Chemical Engineering Journal 173 (2011) 303308

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Chemical Engineering Journal

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Pollution control of surface waters by coupling gliding discharge treatment with

incorporated oyster shell powder
E. Njoyim-Tamungang a , S. Laminsi a , P. Ghogomu a , D. Njopwouo a , J.-L. Brisset b,
a
b

Inorganic Chemistry Laboratory, Chemistry Department, University of Yaounde-I, Yaounde, Cameroon

Chemisty Department, Faculty of Science, University of Rouen, 76821 Mont-Saint-Aignan, France

a r t i c l e

i n f o

Article history:
Received 9 May 2011
Received in revised form 19 July 2011
Accepted 19 July 2011
Keywords:
Gliding electric discharge
Non-thermal air plasma
Industrial efuents
Domestic pollutant abatement
Wastes water degradation
Oyster shells powder

a b s t r a c t
Highly oxidizing gaseous species ( OH, NO and derivatives) formed in an electrical discharge (a gliding
discharge burning in humid air), are suitable for abating the organic pollutant concentration of surface
waters sampled in Cameroonian brooks, e.g., 47% (Total Organic Carbon, TOC) within 10 min exposure.
The plasma technique coupled with the use of nely powdered oyster shell (OS) acting as a catalyst and
an acidity control agent thus yields improved results. This paper is devoted to determining the optimum
amount m (g L1 ) of incorporated OS before switching on the discharge for given exposure times t* (min).
The process effects are controlled by means of pH, Biological and Chemical Oxygen Demands (BOD,
COD), and Total Organic Carbon (TOC) measurements performed for various t* and m values and the
results are compared with a mere plasma treatment on the same samples. The BOD5 and TOC values
respectively decrease by 86% and 36% for 10 min exposure with 1 g L1 incorporated OS. Treatments
with OS stabilize acidity around pH: 6.5 while the pH decrease is more important without OS. BOD5 and
TOC exponentially decrease with t* with or without incorporated OS, as does COD with OS only. BOD5
exponentially decreases with increasing m while COD linearly depends on t* and m, and TOC on m only.
Optimized treatment parameters are t* = 30 min, m = 0.1 g L1 .
2011 Elsevier B.V. All rights reserved.

1. Introduction

2. Materials and methods

A matching paper by Njoyim-Tamungang et al. [1] shows that

electric discharges burning in air over samples of waste surface
waters are suitable for abating pollution of industrial and domestic
efuents. The reported results conrm previously published important results relevant to the plasma treatment of efuents from food
industry [2,3]. This paper accounts for technical developments of
using electrical discharges with the same environmental purpose
of eliminating organic waste solutes.
This paper focuses on an improved process tested at the laboratory scale and based on coupling a gliding electrical discharge in
humid air at temperatures close to ambient and atmospheric pressure, with nely powdered oyster shells (OS). These useless solid
wastes are claimed to x pollutants by adsorption. In the present
study, they are incorporated to the liquid samples before being
exposed to the discharge. The targeted samples were the same as
previously considered by the same authors [1] in order to make easy
a comparison between a mere plasma treatment and the mixed
process and check whether coupling gives rise to synergistic effects.

2.1. Collection and analyses of the liquid samples

The liquid samples were directly collected in several points from
2 brooks which ow through Yaounde and Douala (i.e., the most
important cities in Cameroon) and gather domestic and industrial
waste waters. The samples were stored at 4 C before being analysed or processed. The main organoleptic characteristics of the
samples as analytical techniques specify to pollution have been
reported [1,4]. Exposure of the liquid samples with various masses
of incorporated OS for known exposure times t* (min) modies the
properties of the liquid and consequently the efcacy of the plasma
treatment.
The treatments were checked by pH-metry, Total Organic Carbon measurements (TOC), according to the Walkley and Black
method [5], Biological and Chemical Oxygen Demands (BOD5 and
COD) as previously mentioned [1,4]. Due to the variety of the samples and their different characteristic values, we had also to use
statistical analysis (minitab software, 2003).
2.2. Collection of oyster shells

Corresponding author. Tel.: +33 235 146 658.

