Development of an Eco-Friendly

Material Recycling Process for

Spent Lead Glass Using a
Mechanochemical Process and
Na2EDTA Reagent
RYO SASAI,* HISASHI KUBO,
MASAHIRO KAMIYA, AND HIDEAKI ITOH
Division of Environmental Research, EcoTopia Science
Institute, Nagoya University, Furo-cho, Chikusa-ku,
Nagoya 464-8603, Japan

Received August 6, 2007. Revised manuscript received

January 9, 2008. Accepted March 17, 2008.

To develop a novel nonheating method with lower energy

consumption and higher efficiency for recovering both lead
and SiO2 glass matrix from spent lead-glass powder, we attempted
to treat the spent lead glass by the mechanochemical
method using the metal chelate reagent, sodium ethylenediaminetetraacetate (Na2EDTA). As a result of the wet ball-milling
treatment of spent lead-glass powder sealed in a polypropylene
bottle with zirconia balls, Na2EDTA, and water at room
temperature, we found that more than 99 mass % of lead
contained in the spent lead-glass powder was extracted as a leadEDTA species from the solid silica glass network matrix. This
separation phenomenon was accelerated by the enlargement of
the solid-liquid interface area due to ball-milling atomization
and by the high stability constant of lead-EDTA. High extraction
yield suggests that Pb-O-Pb bonds in lead glass are
weakened or are broken down by the wet ball-milling treatment,
i.e., the strong mechanical energy such as the potential and/
or friction energy provided by ball-milling may be high enough
to elute lead ions from silica matrix. Moreover, we succeeded
in recovering both lead ions as lead sulfate, which is the main
compound of anglesite, and the EDTA as sodium-EDTA,
which is reusable as the metal chelate reagent in wet chemical
process using the ferric sulfate.

Introduction
Lead is very important as one of the constituent elements for
various materials such as batteries, solder, dielectric materials,
piezoelectric materials, glass, etc. However, it has been wellknown for many years that lead is very toxic, even when the
intake is extremely small. Recently the restriction of utilization
and import of lead and/or lead-containing instruments has
started since WEEE and RoHS directives have been announced in the European Union. Thus, research and
development of lead-free materials, which can replace leadcontaining materials, are being vigorously promoted in all
industrial fields. As a result, lead-free solder is progressively
becoming popular. However, a huge amount of leadcontaining materials is still used and discharged at present,
because all the lead-containing materials can not be replaced
* Corresponding author phone/fax: +81-52-789-5859; e-mail:
rsasai@esi.nagoya-u.ac.jp.

