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Silver Recovery from Waste Radiographic Films by Cementation and Reduction

Article  in  Canadian Metallurgical Quarterly · April 2010

DOI: 10.1179/cmq.2010.49.2.147

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 147

Canadian Metallurgical Quarterly, Vol 49, No 2 pp 147-154, 2010

© Canadian Institute of Mining, Metallurgy and Petroleum
Published by Canadian Institute of Mining, Metallurgy and Petroleum
Printed in Canada. All rights reserved

Silver Recovery from Waste Radiographic Films by

Cementation and Reduction
S. Aktas, M. H. Morcali and O. Yucel

Istanbul Technical University, Faculty of Chemistry and Metallurgy,

Maslak, 34469, Istanbul, Turkey
serdaraktash@yahoo.com

(Received in revised form February, 2010)

Abstract — Waste radiographic films can act as potential source materials for the recovery of valuable
silver. In this study, a chemical processing scheme was adopted to recover silver metal from waste
radiographic films. The films were dissolved in 1 M nitric acid (HNO3) solution for 3 hours at 70°C to
convert silver into silver nitrate (AgNO3(aq)). Subsequently, the silver nitrate solution was treated using
two different methods. The first involved cementation with fine iron powder and with fine zinc powder.
These two well-known cementators were compared to each other with respect to purity of the final
product and the recovery efficiency. The second method was sodium hydroxide (NaOH) precipitation.
The treatment with Fe powder and Zn powder resulted in the formation of metallic silver powder in just
one step. Ag2O obtained via NaOH precipitation was then treated using two different methods: a
treatment with a mixture of glucose (C6H12O6) and NaOH to yield metallic silver and a heat treatment,
in which Ag2O was converted to silver metal at 500°C. TGA analysis revealed that at 400°C Ag2O
decomposes into silver and oxygen. With the exception of the powder produced by glucose reduction, all
the powders would easily find industrial application. In addition, by using relatively inexpensive
chemicals these applied processes show promise for further scaling up.

Résumé — Les films radiographiques usés peuvent agir comme source potentielle de matériaux pour la
récupération de l’argent de valeur. Dans cette étude, on a adopté un schéma de traitement chimique pour
récupérer l’argent métallique des films radiographiques usés. On a dissous les films dans une solution d’acide
nitrique (HNO3) 1M pendant 3 heures à 70°C pour convertir l’argent en nitrate d’argent (AgNO3(aq)).
Subséquemment, on a traité la solution de nitrate d’argent en utilisant deux méthodes différentes. La première
impliquait la cémentation avec une poudre fine de fer et une poudre fine de zinc. On a comparé ces deux
agents de cémentation, bien connus, l’un à l’autre par rapport à la pureté du produit final et au rendement de
récupération. La seconde méthode impliquait la précipitation à l’hydroxyde de sodium (NaOH). Le
traitement avec la poudre de Fe et la poudre de Zn a entraîné la formation de poudre d’argent métallique en
une seule étape. Par la suite, on a traité l’Ag2O obtenu par précipitation au NaOH en utilisant deux méthodes
différentes: un traitement avec un mélange de glucose (C6H12O6) et de NaOH pour produire de l’argent
métallique et un traitement thermique, dans lequel l’Ag2O était converti en argent métallique à 500°C.
L’analyse par TGA a révélé que l’Ag2O se décomposait à 400°C en argent et en oxygène. Avec l’exception
de la poudre produite par réduction au glucose, toutes les poudres pourraient facilement trouver une
application industrielle. De plus, en utilisant des produits chimiques relativement peu coûteux, ces procédés
d’application sont prometteurs pour amplification future.

Key words: Silver, Radiographic films, Recovery, Cementation

INTRODUCTION
Silver, with a price around $500 per kilo [1], is one of the
precious and noble metals. It is used in large quantities for
many purposes, particularly in the photographic industry due
to its photosensitive properties. It has been reported that 25%
of the world’s silver needs are supplied by recycling and that
75% is obtained from photographic waste [2]. In terms of the
environment and economy, it is important that silver be
recovered from photographic waste.
Compared to other films, waste X-ray photographic
films contain an appreciable amount of silver to enhance