E-mail address: brissjl@club-internet.fr (J.-L. Brisset).
1385-8947/$ see front matter 2011 Elsevier B.V. All rights reserved.
doi:10.1016/j.cej.2011.07.021

Oyster shells (OS) are a waste product from aquaculture. They

are still useless and thus present a major disposal problem in coastal

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E. Njoyim-Tamungang et al. / Chemical Engineering Journal 173 (2011) 303308

Fig. 1. Set up for plasma batch treatment.

regions such as south-east Korea. However, pyrolysis of waste oyster shells under dened conditions (750 C for 1 h under nitrogen
atmosphere) was recently claimed to transform this material into a
sustainable reagent for efcient removal of phosphates from waste
water. This huge effect (up to 98%), compared with raw oyster
shells which removed almost no phosphate from water, accounts
for largely more efcient modication than heating the shells to
750 C in air which only removed up to 68% of phosphates from
water. Shamim et al. [6] investigated the temperature effect on
waste water treatment with natural shells: they observed a signicant enhancement of the removal of suspended solids and COD.
Xiong and Zhilong [7] evidenced the removal capacity of oyster
shell biolter which reached 97% Ammoniumnitrogen for an initial concentration of 60 mg L1 and in a pH range of 5.35.7. They
also observed that the pH of the input liquid could be maintained at
6.5. These pieces of information were essential and determined our
attempts of coupling plasma with the properties of OS to evidence
positive synergistic effects.
The collected natural shells were directly used for the process
after washing, sun drying, mechanically crushing to a ne powder in a porcelain mortar and sieving with merge of size 0.5 mm.
Weighed quantities of powder were incorporated to the liquid
sample before switching on the discharge and exposing the target
solution to the plasma plume for time t*.
A part of the raw OS material was devoted to structural and
chemical analysis by Inductively Coupled Plasma Atomic Emission
Spectroscopy after dissolution in HCl [4]. X-ray diffraction analysis
conrmed that calcium oxide was the main component of pyrolysed oyster shells, whereas calcium carbonate (calcite) was that
of raw shells [4,8]. The present form of Ca CO3 was mainly calcite
and little aragonite, as shown by X-ray diffraction and conrmed
by FTIR spectra.
2.3. The Gliding discharge and the plasma reactor
The gliding discharge (GD) technique was rst proposed by
Lesueur et al. [9] and developed by Czernichowski [10] for the
decontamination of gases. The technique is detailed and illustrated
elsewhere [11,12]; the species generated in a discharge in humid air

are listed and the relevant induced chemical properties mentioned

as well. The main active species in our case are OH and NO radicals
and their derivatives (e.g., H2 O2 and ONO2 H) which induce strong
oxidizing and acid effects [12]. The electric device and the 500 mL
reactor were the same as previously used and described (Fig. 1);
the electric power delivered to the discharge is not modied and
remains close to 100 W.
It is worth being underlined that the arc that forms at the narrowest electrode gap is actually a thermal plasma. The gas ow
(humid air) delivered according to the axis of the reactor moves
the arc feet along the diverging electrodes, so that the arc length
increases (and its temperature decreases) until it breaks into a
plasma plume (i.e., a quenched plasma) when it is short-circuited
by a new arc. Thus the macroscopic temperature of the liquid target
remains close to ambient and increases by a few tens of degrees Celsius, which may discard the thermal effect in microbial inactivation
plasma treatments.
This device is adapted to operate in circulating and batch modes
but the batch treatment was preferred for this introductory study.
The liquid samples were exposed to the GD for time t* (min) after
having incorporated known masses m (g L1 ) of oyster shells. For
making easier the comparison between the mixed process and the
plasma process alone, the exposure times t* were identical, so that
both processes involve the same energy costs.