by alternative materials. Thus, the development of recycling,

detoxification, or resource recovery technology is a very
important and urgent issue. A practical recycling system of
lead batteries has been established already. On the other
hand, lead glass is one of the very popular glass materials
used as a protection material against radioactive rays, in a
cathode-ray tube (CRT), and as decorative glass. The amount
of spent lead glass will increase in the near future because
of a lot of discharged lead glass after CRT consumption. It
is anticipated, especially in Japan, that the discharged amount
will increase rapidly due to the law for recycling electric home
appliances being enacted in 2001 and because the CRT display
of color television has been replaced by the liquid crystaltype display. However, most spent lead glass has been
landfilled after some detoxification and stabilization processes to pass this enforcement.
Lead atoms contained in lead glass are firmly fixed by
encapsulation in the cavity of the glass network, which mainly
consists of the -O-Si-O- network and/or partly consists
of the structural component of the glass network such as
-O-Si-O-Pb-O-. Thus, the Pb extraction cannot be
fulfilled under ordinary temperature and pressure conditions.
Pb in lead glass is so strongly bonded that heating at
temperatures higher than 1273 K, at which SiO2 glass will
melt, is usually required for extraction, evaporation, and
removal of Pb from the SiO2 glass network. The current
recycling process, which is applied to a part of the spent lead
glass, requires very high energy consumption, thus its
recycling rate is still low in Japan. Moreover, there are a variety
of lead glasses with various chemical compositions depending
on usage. It is necessary, therefore, to sort them according
to each chemical composition, as far as the spent lead glass
should be recycled by the current method. The difficulty in
sorting will also cause a lower recycling rate. The development
of a novel recycling process for spent lead glass is essential
in order to increase the recycling rate with higher efficiency,
lower energy consumption, and lower price for operation,
regardless of its chemical composition.
The mechanochemical method with ordinary ball milling
and planetary ball milling is well-known as one of the grinding
and mixing methods for manufacturing fine powder of
various inorganic raw materials. Recently, the mechanochemical process attracted special attention as a process that
induces solid-state chemical reaction or alloying by mechanical energy at room temperature. This phenomenon may
be aroused by the cleavage and/or formation of covalent
bonding, an increase in surface area, or an increase in surface
energy through atomizing of larger particles. Application of
the mechanochemical technique to various waste disposals
has been already reported (1, 2). In our previous study, lead
was selectively collected as sulfate from lead zirconate titanate
(PZT) and lead lanthanum zirconate titanate (PLZT) sintered
bulks by the wet ball-milling method in the presence of
sulfuric acid (3, 4). In this case, other elements, Zr, Ti, and
La, were found to dissolve into acid solution as water-soluble
salts. However, it is very difficult to dissociate the SiO2 glassnetwork structure and dissolve lead ions into acid solution
at room temperature. Thus, we attempted to remove Pb atoms
from lead-glass powder by using the chelate reagent sodium
ethylenediamine-N,N,N,N-tetraacetate (Na2EDTA) dihydrate during the wet ball-milling process at room temperature.
In this study, we selected Na2EDTA as the chelating reagent
because Na2EDTA is well-known to form water-soluble and
stable metal complexes with various heavy metals. Na2EDTA
has been applied to the removal of various toxic heavy metals

TABLE 1. Chemical Composition of Lead-Glass Powder

compound

mass %
a

SiO2

PbO

BaO

K2O

Na2O

35.3

56.8

5.1

2.3

0.5

This mass ratio was calculated as oxide-base.

order to accomplish both metal recovery from metal-EDTA

and recycling of EDTA, various metods such as the electrolysis
method with cation-exchangeable film (5, 6), the coprecipitation method (7), the sulfide method (8), and the metalcation exchange method (5, 6, 911) have been developed by
many researchers and proposed as practical techniques
(511). However, these methods have some problems such
as higher operation and maintenance costs, a huge amount
of reagent addition, a huge amount of secondary hazardous
wastes, and a limit for application in a wide metalconcentration range. Therefore, a new recycling process
should be developed that allows us not only to separate the
heavy metals from metal-EDTA but also to recycle the EDTA
chelate reagent simultaneously.
In this study, we investigated on the extraction of lead
from the spent lead-glass powder by the wet ball-milling
treatment with Na2EDTA chelate reagent. Then, the separation and recovery of both lead minerals and sodium-EDTA
from lead-EDTA aqueous solution was attempted by the
chemical substitution method using ferric sulfate as additive.
Finally, we proposed an eco-friendly material recycling
system, in which most components in spent lead glass such
as lead, silica glass, etc. could be totally recovered as well as
the added Na2EDTA at room temperature.

Experimental Section

FIGURE 1. Dependence of the extraction rate (filled symbols

and left axis) of Pb (squares) and Ba (circles) and specific
surface area (open symbols and right axis) on the water/solid
ratio for 45 h. The added amounts of Na2EDTA are (a) 2.5, (b)
3.0, and (c) 3.5 g.

FIGURE 2. Treatment time dependence of the Pb- (squares) and

Ba- (circles) extraction rate (filled symbols: left axis) and
specific surface area (filled symbols: right axis). Na2EDTA:
3.5 g. Water: 4.0 cm3.
from the polluted soil or the municipal waste incineration
fly ash (MW-IFA). Although Na2EDTA is effective to detoxify
these metals, it is considerably difficult to recover them as
minerals from metal-EDTA species because the chelating
stability constant is too high. Furthermore, Na2EDTA is
relatively expensive as a reagent for the waste treatment. In

Materials Used and Pretreatment of Lead-Glass Powder.

