO3 ; then, heat the solution to the preset
reaction temperature. Next, air was supplied and the reaction
was timed. Reaction times of 20, 40, 60, 80 and 120 min were
used separately. The solution was filtered after it was cooled.
The sludge was dried in an oven at 105 ◦ C. The concentration of
each heavy metal in the filtered liquid was analyzed and, finally,
TCLP was applied to the sludge.
 J.-C. Lou, C.-K. Chang / Separation and Purification Technology 57 (2007) 513–518 515

Table 2
Heavy metal concentrations of filtered liquid of conventional FP
Heavy metal (mg/L)

Cd Cu Pb Cr Zn Ag Hg Ni Sn Mn Fe

Standarda <0.03 <3.0 <1.0 <2.0 <5.0 <0.5 <0.005 <1.0 b <10.0 <10.0
Maximum 0.287 0.421 0.575 1.979 1.232 0.210 0.029 0.438 0.891 0.258 0.686
Medianc 0.014 0.107 0.226 0.878 0.510 0.139 0.011 0.089 0.053 0.135 0.355
Minimum 0.008 0.046 0.025 0.081 0.039 0.076 0.002 0.021 0.006 0.037 0.132
Unqualified ratio 5/27 0/27 0/27 0/27 0/27 0/27 12/27 0/27 – 0/27 0/27
a Effluent standard of Taiwan.
b Sn has not limited standard at present.
c “Median” means the datum in the center when measured results were arranged in sequence of size. It, having not statistical meaning, shows merely distribution

of experiment data.

A full-factorial experiment is performed to determine the effi-
cacy of conventional FP. Twenty-seven reaction conditions with
the following levels of factors are used; pH 9, 10, 11; tempera-
ture 70, 80, 90 ◦ C; dosage of FeSO4 0.1, 0.14, 0.2 mol; air supply
rate 3 L/min.
2.5. Treating HMLWL by ERFP
The extended reaction ferrite process (ERFP) comprises two
stages. The initial stage is similar to a conventional FP, but
it is followed by an extended stage. In this work, the condi-
tions of the initial stage are: dosage of FeSO4 0.2 mol, pH 9,
temperature 90 ◦ C, air supply rate 3 L/min and reaction time
40 min. Apart from the manner in which FeSO4 is added, the
conditions of the extended stage are the same as those of the
initial stage. In the extended stage, a 1 M solution of FeSO4 is
added to the reaction system. The adding of FeSO4 is separated
into two ways—continuous dosing and intermittent dosing. In
continuous dosing, the FeSO4 solution was delivered using a
peristaltic pump at fixed rates of 2, 5 and 10 mL/min. In inter-
mittent dosing, a pipette was used to add instantly the FeSO4
solution at a fixed frequency, as follows: (1) 2 mL FeSO4 solu-
tion was added at 1 min intervals, (2) 10 mL FeSO4 solution was
added at 5 min intervals, (3) 20 mL FeSO4 solution was added at
5 min intervals. Following the extended stage, the temperature
was maintained and the air supplied for 40 min to ensure that the
ferrite was mature enough. Every experiment was repeated three
times.
2.6. Treating sludge by elutriation
The 5.7 mL glacial acetic acid was placed into a 1 L volu-
metric flask; adding 1 L of deionized water, and the pH was
adjusted by adding HNO3 or NaOH yielded the elutriation liq-
uid at pH 2, 2.88, 4 and 4.93. Some of the sludge that had already
been generated in conventional FP was mixed thoroughly before
further use. The 10 g of mixed sludge was placed in a 500 mL
bottle, to which 400 mL of the elutriation liquid was added. Five
bottles was prepared for each pH, and then put the bottles in a
shaker. Following 0.5, 1, 2, 6 and 18 h of shaking, samples were
obtained; the concentration of each heavy metal in the elutria-
tion liquid was analyzed, and the sludge underwent TCLP. Every
experiment was repeated three times.
3. Results and discussions
3.1. Treating HMLWL by conventional FP
This work examined 27 reaction conditions for conventional
FP, covering reasonable operating ranges. In none of the 27 sets
was the simulated waste liquid treated completely. Tables 2 and 3
summarize representative data obtained from these experiments.
Most samples of the filtered liquid are qualified. A few filtered
liquid is unsatisfactory because the concentration of Cd or Hg
slightly exceeds the effluent standards. Any qualified reaction
condition set can be adopted or this problem can be solved by
adding an ion exchange unit. The difficulty concerns the sludge.