2.4. A glance on the matching plasma chemistry

The gliding discharge burns in humid air, i.e., in environmental
conditions characterized by the main parent species O2 , N2 and
H2 O. The arc is an electric energy carrier which favours energy
exchange with the surrounding species and induces bond breakings and excitation (and partly, ionization) of moieties by electron
impact. The so formed primary species are OH and NO, which are
present between the electrodes and identied and quantied by
emission spectroscopy:
H2 O + e H + OH + e

O2 + e 2 O + e
N2 + O NO + N

E. Njoyim-Tamungang et al. / Chemical Engineering Journal 173 (2011) 303308

6.8

6.6

6.4

6.2

pH

pH

305

4
3

6
5.8

5.6

5.4

10

20

30

40

exposure time t* (min)

m (g L-1)

Fig. 2. pH evolution (A) with exposure time t* of samples exposed to plasma only (black dots) or in the presence of incorporated OS (0.1 g L1 , empty squares); (B) with the
mass m (g L1 ) of incorporated OS for samples exposed for 5 min to the discharge.

and the matching disappearance reactions, e.g.,

H + H
H + O
2

H2
HO2

O + O (+M) O (+M)
2
3
O3 + NO NO2 + O2

In the plasma plume, the primary and parent species may react
together and yield secondary species which impinge at the liquid
surface with the parent species, e.g.,
NO + OH

ONOH
NO2 + OH ONOOH

2 OH H2 O2
HO2 + NO ONOOH

The reactions induced by the plasma species take place at the

liquid surface, but also in the liquid phase for the soluble moieties.
In case of discharges burning in air over the solution, peroxynitrite, ONOOH and hydrogen peroxide, H2 O2 are the main species
concerned; the case is different with immerged discharges (electrohydraulic discharges) where the formed OH are directly in contact
with the waste solutes.
Three plasma formed compounds are mainly concerned with
solute/plasma interactions and induce acid and oxidation reactions.
The acid effect is related to the formation of transient nitrous
acid, ONOH (which disproportionates into NO and Nitric acid for
pH < 6) and stable Nitric acid. Peroxynitrous acid is a weak acid
(pKa = 6.8).
The oxidizing character is attributed to OH, since hydrogen peroxide can dissociate, H2 O2 and ONO2 H. The relevant oxidation potentials, e.g., E (H2 O2 /H2 O) = 1.68 V/SHE,
E ( OH/H2 O) = 2.85 V/SHE and E (ONOOH/NO2 ) = 2.05 V/SHE are
largely higher than that of the oxygen system E (O2 /H2 O) and
most of those of organic waste compounds which are close to
0.5 V/SHE.

allowed us to determine whether the les of results relevant to a

couple of treatments were signicantly different or not. The results
reported in tables are mean values.
3.1. Effect of incorporated OS on sample acidity
Fig. 2 illustrates the pH variations of the coupled treatment
involving incorporated OS (m = 0.1 g L1 ) compared with plasma
treatment only.
The general behaviour of the plots pH vs. t* for plasma treatment in the presence of incorporated OS (Fig. 2A) shows a general
pH decrease by approximately one unit for standardized 30 min
treatments. The plot pH vs. t* shows a weak maximum after the
beginning of the treatment. This acid effect is much more limited
than in the case of single plasma treatment which presents a regular
pH decrease close to 3.5 pH units within 30 min exposure and may
be attributed to adding HNO3 to the solvent [11] and neutralizing
the target impurities.
The pH of samples exposed to the discharge for t* = 5 min as
standard exposure, slightly increases with the incorporated mass m
of OS (pH = 0.46 m + 5.59; r2 = 0.99; Fig. 2B) for m > 0.1 g L1 (Fig. 2B).
This feature is related to several reactions. Incorporation of the
(basic) shells to the sample induces the dissolution of the sparingly
soluble salt, CaCO3 (solubility product pKs : 8.3) according to a slow
reaction which causes a very limited pH increase (i.e., about 0.3 pH
unit at the very beginning of incorporation). Exposure to the discharge strengthens local acidity, and helps in dissolving the shells,
which neutralize the formed protons. The resulting pH turns to be
slightly more acid by about 1 pH unit for t* = 30 min with increasing t* (for a given value m = 0.1) and the medium becomes buffered
[pKa (CO2 /HCO3 ) = 6.35].
CaCO3 Ca2+ + CO3 2