Commercially available lead glass for radiation shield was
used as an experimental specimen, which has the average
chemical composition as shown in Table 1. Sodium ethylenediamine-N,N,N,N-tetraacetate dihydrate (Na2EDTA:
DOJIN) was used as the chelate reagent. Coarsely ground
lead-glass powder was pretreated by the planetary ball-milling
apparatus (P-5, FRITSCH). This milling operation was carried
out by repeating the unit operation 12 times, which consists
of grinding for 1.5 h at 300 rpm with an interval of 0.5 h. The
pretreated lead glass, hereafter abbreviated as pre-PbG, was
dried at 383 K for 18 h under a vacuum. All the chemicals
were used without further purification.
Mechanochemical Treatment of the Lead-Glass Powder.
The pre-PbG powder (2.5 g) was sealed in a polypropylene
bottle (50 cm3) together with an appropriate amount of
Na2EDTA and deionized/distilled water as well as 60 g of
zirconia ball (size: 5.0 mm). Ball-milling treatment of a
powder sample was performed by a rotary ball-milling
apparatus (UB-32, YAMATO) at 300 rpm for 0-96 h. After
this ball milling, the powder sample and zirconia balls
adhered with powder were rinsed with 100 cm3 of water by
sonication for 0.5 h, and then the white powder was
completely separated from aqueous media and collected by
a vacuum filtration. The obtained white powder was dried
at 383 K for 24 h under a vacuum.
Metal Recovery by Ferric Sulfate. Ferric sulfate 14hydrate, Fe2(SO4)3 14HO2 (purity: 60-80%, KISHIDA reagents
chemicals), was added to the metal-EDTA aqueous solution
(50 cm3) obtained by the mechanochemical treatment under
the optimal condition of the molar ratio Fe/metal ) 0.5-1.5,
and then the mixed solution was stirred for 1-12 h at room
temperature. After the reaction treatment, the solid-liquid
separation was performed by vacuum filtration. The prepared
precipitates were dried at 333 K for 24 h.
Recycling of EDTA after the Metal Recovery Treatment.
The pH value of the Fe-EDTA aqueous solution obtained by
the lead recovery operation was adjusted to more than 13 by
adding NaOH (WAKO pure chemicals industries, Ltd.), and
then the precipitates were collected by vacuum filtration.
This precipitation was identified as hydrous iron oxide,
Fe2O3 nH2O, by XRD analysis, and the recovery rate of iron
was almost 100%. This basic aqueous solution, probably
containing sodium-EDTA, was treated by two kinds of

FIGURE 3. SEM images of lead-glass particles after wet ball-milling (Na2EDTA: 3.5 g; water: 4.0 cm3) for (a) 0, (b) 4, (c) 8, (d) 24, (e)
45, and (f) 72 h.
AES. Crystalline compounds after each treatment were
identified by X-ray diffractometer (XRD: RINT2500, RIGAKU)
using Ni-filtered Cu KR radiation. The microstructure of leadglass powdery particles before and after the mechanochemical treatment was observed by the scanning electron
microscope (SEM: JSM-6330F, JEOL). At the same time as
the microstructural observation of lead-glass powdery particles, the element analysis on particle surface was performed
by the energy-dispersive X-ray spectroscopy (EDS: JED-2140,
JEOL). Specific surface area of glass powder was measured
by the BET one-point method (MS-21, Qantachrome). X-ray
photoelectron spectroscopy (XPS: ESCA-3300, Shimadzu) was
performed for determining the surface analysis of the leadglass powdery particles before and after the treatment.

Results and Discussion

FIGURE 4. XRD patterns of the precipitate obtained after adding
Fe2(SO4)3 14H2O (Fe/(Pb + Ba) ) 1.5) to the extracted solution
and agitating for 12 h. Symbols: PbSO4 (b); BaSO4 (().
recycling techniques: (1) the pH value of the basic aqueous
solution was adjusted to 4.44 by adding the concentrated
hydrochloric acid solution (WAKO pure chemical industries,
Ltd.). The obtained aqueous solution was called re-EDTA(lq)
hereafter. (2) The pH value of the basic aqueous solution
was adjusted to less than 3 by adding the concentrated
hydrochloric acid solution. Then, the precipitated powder
was collected by vacuum filtration. After this, the precipitates
were dissolved in NaOH aqueous solution (0.324 mol/dm3),
the white powder was collected by evaporating the water
under reduced pressure, and then the powder was dried at
333 K for 24 h. This white powder was called re-EDTA(s)
hereafter. These recycled EDTAs, i.e., re-EDTA(lq) and reEDTA(s), were used as the chelate reagents for the metal
extraction experiments from the pre-PbG powder under the
optimal conditions.
Analysis. Quantitative analysis of metal (Pb, Ba, etc.)
content in lead-glass powder before and after the mechanochemical treatment was carried out by the inductively
coupled plasma atomic emission spectrometry (ICP-AES:
OPTIMA 3300DV, Perkin-Elmer) analysis of the solution
obtained after the glass powder was fully dissolved into the
hydrofluoric acid. The metal amount in aqueous solution
after the each treatment was quantitatively analyzed by ICP-