Canadian MetallurgiCal Quarterly, Vol 49, no 2

148 S. Aktas, M. H. Morcali and O. Yucel
sensitivity to transmitted X-rays and there is 0.7 to 2.0% silver
by weight left behind in the emulsion on the polyester film
base, even after the development and fixing processes [2].
These waste films are a good source of silver, which is reused
for a variety of purposes, including light sensitive materials.
Various studies have been carried out over a long period
of time to recover valuable silver from these wastes and most
of them have been patented [3-7]. Silver recovery methods
from waste films can be classified as a) burning the films
directly, b) oxidation of the metallic silver followed by
electrolysis and c) stripping the gelatine-silver layer using
different solutions. The second and third methods have been
used more extensively than the first method [2]. In general,
the methods reported for the recovery of silver from films
involve two steps; the first one involves stripping the silver
from the film and the second one is the recovery of the stripped
silver by smelting or electrolysis. The first step is commonly
leaching, which may be either microbiological [7-9] or
chemical [10]. Reagents such as sodium cyanide cause
environmental problems. However, the process involving
microorganisms is reported to be relatively slow [11-12].
EXPERIMENTAL WORK
Waste radiographic films containing 1.5% silver were
supplied from a hospital in Istanbul, Turkey. As mentioned in
the previous section, burning off the films is an option to
recover silver from waste radiographic films. However, in
this study, we did not prefer this method because it causes
environmental problems and leads to the loss of polymeric
materials which can subsequently be recycled.
The waste radiographic films with dimensions of 297
¥ 420 mm were cut manually into pieces with scissors; small
pieces with dimensions of 50 ¥ 50 mm were obtained and
these small films were subsequently placed in a borosilicate
beaker. Three hundred grams of waste films were dissolved in
3 L of 1 M HNO3. Excessive water content was subsequently
evaporated and optimal dissolution parameters were
established. These are 3 hours at 70°C at an agitation rate of
300 rpm in a temperature controlled water bath. The
experiment was carried out in a fume cupboard. Nitrogen
oxide gases, which formed during the dissolution reaction,
were successfully neutralized with the help of the washing
unit of the fume cupboard and subsequently released to the
atmosphere. The reason the leaching time was so long was
because the films were so voluminous that they became
pasted to each other and hence made interaction with the acid
difficult. After the silver was dissolved in the nitric acid
solution, the concentrations of elements present in the
solutions were measured with an atomic absorption
spectrophotometer (AAS) (Perkin Elmer Analyst 800) at the
end of each experiment. After leaching with nitric acid, a
solution with 4.5 g/L silver was obtained.
In the recovery step, two different precipitation methods
were studied: cementation and hydroxide precipitation. Since
they are common cementators, Fe and Zn powders with a
Canadian MetallurgiCal Quarterly, Vol 49, no 2
particle size less than 60 microns were employed to cement
the silver out of the solution. With this metallic replacement,
sub-micron metallic silver was precipitated after 1 hour at
room temperature in a shaking bath at 200 rpm. After the
cementation, excessive iron and zinc were reacted with 1 M
HCl to clean the product. The morphology of all products
was investigated using a scanning electron microscope
(SEM). X-ray analysis was also performed on the samples.
In the hydroxide precipitation method, sodium hydroxide
was employed to precipitate silver as silver oxide. At a pH
value of 11, a precipitation efficiency of 99.9% was attained
after 60 minutes at room temperature in a shaking bath at 200
rpm. After silver was precipitated as silver oxide, two different
routes were followed. In the first route, silver hydroxide was
subjected to a reaction with a mixture of glucose and NaOH.
This process resulted in porous metallic silver. In the second
route, silver hydroxide was heated to 500°C in a furnace under
argon atmosphere. It was possible to remove oxygen entirely
from silver oxide to yield metallic silver.
All the chemicals used in this study were of analytical
grade. Oxygen content of the samples was measured with a
NOH-2000 determinator and concentrations of impurities
present in the products were determined by an atomic
absorption spectrophotometer. The proposed process for
recycling waste radiographic films is shown in Figure 1.
For each experiment, 10 mL of the silver solution with
4500 ppm was reacted with a cementator in a falcon tube to
avoid exposure to air; otherwise, due to the vortex that