Table 3
Heavy metal concentrations of TCLP extracted liquid of conventional FP
Heavy metal (mg/L)

Cd Cu Pb Cr Zn Ag Hg Ni Sn Mn Fe

Standarda <1.0 <15.0 <5.0 <5.0 b <5.0 <0.2 b b b b

Maximum 109.7 94.1 51.1 0.517 4.20 0.235 0.176 12.4 0.975 6.06 0.685
Medianc 78.5 41.7 38.4 0.258 0.682 0.104 0.088 3.85 0.317 1.234 0.335
Minimum 67.6 39.5 27.3 0.173 0.154 0.040 0.012 0.338 0.068 0.066 0.138
Unqualified ratio 27/27 27/27 27/27 0/27 – 0/27 0/27 – – – –
a The identification criteria for hazardous industrial wastes of Taiwan.
b Zn, Ni, Sn, Mn, Fe have not limited standard at present.
c “Median” means the datum in the center when measured results were arranged in sequence of size. It, having not statistical meaning, shows merely distribution

of experiment data.
516 J.-C. Lou, C.-K. Chang / Separation and Purification Technology 57 (2007) 513–518

Fig. 1. TCLP extracted concentration vs. reaction time in conventional FP.

All samples of the TCLP are unqualified because of Cd, Pb

and Cu. Their extracted concentrations significantly exceed the
allowed values, but those of the other heavy metals do not. There-
fore, the claim of Tamaura [1] that the FP can be utilized to treat
all heavy metals simultaneously does not hold in the light of cur-
rent Taiwanese environmental laws, because the claim neglects
the quality of the sludge. The main benefit of FP is that the quality
of the sludge it produces satisfies legal environmental standards,
reducing the costs of solidification and landfill treatment. In Tai-
wan, unless FP can be improved to increase the quality of the
sludge, it will no longer be applied because it is more expensive
than the precipitation procedure.
Further analyzing the TCLP data of the sludge formed over
various reaction periods reveals that the quality of the sludge
does not alter after 40 min. Using Cd, Pb and Cu as examples,
Fig. 1 reveals that increasing the reaction time does not improve
the quality of the sludge.
Kiyama [5] indicated that the first step in forming the heavy
metal into the spinel structure of ferrite is to form M(OH)+ (with
a divalent metal, for example). FP must be conducted under Fig. 2. Comparing the effects of continuous dosing ERFP on various Fe2+ adding
basic conditions, under which the most of precipitates are metal rate: (a) Cd, (b) Pb, and (c) Cu.
hydroxide, which must be dissociated before it can be treated.
FP can extract heavy metals from the liquid phase to yield the found to yield the lowest efficiency. The amount of Fe2+ added
solid of ferrite and to reduce the concentration of M(OH)+ in at a rate of 2 mL/min for a reaction time of 300 min is the same
the liquid phase. Chemical balance causes the dissociation of as that added at 5 mL/min for a reaction time of 120 min, but
metal hydroxide precipitate. Based on a similar principle, FP the effects differ considerably. This finding demonstrates that,
also causes the dissolution of non-metal hydroxide precipitates. in this reaction system, FP offers better treatment efficiency as
Accordingly, FP can also treat them effectively. the concentration of Fe2+ is increased. Only a high concentration
Conventional FP adds all FeSO4 immediately before reac- of Fe2+ can reduce the concentration of M(OH)+ in the liquid
tion. Thus, the concentration of Fe2+ falls rapidly with time. phase sufficiently to make the precipitates dissolve quickly.
The mechanism that promotes heavy metal precipitate dissoci- Fig. 3 shows the comparison of treatment efficiency of four
ation then terminates. Therefore, increasing the reaction time is different dosing modes. Intermittent dosing is more effective
ineffective. than continuous dosing. Continuous dosing can be regarded as
intermittent dosing with an infinitesimal interval. Fig. 3 shows
3.2. Treating HMLWL by ERFP that continuous dosing offers the worst performance. The treat-
ment efficiency of intermittent dosing with mode (3) (10 mL
ERFP is based on adding Fe2+ as necessary to sustain a con- FeSO4 solution once every 5 min) exceeds that of mode (2)
tinuous reaction. The result of so doing shows that the sludge (2 mL FeSO4 solution once every minute). Accordingly, the
following a suitable ERFP comprehensively satisfies the relevant extended stage yields better-quality sludge when the dose of
standards. Fe2+ is larger and the interval is longer for a particular total
Fig. 2 compares the effects of continuous dosing ERFP at amount of Fe2+ . This finding establishes again that if the tran-
various rates of addition of Fe2+ . Experimental results reveal sient concentration of Fe2+ is high enough, then the treatment
that addition rates of 5 and 10 mL/min can effectively improve efficiency of extended stage will be high. By comparing the
the quality of sludge. The rate of addition of 2 mL/min was results of modes (3) and (4) of Fig. 3, it reveals that increas-
 J.-C. Lou, C.-K. Chang / Separation and Purification Technology 57 (2007) 513–518
Fig. 3. Treatment efficiency of (a) Cd, (b) Pb, and (c) Cu by four FeSO4 adding
modes: (1) continuous dosing, 2 mL/min; (2) intermittent dosing, 2 mL FeSO4
solution once at 1-min interval; (3) intermittent dosing, 10 mL FeSO4 solution
once at 5-min interval; (4) intermittent dosing, 20 mL FeSO4 solution once at
5-min interval.