Mechanochemical Treatment of the Lead-Glass Powder.

Figure 1 shows the dependence of extraction rate of Pb or
Ba from lead glass (left axis) and specific surface area (right
axis) on the water [mL]/solid [g] ratio for 45 h. It is found that
the wet ball-milling treatment in the presence of Na2EDTA
can remove Pb and Ba from lead-glass particles. In addition,
the extraction behavior of Pb or Ba exhibited an tendency
analogous to that of the specific surface area against the
horizontal axis. This result shows that the extraction of Pb
or Ba ions from a lead-glass particle occurs by the complexation between EDTA chelate and Pb or Ba ions which
are exposed on the glass particle surface formed by ball
milling. In the case of the Na2EDTA added amount of 2.5 g,
the extraction rate of both Pb and Ba ions was constant at
ca. 90 mass % for the water/solid ratio more than ca. 0.4
cm3/g, while the specific surface area saturates at a higher
water/solid ratio value. This discrepancy between the
extraction rate and specific surface area could be explained
by the shortage of added Na2EDTA, i.e., the added amount
of Na2EDTA (6.71 mmol) is lower than that of the total amount
of Pb and Ba (0.51 mmol (Pb: 0.5 mmol and Ba: 0.01 mmol))
that remain in the treated lead-glass powder. The saturation
behavior of the Pb- or Ba-extraction rate was also observed
in the case of the added Na2EDTA amount of 3.0 g, although
the amount is enough to extract Pb and Ba ions from leadglass powder. This saturation behavior of extraction rate is
supposed to correspond to that of specific surface area, which
demonstrates that more pulverization of glass particles is

TABLE 2. Metal Recovery Rate from the Extracted Solution by Ferric Sulfate Treatment with the Different Added Amounts of
Fe2(SO4)3a
Fe/metal ratio

Pb (mass %)
Ba (mass %)
a

0.5

1.0

1.5

2.0

2.5

3.0

4.0

5.0

87.00
98.00

99.95
100.00

99.98
100.00

99.98
100.00

99.98
100.00

99.98
100.00

99.97
100.00

99.97
100.00

Error of data was (0.05 mass % as a result of several time experiments.

TABLE 3. Metal Recovery Rate from the Extracted Solution by

Ferric Sulfate Treatment with the Different Added Amounts of
Fe2(SO4)3 for Various Treatment Timesa
treatment time (h)

Pb (mass %)
Ba (mass %)

1.0

2.0

4.0

8.0

12.0

99.92
100

99.98
100

99.98
100

99.98
100

99.97
100

a
Error of data was (0.05 mass % as a result of several
time experiments.