Apart from these basic reactions, peroxynitrous acid and its

matching salt, peroxynitrite, react as nitrosing and nitrating agents
on double bonds and carboxylic acids, which makes them the key
agents for bacterial inactivation because of their chemical attack at
the microorganisms membranes.
3. Results and discussion
Analyses were performed in triplicate. The composition of the
samples covers a large range so that we found mandatory to apply
statistical methods to the results. The results of the plasma treatments were discussed on the basis of one-way and individual 95%
analysis of variance (ANOVA) statistical program, and this analysis

CO3 2 + H+ (+NO3 ) HCO3 (+NO3 )

HCO3 + H+ (+NO3 ) H2 CO3 (+NO3 )
H2 CO3 CO2 + H2 O
Adding various masses of powdered OS to the sample solution
and exposing to the discharge for 5 min, conrms the observed pH
evolution towards slightly lower acidities. The excess carbonate
progressively neutralizes the protons in favour of the formation of
a buffered medium, and pH slowly and linearly increases with m
for 0.1 m (g L1 ) 2.5.

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E. Njoyim-Tamungang et al. / Chemical Engineering Journal 173 (2011) 303308

Table 1
Variation of mean BOD5 with exposure time and mass of oyster shell.
Incorporated mass of oyster shell (g L1 )

t* (min)

0
5
10
15
20
25
30

0.1

0.5

1.0

1.5

2.0

2.5

716
350
98
46
25
15
16

716
99
93
75
76
69
62

716
130
95
60
45
32
25

716
120
98
51
30
25
19

716
20
35
29
28
26
28

716
80
60
35
29
24
20

716
88
68
56
47
33
29

Also, the presence of NO in discharges in air induces a huge family of reactions which were mainly detailed by Biomedical workers.
In case of discharges, the formation of transient nitrite ions was
evidenced which is the source of peroxynitrite ONOO , i.e., a transient precursor to nitrate. The carbonate ions lead to CO2 in slightly
acidic medium which partly combines with peroxynitrite ONOO
and form nitrosoperoxycarbonate ONOOCO2 which later decomposes in aqueous medium into hydrogenocarbonate and nitric acid.
H2 O + O2 NOCO2 CO3 2 + NO3 + 2H+
Peroxynitrite
is
a
strong
oxidizing
agent
E (ONOO /NO2 ) = 2.44 V/SHE and is thus involved in the
degradation process of organic pollutants and microorganisms.
3.2. Inuence of the coupled treatment on BOD5 and COD
measurements
The main parameters that must be checked for water quality,
i.e., BOD, COD and TOC were measured for various exposure times
and masses, m of incorporated shells (Table 1). They are related to
the oxidizing properties of the plasma species, the standard oxidation potential of which is higher than 1 V/SHE, while those of most
organic systems are close to 0.5 V/SHE.
All the values for m = 0 decrease with increasing t* and large
abatements (e.g., 78% and 98%) were observed for 30 min treatments, which conrms the efcacy of the mere plasma treatment.
The BOD5 data reported in Table 1 for m = 0 conrm that a mere
plasma treatment induces a large decrease in BOD values for
increasing t* and follows a pseudo 1st order kinetics with a constant kBOD ,PO = 0.15 min1 . The general behaviour of the matching
BOD vs. t* plots relevant to coupled processes (at given m) also
shows that large abatements take place in the very rst minute of
the treatments even for small m values. BOD of treated samples
behaves as a decreasing exponential function of t* for t* < 30 min in
the range of given m values: 0.1 m 2. The accuracy on data is not
sufcient to conclude with a linear evolution of log(BOD) although
it is likely.
All log (BOD) values decrease almost linearly for increasing m,
for given exposure times. The limited accuracy on data prevents
further conclusions. The dispersion of the results as well as the