enables air to diffuse into the solution silver can redissolve
into the solution, resulting in lower efficiencies, as observed
in the study by Aktas. [13]. In this manner, air was not able to
diffuse into the system. Experiments were conducted in a
temperature-controlled shaking water bath to ensure uniform
heat convection at the surface of the falcon tube.
Solid/liquid separation was performed following each
run. For the AAS analyses, the 10 mL filtered solution was
Fig. 1. The proposed recycling process for waste radiographic films.
 Silver Recovery from Waste Radiographic Films by Cementation and Reduction
introduced into the machine with an appropriate dilution. The
efficiency of this recovery process was calculated from the
percentage of silver recovery using the following equation:
Recovery Efficiency (%) = (Co – Ct) ¥ 100 / Co (1)
where Co is the initial silver concentration (4500 ppm) and Ct
is the concentration at the end of the experiment.
RESULTS AND DISCUSSION
The process outlined in this paper can be used to treat waste
radiographic films and recover almost all of the silver present
in these films.
Dissolution of Silver Incorporated in Waste Radiographic
Films
As a noble metal, silver does not dissolve in HCl at room
temperature under moderate conditions, but it readily
dissolves in HNO3 to yield silver nitrate solution [14]. The
following reaction takes place (Equation 2):
3 Ag(s) + 4 HNO3(a.q) Æ 3AgNO3(a.q) + 2H2O(l) + NO(g) (2)
The following parameters were investigated to obtain the
optimum conditions to dissolve silver from waste
radiographic films.
Effect of Agitation Rate: In this experimental series, the effect
of agitation rate on the dissolution efficiency of silver from
waste radiographic films was investigated. Figure 2 displays
the effect of agitation rate on the dissolution efficiency of silver.
Fig. 2. The effect of agitation rate on the dissolution efficiency of silver
(1M HNO3, 1 hour, room temperature).
149
As can be seen from the figure, optimal dissolution
efficiency can be attained at an agitation rate of 300 rpm.
Without agitation, a poor efficiency is obtained although
efficiency increases up to 300 rpm. After this point, the
efficiency is observed to drop due to the fact that films are
pasted to each other resulting in poor contact of nitric acid
with the films. Thus, an agitation rate of 300 rpm was chosen
for further experiments.
Effect of Temperature: In this experimental series, the effect
of temperature on the dissolution efficiency of silver from
waste radiographic films is investigated. Figure 3 displays the
effect of temperature on the dissolution efficiency of silver.
As can be seen from the figure, temperature plays an
important role in the dissolution of silver from the waste
radiographic films. At 30°C, an efficiency of 65% was
obtained although at 70°C an efficiency of 88% was obtained.
After 70°C, there was no change in dissolution efficiency of
silver. This is the reason why 70°C was kept constant in the
following experimental series.
Effect of Time: In this experimental series, the effect of
contact time on the dissolution efficiency of silver from waste
radiographic films is studied. Figure 4 displays the effect of
time on the dissolution efficiency of silver.
It can be seen in the figure that contact time plays an
important role in the dissolution of silver from the waste
radiographic films. A dissolution efficiency of 88% is
obtained for a duration of 1 hour at 70°C although under the
same conditions when the leaching time is extended to 3
hours almost all the silver incorporated in the waste films was
achieved to be dissolved. Thus, a silver containing solution of
4500 ppm was obtained in the condition of 1M nitric acid, 3
hours, 300 rpm and 70°C.
Fig. 3. The effect of temperature on the dissolution efficiency of silver (1M
HNO3, 300 rpm, 1 hour).
Canadian MetallurgiCal Quarterly, Vol 49, no 2
150 S. Aktas, M. H. Morcali and O. Yucel
Fig. 4. The effect of time on the dissolution efficiency of silver (1M HNO3,
300 rpm, 70°C).
Precipitation of Silver by Cementation
After silver was dissolved into the solution, metallic
replacement was used to precipitate silver. For each
experiment, 10 mL silver solution with 4500 ppm was
employed, which contained 45 mg silver. Recovery efficiencies
were calculated by varying the amount of cementator from 10
to 80 mg corresponding to weight ratios of 0.22 to 1.76.
With this method, a precipitation efficiency of over
99% was attained in a shaking bath after an hour at 200 rpm
at room temperature. It is beneficial to employ an excessive
amount of cementator to attain higher precipitation
efficiency. Figure 5 shows the recovery efficiency with
regard to weight ratio.
As the figure suggests, zinc powder proved to be a
better cementator than iron powder for silver recovery. This
was also observed in a study by Karavasteva [15]. In the