ing the amount of Fe2+ is not always preferable. The dosage in
mode (4) is double that in mode (3), but the effectiveness of the
treatment is only slightly stronger. The cost of FeSO4 represents
most of the expense of ERFP. The performance of unit FeSO4
is maximized by the intermittent dosing—by adding 10 mL
FeSO4 solution at 5 min intervals, throughout the 80 min of the
reaction.
The FP is capable of reducing hexavalent chromiun and per-
manganate because there is no unqualified record of Cr or Mn in
all experiments of this work. This function represents an advan-
tage of FP because chemical precipitation cannot be applied to
treat these metals directly.
3.3. Treating unqualified sludge by elutriation
Although the results herein showed that extending FP without
limit would enable all heavy metals to be completely treated, the
economic benefit of ERFP would be lost. Moreover, LWL is very
complex and variable, so a fixed process cannot be guaranteed
to treat all HMLWL completely, and unqualified sludge will
517
Fig. 4. Sludge’s TCLP extracted concentration vs. elutriation time: (a) Cd, (b)
Pb, and (c) Cu.
probably be present. A further strategy must be studied to treat
the general unqualified sludge.
Some of the sludge that had been generated in earlier con-
ventional FP experiments was mixed thoroughly to simulate
unqualified sludge. This work uses elutriation to wash out the
easily dissolved components of the sediment, ensuring that the
sludge satisfies TCLP standards. Four pH values (2, 2.88, 4
and 4.93) of the elutriation liquid were used. The experimen-
tal results show that the elutriation liquid at any of these four
pH values can dissolve the rest of the heavy metals, enabling the
sludge to meet TCLP standards. Less time is required as the pH
of the elutriation liquid decreases. Heavy metal precipitates have
various physical or chemical characteristics, and so exhibit var-
ious behaviors during elutriation. For example, the very small
dissociation constant of Cd causes it to exist in the form of
Cd(OH)2 [11]. Fig. 4(a) shows that the Cd that is not captured
in the ferrite will almost completely be dissolved after 0.5 h of
elutriation. Fig. 4(b) indicates that the Pb requires more time for
elutriation. A part of Pb should exist in non-hydroxide form in
the sediment. The most likely form is PbSO4 because high con-
centration of SO4 2− ion is present in the reaction solution of FP.
Fig. 4(c) shows that the Cu exhibits in a similar characteristic to
that of Pb. Some studies have demonstrated that CuO and Cu2 O
are the main forms of non-ferrite Cu in the sediments [15,16].
518 J.-C. Lou, C.-K. Chang / Separation and Purification Technology 57 (2007) 513–518
Fig. 5. Concentration of Fe in elutriation liquid vs. elutriation time.
Fig. 6. A flowchart for treating heavy metal laboratory waste liquid.
Fig. 5 reveals that the increasing concentration of Fe in the
elutriation liquid which reflect the dissolution of the ferrite at
pH 2. However, dissolution did not occur in the elutriation liq-
uid at pH 2.88. Hence, the acid tolerance limit of the ferrite is in
the range pH 2–2.88. Therefore, the pH of the elutriation liquid
should exceed 2.88. In practice, hydrochloric acid or sulfuric
acid are better elutriation liquids than acetic acid. When strong
acid is used without a buffer and the sludge formed by FP makes
the solution alkaline, an elutriation liquid pH of 4.93 is not fea-
sible. We therefore recommend an operating pH from 2.88 to 4
and an elutriation time of 6 h.
The waste elutriation liquid cannot be discharged because it
contains concentrated heavy metals. It should be returned to FP
to be treated. Though experiment result shows that the filtrated
liquid of FP or ERFP can meet the effluent standards, we should
be more discreet attitude toward environment. The effluent from
FP should be treated using an ion exchange unit before it is dis-
charged to ensure that it is harmless. Fig. 6 presents a suggested
flowchart for the treatment of HMLWL.
4. Conclusions
ERFP effectively improves the efficiency of conventional FP.
ERFP is required to treat large amounts of Cd, Pb or Cu to form
ferrite. If the amounts of Cd, Pb and Cu are small, then the
LWL can be treated with just a short extended stage, or even
conventional FP only. This work verified that Cr2 O7 2− , CrO4 2−
and MnO4 − can be directly treated and need not be reduced
beforehand. Elutriation is an effective approach for ensuring
the quality of the sludge at reasonable cost. Based on the find-
ings herein, a procedure was proposed for treating completely
HMLWL. For the simulated waste liquid of this work, the opti-
mum operating parameters in the initial stage are pH 9, FeSO4
dosage 0.2 mol/L, temperature 90 ◦ C, air supply rate 3 L/min and
reaction time 40 min; in the extended stage, they are intermit-
tent dosing, adding 10 mL 1 M FeSO4 solution every 5 min, pH
9, temperature 90 ◦ C, air supply rate 3 L/min and reaction time
80 min; in elutriation, the pH of the elutriation liquid should be
2.88, and the elutriation time 6 h.
Acknowledgement
The authors would like to thank the National Science Council
of the Republic of China, Taiwan for financially supporting this
research under contract number NSC 90-MOE-S-110-002-X.
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