large abatement observed may be attributed to post-discharge

phenomena, i.e., to reactions that develop after the discharge
has been switched off. In the present case, some BOD measurements could be performed without taking into account the time
elapsed after the plasma treatment before BOD analyses. Such
post-discharge phenomena were considered [12] and also concern
micro-organisms inactivation.
The COD values are gathered in Table 2 for various working
conditions (i.e., t* and m). The general behaviour of the logarithm
transform is a pseudo linear decrease with t* and m which takes
place for short treatments (t* 5 min) and small OS concentrations
(m 0.1 g L1 ). The evolution of log (COD) with t* of samples with
given incorporated shells, tends to follow a line with a negative
slope close to 2.5 min1 .
The observed effects of m on COD are similar to those relevant
to t*. A steep decrease in COD is observed for all the considered m
values. At given t*, log(COD) is also a linear decreasing function of
m, with a slope directly related to t*. The inuence of the key factors
t* and m may be summed up as follows: the higher m, the faster the
reaction. This correlation suggests that the charge on OS accelerates the pollutant abatement reactions, which occurs at the very
beginning of the coupled treatments. Additionally, all the COD values relevant to coupled process treatments are lower than those of
the corresponding single plasma treatment for the same exposure
time. Hence using OS in the process enhances its efcacy.
The discussion on COD results needs no further development,
because they are only indicative in cases of discharges in the air. The
transient presence of nitrite in the solution leads to an enhanced
COD value for a given plasma treatment, because NO2 is oxidized
to NO3 in the analytical process. The matching acidity increase
favours the disproportionation of NO2 in reacting NO and NO3 .
The resulting COD values actually depends on the time elapsed
between sampling and analysis of NO2 and thus cannot be unreservedly accepted.

3.3. Inuence of the coupled treatment on TOC

Total Organic Carbon is a signicant parameter which accounts
for organic pollution of aqueous efuents and its abatement is
sought by most purifying techniques. The experimental data for
Total Organic Carbon measurements of the samples are reported in

Table 2
Variation of mean COD with exposure time t* and mass m of oyster shells.
t*(min)

0
5
10
15
20
25
30

Mass of oyster shell (g L1 )

0

0.1

0.5

1.0

1.5

2.0

2.5

960.1
912.3
882.4
782.4
729.6
512.2
456.3

960.1
85
73.7
65.4
54.1
42.8
38.1

960.1
54
96.3
48.6
56.9
32.5
35.2

960.1
96.4
96
56.7
48.6
48.3
36.5

960.1
43.2
96.3
56.1
48.6
48.2
32.8

960.1
96
96.4
56.7
48.6
28
28.8

960.1
48.6
28.4
28.8
24.8
24.6
19.2

E. Njoyim-Tamungang et al. / Chemical Engineering Journal 173 (2011) 303308

307

Table 3
Mean TOC (mg L1 ) for PB treatment and exposure time, t* (min).
Time (min)

Incorporated mass of oyster shell

0

0.1

0.5

1.5

2.5

0
5
10
15
20
25
30

54.2
38.3
28.9
19.6
15.6
14.0
12.0

54.2
39.7
32.9
19.8
15.6
15.2
11.9

54.2
38.7
32.0
20.3
17.7
14.1
13.1

54.2
39.0
34.5
28.5
20.0
16.8
15.6

54.2
38.5
37.7
26.9
21.6
19.7
14.3

54.2
38.1
37.9
25.3
17.5
16.4
14.4

54.2
26.6
27.7
27.8
27.7
16.2
16.3

TOCt = t m + cst
These results suggest an interesting conclusion: a large concentration of incorporated shells slows down the process while a too
little concentration has a very limited effect on pollutant abatement. Then an optimized OS concentration will be around 12 g L1 .

60
50

TOC (mg L-1)

40
30
20
10
0

10

20
t*(min)

30

40

Fig. 3. Variation of TOC (mg L1 ) with the exposure time t* to the discharge for
mere plasma treatment. without OS (black diamonds) and for the coupled process
(m = 0.5, empty squares).