impossible, i.e., the amount of Pb and Ba exposed on particles

surface is constant. These results indicate that the extraction
of Pb or Ba by Na2EDTA chelation will occur on only the
surface of the lead glass bared by ball milling. These
conclusions are also supported by Figure 1c, in which both
the Pb- or Ba-extraction and the specific surface area
increased with an increase in the water/solid ratio.
Figure 2 shows the treatment time dependence of the Pbor Ba-extraction rate and the specific surface area after the
wet ball-milling process with 3.5 g of Na2EDTA and 4.0 cm3
of water. About 88 mass % of Pb or Ba was extracted only on
the sonication stage from the pre-PbG, which was a sample
powder before wet ball milling. This result shows that ca. 88
mass % of Pb or Ba included in lead glass is exposed as ions
loosely bound on the surface of glass particles formed by the
planetary ball-milling treatment, and these Pb or Ba ions are
extracted by chelation with Na2EDTA. The specific surface
area gradually increased with an increase in the treatment
time, and it became almost constant for more than 72 h. On
the other hand, the extraction rate of Pb and Ba increased
rapidly up to 8 h, and then it exhibited a gradual increase
with an increase in the treatment time, attaining an almost
constant value over 20 h. Therefore, the optimal treatment
time was found to be 20 h under these conditions (Na2EDTA:
3.5 g, water: 4.0 cm3), which is when we succeeded in
removing 99.5 mass % of Pb and 99.0 mass % of Ba from lead
glass by ball-milling treatment with no heating.
Figure 3 shows the SEM images of lead-glass particles
after the ball-milling treatment under the optimal conditions
for various treatment times. The pre-PbG particles had
relatively wide grain size distribution (cf. Figure 3a). From
SEM images of lead glass treated for 4 and 8 h, larger particles
as shown in Figure 3a were preferentially pulverized by wet
balling (cf. Figure 3b,c). This preferential pulverization of
coarse particles would cause a rapid increase in Pb- or Baextraction rate within 8 h. The particle size did not drastically
decrease, but it did slightly decrease after 24 h ball milling.
This gradual decrease in particle size is responsible for the
slight exposure of Pb or Ba atoms to the particle surface, and
thus the extraction rate slightly increased, too. Finally, the
extraction rate saturated, because the exposure of the fresh
surface by ball milling was completed. This is also supported
by the saturation of specific surface area.
Metal Recovery by Ferric Sulfate. Figure 4 shows the
XRD patterns of the precipitates obtained after adding ferric
sulfate, Fe2(SO4)3 14H2O (the mol ratio of Fe/metal ) 1.5),

FIGURE 5. XRD patterns of the precipitates after the wet

ball-milling treatment with (a) re-EDTA(lq) and (b) with
Na2EDTA reagent solutions. Symbols: BaSO4 (b).

FIGURE 6. XRD patterns of (a) precipitates obtained after acid

treatment of re-EDTA(lq) and (b) re-EDTA(s). Symbols: H4EDTA
((); Na2EDTA (b); Na4EDTA (().
to the extracted solution (Pb: 1.2 g/dm3, Ba: 0.9 g/dm (3))
and agitating for 12 h. Diffraction lines for PbSO4 and BaSO4
are apparently identified in the precipitates. This result
indicates that the Pb and Ba ions in EDTA are substituted
by the Fe3+ ions, which form by dissolution of Fe2(SO4)3 14H2O into water, and then the eluted ions are
collected as the precipitates, PbSO4 and BaSO4, by the reaction
with SO42-.
The metal recovery rate from the extracted solution is
shown in Table 2 for the different added amounts of ferric
sulfate. In the case of more than 1.0 of Fe/metal ratio, both
Pb and Ba ions contained in the extracted solution were fully
collected by this technique. This result indicates that the
substitution of Pb and Ba ions with Fe(III) ions will be mostly
a stoichiometric reaction, because the metal-complex stability
constant of Fe3+ (log KMY ) 25.1) is larger than those of both
Pb2+ and Ba2+ (log KMY ) 18.04 and 7.76, respectively) under