study, the author investigated silver precipitation efficiency
using zinc, iron, copper and aluminum respectively and zinc
was reported to show the best performance among them. In
our study, we preferred using zinc and iron powders rather
than copper and aluminum powders because copper is a more
expensive metal in comparison to Zn and Fe. However,
aluminum powder is easily converted to aluminum oxide
resulting in poor recovery efficiencies when it is in a
powdery form [15]. Iron is the cheapest and the most
abundant metal among them and also a good cementator
under oxygen controlled atmosphere as proven in the present
study. On the other hand, zinc proved to obtain the best
recovery efficiency of silver. For instance, at a weight ratio
of 0.88 (40 mg zinc/45 mg silver), 96.15% of the silver was
precipitated using zinc powder, whereas an efficiency of
91.14% was achieved using the same amount of iron powder
(40 mg). This can be attributed to the fact that zinc is less
noble than iron.
Canadian MetallurgiCal Quarterly, Vol 49, no 2
Fig. 5. Silver recovery efficiency with respect to changing weight ratio
(200 rpm, room temperature, 1 hour).
Fe(s) Æ Fe2+(aq) + 2 e- Eox= – 0.44V (3)
Zn(s) Æ Zn2+(aq) + 2 e- Eox= – 0.76V (4)
The net cementation reaction takes place as follows:
2 Ag+(aq) + Meo(s) Æ 2 Ago(s) + Me2+(aq) (5)
The more noble silver is cemented out whereas the less
noble zinc or iron dissolves into the solution. It is
recommended that much more than a stochiometric amount
of cementator should be employed for a successful recovery.
By using an excessive amount of both cementators, it was
possible to achieve more than 99% recovery efficiencies, as
can be seen from the figure.
Silver Oxide Precipitation by Sodium Hydroxide
Following the dissolution of silver, concentrated NaOH
solution was deliberately added to the solution until the
solution pH became alkaline. Figure 6 shows the precipitation
efficiency of silver with regard to the solution pH.
At room temperature, over 99.9% silver precipitation
efficiency was attained in 60 minutes in a shaking bath at 200
rpm at pH=11. It can be seen from the figure that the pH
solution plays an important role in the precipitation of silver
from the solution. Unlike rhodium and palladium, silver does
not dissolve in excessive sodium hydroxide which enables us
to precipitate it quite effectively. The effluent solution can be
directly discharged after it is neutralized with acid.
Metallic Silver Production by Heat Treatment: After silver
oxide was produced by means of sodium hydroxide, it was
heated to 500°C under argon atmosphere. Figure 7 shows
 Silver Recovery from Waste Radiographic Films by Cementation and Reduction
decomposition of silver oxide with respect to temperature.
As shown in Figure 7, at around 350°C silver oxide
rapidly begins to decompose and this decomposition reaction
is complete at 400°C, which results in pure metallic silver.
The theoretical silver content of the silver oxide compound is
93.09%. As shown in the figure, it was successfully achieved.
Fig. 6. The precipitation efficiency of silver with respect to the solution pH
(200 rpm, room temperature, 1 hour).
Fig. 7. Decomposition of silver oxide with respect to temperature.
151
Metallic Silver Production by Glucose Reduction: Organic
reducers such as tartaric acid, glucose and formaldehyde etc.,
are used in various applications. An organic reducer, glucose
(C6H12O6), reduces silver oxide to metallic silver when it
reacts with the Ag2O in the presence of sodium hydroxide.
This was also observed in a study carried out by Wieczorek et
al. [16]. Following the precipitation, the silver oxide powder
was subjected to a reaction with glucose in the sodium
hydroxide media. By this treatment, silver oxide was
converted to silver by glucose [17]. Figure 8 displays the
conversion efficiency of silver oxide to metallic silver by the
help of glucose in the sodium hydroxide medium. The
pertinent reaction is presented below. (Equation 6)
At room temperature, over 99.97% silver conversion
efficiency was attained in 30 minutes at 200 rpm. As can be
seen from the figure, increasing amount of glucose results in
higher conversion efficiency of silver oxide to silver. It
should also be noted that sodium hydroxide should be present
in order to convert silver oxide to silver. Otherwise, glucose
cannot make this conversion alone.
Characterization of the Powders obtained
After silver was produced by each method, the samples were
washed with 1M HCl, then with distilled water and then with
pure alcohol. The powders were subsequently dried under
vacuum at 80°C for 1 hour. Effluent solutions, which formed
Fig. 8. The conversion efficiency of Ag2O to Ag (%) with respect to chang-
ing weight ratio of Ag2O/glucose (200 rpm, room temperature, 1/2 hour).
(6)
Canadian MetallurgiCal Quarterly, Vol 49, no 2