60
50

TOC (mg L-1)

Table 3. The results are affected by the exposure time t* as expected,

and by the incorporated mass m of shells, i.e., by the couple of key
factors that inuences the process. The TOC exponential decrease
with t* may be attributed to the dissolution of a main shell component CaCO3 by acid effect and the transform of CO3 2 to volatile
CO2 and to the mechanical stirring which helps evaporating the
Volatile Organic Carbons.
The plots TOC vs. t* behave as exponentially decreasing functions of t* for both treatments, with and without incorporated
shells, so that the logarithm transforms ln (TOC) = f(t*) are linear
with slopes close to 0.10 min1 .
Additionally, the coupled process plots do not largely differ from
the mere plasma treatment at rst approximation with an overall
TOC abatement by 44 mg L1 for 30 min exposure time (Fig. 3). Statistical analysis fails to show signicant differences between the
result les, but the coupled process les are distributed at slightly
higher TOC values than mere plasma treatment, which suggests
that the kinetics are slightly slower for the coupled processes. Fig. 3
is drawn for comparing the two plasma processes with an example. The coupled process treatments are thus slightly less stabilizing
than mere plasma treatment for given t*.
The TOCt* values for the coupled process at discrete exposure
times arrange along increasing lines as m increases (Fig. 4). The
relevant slopes t* are of the same order of magnitude and do not
substantially differ from 3.4 except for the plot drawn for t* = 5 min.

40
30
20
10
0
0

0.5

1.5

2.5

m (g L-1)
Fig. 4. Inuence of the mass m (g L1 ) of OS on TOC (mg L1 ). Mere plasma treatment (m = 0): lled diamonds. Coupled treatments: empty squares (t* = 5); triangles
(t* = 10); lled squares (t* = 25).

4. Conclusion
This study has shown that coupling a cold plasma treatment at
atmospheric pressure with incorporating OS as cheap solid adsorbents and acidity controller allowed the removal of organic wastes
in surface waters with similar efcacy to plasma treatment alone.
The oxidizing species OH and NO formed in the discharge are
directly or indirectly (through their derivatives) responsible for
the waste degradation. The salient results provided by this study
demonstrated that:

- The removal of domestic and industrial wastes from surface

waters may be performed by both plasma treatments alone and
the coupled process involving adsorption on unemployed powdered oyster shells. The coupling technique may thus be an
interesting way for enhancing the value of these special solid
wastes.
- The resulting efcacy of the coupling process is similar to that
of single plasma treatments. A pollutant abatement by 50% is
obtained for 10 min treatments in batch conditions.
- The process requires limited masses of OS powder (less than
2 g L1 ) and short exposure times to the discharge (around
510 min) in batch reactors.
- The mechanism for pollutant abatement TOC = f(t*) is close to an
overall 1st-order kinetic law (k 3 min1 ).
- The coupled processes also induce large COD and BOD abatements, The coupled Process is cheap and easy to operate; it may
be easily developed for further application at industrial scale. The
good results of the coupled process may be attributed to the limited decreasing pH and associated to buffer effects which accounts
for the acidbase reaction between the treated liquid sample
and the incorporated basic solid and to its adsorption properties
which enables concentration of the pollutants.

308

E. Njoyim-Tamungang et al. / Chemical Engineering Journal 173 (2011) 303308

The coupling technique is an interesting way of enhancing the

value of these special solid wastes and particularly for controlling the pH of the processed efuents to about 6 before release.
Special attention was devoted to an industrial sample due to its
heavy organic load. Mean pollutant abatements close to 50% are
obtained for 10 min treatments in batch conditions. Fullment of
COD and BOD standard regulations (COD < 150; BOD5 < 30 mg L1 )
requires short exposures times and small m values (e.g., t* = 5 min;
m = 0.5 g L1 ) which could still be reduced by using a circulating
mode. The overall kinetic law for TOC abatement, i.e., TOC = f(t*)
is close to 1st-order (k 3 min1 ) and depends little on m for
given t*.
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