FIGURE 7. Schematic diagram of a novel material recycling system for spent lead-glass powder.
the neutral condition. On the other hand, the amount of the
collected precipitates was more than the stoichiometric
amount, when the Fe/metal ratio was 0.5. This nonstoichiometric behavior could be caused by the coprecipitation
reaction, in which Pb- and/or Ba-EDTA would be included
in the collected precipitates. Thus, the optimal Fe/metal ratio
was determined to be 1.0. The metal recovery rate from the
extracted solution by the ferric sulfate treatment for a given
treatment time is shown in Table 3. Both Ba and Pb ions in
the extracted solution could be fully recovered by the ferric
sulfate treatment for more than 1 h. These results lead to the
conclusion that the optimal conditions for the metal recovery
treatment by ferric sulfate are an Fe/metal ratio of 1.0 and
reaction for 1 h at room temperature.
Recycling of EDTA Chelate Reagent. As mentioned in
the Experimental Section, the Fe-EDTA aqueous solution
obtained by the ferric sulfate treatment was converted into
the Na2EDTA basic aqueous solution described as reEDTA(lq) by the pH adjustment (pH ) ca. 13) with NaOH
addition, which resulted in the formation of iron hydrous
oxide precipitates. Figure 5a shows the XRD pattern of the
powder treated by the wet ball milling of the pre-PbG with
re-EDTA(lq) under the optimal milling conditions. The
diffraction lines from BaSO4 crystallites could be observed,
whereas the lines could not be observed in the case of the
wet ball milling with Na2EDTA reagent solution (see Figure
5b). Moreover, there are no Ba ions in the extracted solution,
the reason of which is attributed to the large amount of SO42anions that remained in re-EDTA(lq). During the wet ballmilling treatment, the Ba ions dissolved from the lead-glass
surface reacted promptly with SO42- anions to form insoluble
and stable BaSO4. Therefore, re-EDTA(lq) is not appropriate
for the metal recovery from the spent lead glass by wet ball
milling, which suggests that the EDTA recycling by the pH
adjustment is not enough.
Purification of re-EDTA(lq) was attempted according to
the second protocol described in the Experimental Section
for yielding re-EDTA(s). Figure 6 shows the XRD patterns of
both white powders obtained by the acidic pH adjustment
(pH < 3) and re-EDTA(s). XRD patterns exhibited that the
recovered powders of re-EDTA(lq) (Figure 6a) and re-EDTA(s)
(Figure 6b) were identified as the free acid, H4EDTA, and
Na2EDTA with a small amount of Na4EDTA, respectively.
Moreover, the recovery rate of EDTA was as high as ca. 95
mass %. As a result of the wet ball-milling treatment of the
pre-PbG powder with re-EDTA(s) aqueous solution, both Pb
and Ba recovery rates were almost the same as that of the
treatment with virginal EDTA reagent solution. It was
concluded, therefore, that the present recovery process of
Na2EDTA powder through the production of free acid was
very effective, as the purity of re-EDTA(s) was more than 99
mol%.
Proposal of a Novel Material Recycling System for Spent
Lead Glass. Finally, we propose a novel material recycling
system for spent lead glass as shown in Figure 7. In the
first step of the wet ball-milling process, ca. 99.5 mass %

of Pb and ca. 99.0 mass % of Ba contained in lead-glass

powder are extracted as Pb- and Ba-EDTA complexes into
the liquid phase, and then silica powder with high purity
is separately collected as precipitate after the filtration
process. Unlike the conventional recycling process for
spent lead glass, the present wet ball-milling method has
a lot of advantages: (1) The energy consumption is very
low, because the treatment is carried out at room temperature. (2) The existing powder production equipment
like ball milling can be utilized. (3) The recovered silica
powder can be reused as cullet for glass production.
Moreover, the present separation process will be effective
for recycling of not only lead glass but also other glass
materials containing toxic or precious metal resources.
In the second step of the ferric sulfate method for metal
recovery, ca. 100 mass % of Pb or Ba from the extracted
solution can be recovered as sulfate, PbSO4 or BaSO4, which
will be used as a resource for lead smelting. The Fe-EDTA
dissolved in aqueous solution obtained in the second step
can be converted to Na2EDTA by addition of NaOH, when
Fe ions can be collected as iron hydrous oxide precipitates
(yield: 100%). A large amount of SO42- anions is dissolved
in this Na2EDTA basic aqueous solution. In order to form
the free acid, H4EDTA, the pH value of the Na2EDTA basic
aqueous solution is adjusted to less than 3 by hydrochloric
acid. The obtained H4EDTA powder is dissolved in the
NaOH basic aqueous solution, again, and then Na2EDTA
powder is recovered by evaporating the solvent (yield: ca.
95%). This Na2EDTA powder is reusable as a chelate reagent
for the wet ball milling of spent lead glass. As described
above, the present spent lead recycling system requires
no heating process for recovering lead atoms from spent
lead glass, and the EDTA recycling procedures are very
simple and easy chemical operations. Therefore, the
present system has a potential as a novel practical and
industrial process for recycling spent lead glass without
an excess consumption of energy or expensive maintenance costs.

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