152 S. Aktas, M. H. Morcali and O. Yucel
during the cleaning process, were neutralized with the help of
sodium hydroxide and then they were discharged in line with
the regulations of the Istanbul Municipality.
To determine the purity of the powders that were
produced in this study, potentiometric titration was carried
out. The samples produced by zinc cementation and heat
treatment were found to contain 99.99% silver, whereas those
obtained via iron cementation and glucose reduction were
99.92% and 99.58% silver, respectively.
Oxygen content of the samples was measured with a
NOH-2000 determinator and concentrations of impurities
present in the products were determined using an atomic
absorption spectrophotometer. The oxygen content of the
samples for zinc cementation, iron cementation, heat
treatment and glucose reduction were found to be 0 ppm, 54.6
ppm, 0 ppm and 342 ppm, respectively. Other impurities for
zinc cementation and iron cementation were 16 ppm Zn and
740 ppm Fe, respectively. XRD analysis was also carried out
on the samples, as shown in Figure 9.
In the diffraction pattern, the peaks are clearly observed
at 2q = 37.93, 44.14, 64.68, 77.55, 81.51 which are in good
agreement with the metallic silver peaks.
Figure 10 displays SEM images of the silver powders
produced with each method.
According to Figures 10a and 10b, SEM images of the
powders produced via cementation closely resemble one
another. These images were also obtained in a study carried
out by Abdel-Aal and Farghaly [18]. The particles are sub-
micron in size and have dendritical structure. Figure 10c
clearly shows that a porous nanoscale structure was attained
although the powder produced by heat treatment is agglom-
erated due to sintering at 500°C (Figure 10d) making large
silver particle, which was also observed by Abdel-Aal and
Farghaly [18] although the SEM images are quite different.
CONCLUSIONS
In the present work, a chemical processing scheme was
adopted to recover silver metal from waste radiographic
films; it has been demonstrated that it is possible to recover
the silver metal incorporated in spent radiographic films at a
precipitation efficiency of more than 99%. The films were
dissolved in 1 M nitric acid (HNO3) solution for 3 hours at
Fig. 9. X-ray diffraction pattern of silver.
Canadian MetallurgiCal Quarterly, Vol 49, no 2
70°C so as to convert silver into silver nitrate (AgNO3). The
polymer substrate, which is left over after the treatment of
nitric acid, can be further recycled. The prepared AgNO3 was
treated with two different methods: 1) cementation with zinc
and iron powders and 2) precipitation by sodium hydroxide.
With a metallic replacement reaction by zinc and iron
powders, sub-micron-sized metallic silver powder was
produced. With this method fine silver powder was produced.
The silver purities were found to be 99.99 and 99.92%,
respectively, which can be directly used in various
applications. It should also be noted that zinc proved to be a
better cementator than iron in terms of silver recovery
efficiency.
After the silver oxide was precipitated via sodium
hydroxide, metallic silver powder was then easily produced
with two different methods: glucose reduction in alkali media
and heat treatment at 500°C under argon atmosphere, which
results in pure silver with 99.99% purity. Three nine silver
(99.90%) is acceptable in most silver industries. Since the
purity of silver produced by glucose reduction is less than
99.90% (around 99.58%), it requires further purification.
With the exception of the powder produced by glucose
reduction, all the powders could easily find industrial
application. These powders can be employed in the
production of silver nitrate which is used in anti-bacterial and
pharmacological applications, in the production of silver
cyanide, which is the main component of silver plating baths,
in jewelry and as alloying elements, etc.
Of these powders, the one produced by heat treatment
is the most expensive as argon; a furnace is involved in the
process, but it can be directly used in applications
mentioned above. Powders produced by cementation
exhibit similar properties and are quite inexpensive and
straightforward to be produced, but effluent solutions
emerge following the reaction and need to be discarded in
an environmentally friendly way, which might be costly.
The one that was produced using glucose is easy to be
produced and no harmful solutions are produced following
the reaction, but the product quality is less in comparison to
the other ones as silver content is 99.58% and thus it needs
to be further refined before the end user use it. But it still
can be used as an alloying element in silver ornaments,
plates etc.
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Canadian MetallurgiCal Quarterly, Vol 49, no 2
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