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Volume 1, Numero 1, Avril 2015

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An International Research Journal Of Environmental Science And Technology

ENVIRONMENTAL SCIENCE AND TECHNOLOGY

Copyright © 2015, Algerian Journal of Environmental Science and Technology, All rights reserved

University of Boumerdes Faculty of engineering

Research Laboratory of Food Technology

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Table Of Contents

- Etude du potentiel d’utilisation des déchets agroalimentaires, les grignons d’olives et les noyaux de date pour récupération et adsorption des métaux lourds N. Babakhoya, S. Boughrara, F. Abed, N. Abai, S. Midoune ………………………………..

pp 04/10

- Biodegradation of diclofenac by activated sludge and membrane bioreactor-A review D. Cherik, K. Louhab ………………………………………………………………………

pp 11/17

- Contribution of Anhydrous Milk Fat to environmental impacts generated by the dairy processing F. Younsi . …………………………………………………………………………………..

pp 18/22

- Toxic effect of surfactants on marine species Mediterranean mussel: Mytilus gallprovinciallis and evaluation of their aquatic toxicology impact by LCA methodology M. Belkhir. S. Boughrara. H. Boutiche ……………………………………………………

pp 23/29

- Reaction in water under microwave: rapid and convenient synthesis of N-hydroxymethylimides and N-hydroxymethyl lactams M. Hachemi ………………………………………………………………………………...

pp 30/32

- Study of dispersion of brine water into coastal seawater by using a pilot L. habet, K. benrachedi …………………………………………………………………….

pp 33/39

Algerian Journal of Environmental Science and Technology Volume 01, Numéro 01, (2015), ISSN: 2437-1114

Algerian Journal of Environmental Science and Technology

Avril edition. Vol.1. No1. (2015) ISSN : 2437-1114 www.aljest.webs.com

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Pr. AFFOUNE A.M. (Univ. Guelma, Algeria)

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Pr. BENRACHEDI K. (Univ. Boumerdes, Algeria)

Pr. BOUTALEB A. (Univ Houari Boumediene/USTHB, Algeria)

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Pr. KHEIRDDINE H. (Univ. Bejaia, Algeria)

Pr. MOHAMMEDI K. (Univ. Boumerdes, Algeria)

Pr. SELATNIA A. (The National Polytechnic School, Algeria)

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Dr. NOUANI A. (Univ. Boumerdes, Algeria)





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Algerian Journal of Environmental Science and Technology Avril edition. Vol.1. N

o1. (2015)

ISSN : 2437-1114

www.aljest.webs.com ALJEST


Etude du potentiel d’utilisation des déchets agroalimentaires, les grignons d’olives et les noyaux de date pour récupération

et adsorption des métaux lourds

N. Babakhouya(1,2), S. Boughrara(1), F. Abed(1), N. Abai(1), S. Midoune(2)

1) Laboratoire de Recherche en Technologie Alimentaire Faculté des Sciences de l’Ingénieur Université de Boumerdes 35000-Boumerdes, Algérie

2) Centre de recherche scientifique et technique en analyses physico-chimiques

*Corresponding author: [email protected]

ARTICLE INFO ABSTRACT/RESUME

Article History:

Received : 11/01/2015

Accepted : 15/03/2015

La présente étude porte sur l’application d’un adsorbant naturel

préparé à base de grignon d’olives et de noyaux de dattes à différents

pourcentages dans le domaine de traitement des effluents liquides

industriels. Dans notre travail nous nous sommes intéressés à son

application pour le cadmium (métal lourd). L’effet de plusieurs

paramètres tel que le temps de contact, la concentration initiale en

ions de cadmium, et le pH de la solution a été étudié en système en

batch. Une modélisation des isothermes d’adsorption a été effectuée à

l’aide des models d’isothermes de Langmuir, Freundlich et Temkin et

leur coefficient de corrélation obtenus, indiquent que le model de

Langmuir est favorable pour la plupart des proportions d’adsorbants.

Key Words:

valorisation,

grignon d’olive,

noyau de dattes,

adsorption,

modélisation

I. Introduction

Les métaux lourds d’origine naturelle ou bien

provenant des rejets industriels sont toxiques pour

les êtres humains et autres organismes vivants à des

concentrations élevées [1].

L’élimination des ions de cadmium des eaux usées

industrielles est l’un des problèmes importants qui

doivent être résolues car il est considéré comme

l’un des métaux toxiques s’accumulant lentement

dans les organismes vivants provenant de la chaîne

alimentaire [2] et qui a plusieurs effets nocifs sur la

santé humaine tel que : les lésions rénales,

l’hypertension, la proteinure…etc.

Des processus physiques et chimiques ont été

largement étudiés pour éliminer les métaux lourds,

polluants des eaux usées à des concentrations

élevées.

Certains de ces processus sont : la coagulation, la

flottation, la précipitation chimique et l’adsorption.

Cette dernière peut être considérée comme une

méthode efficace et économique pour l’élimination

des métaux lourds à de faibles concentrations.

Au cours des dernières années, diverses études ont

démontré le potentiel de divers adsorbants naturels

pour la récupération des métaux lourds en solution

[3, 4].

Ainsi des travaux de recherche ont, entre autres,

porté sur la capacité de fixation des métaux sur des

écailles d’arachides [5], des écailles de cacao [6],

des noix de coco [7], des grignons d’olives et des

noyaux de dattes [8,9]

Les déchets de grignon d’olives et de noyaux de

dattes ont été largement utilisés comme charbon

actif [10, 11]. Bien que le charbon actif obtenu a été

signalé comme étant adsorbant, le coût du

traitement pour l’obtenir est élevé, ce qui le rend

non concurrentiel du point de vue économique.

Aussi, l’utilisation des grignons d’olives et des

noyaux de dattes dans leur forme native n’a pas

donné des résultats satisfaisants [12, 13]

En s’inspirant de l’idée d’alliage des métaux on a

procédé donc au mélange entre les deux matériaux.

Notre travail est essentiellement axé sur l’étude des

isothermes d’adsorption par des models

d’isothermes de Langmuir, Freundlich et Temkin

tout en étudiant l’effet de certains paramètres tel

que : le temps de contact, la concentration initiale

en ions de cadmium, le pH de la solution et la

température, à fin de valoriser la solution solide

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N. Babakhouya et al


préparée à base de grignons d’olive et de noyaux de

dattes.

II. Matériel et méthodes

II.1. Préparation de la matière première

Les grignons d’olives utilisés dans cette étude ont

été prélevés au niveau de la région de Beni Amrane

– Boumerdès – Algérie, durant la période oléicole

2006-2007. L’échantillon prélevé est constitué de

pulpes et de fragments de noyaux. Il a été

conditionné dans des sacs en plastique. Pour les

noyaux de dattes, ceux utilisés dans notre étude ont

été prélevés au niveau de la région de Ouêrgla –

Algérie.

Les grignons d’olive ainsi que les noyaux de dattes

sont d’abord lavés plusieurs fois à l’eau courante

afin d’éliminer toute sorte de poussières ou

d’impuretés adhérentes, puis à l’eau distillée. Ils

sont ensuite épuisés par de l’hexane pour éliminer

l’huile résiduel. La matière première ainsi lavée et

séchée subit un broyage grossier avec un broyeur

électrique

Une fois broyé, chacun des deux matériaux subit un

tamisage grâce à une pile de tamis de laboratoire de

différentes ouvertures de maille (200 µ à1000 µ)

Le choix de la granulométrie désirée est compris

entre 500µ et 1000µ. On procède à la préparation

des différents échantillons avant de passer à l’étape

de traitement chimique. Pour cela on mélange les

deux matériaux à des pourcentages variant comme

indiqué dans le tableau 1

On fait subir à chacun de ces mélanges une

activation chimique au moyen d’une solution

aqueuse d’acides phosphorique (3N) à un rapport

massique égal à 2g d’acide/g de matériaux, pendant

3 heures. La température de la solution est

maintenue à environ 100°C avec un reflux total des

vapeurs. Après traitement, le solide est séparé par

filtration simple, lavé plusieurs fois avec de l’eau

distillée à chaud pour éliminer les phosphates

résiduels jusqu’à stabilisation du pH de la solution

d’épuisement à une valeur neutre et enfin séché à

105C° jusqu’à poids constant.

Tableau 1 : différents pourcentage de grignon d’olive et de noyau de dattes mélangés

N0 d’échantillon quantité de grignon d’olive quantité de noyau de dattes

Mélangé en % Mélangé en %

1 0 100

2 10 90

3 90 10

4 100 0

On fait subir à chacun de ces mélanges une

activation chimique au moyen d’une solution

aqueuse d’acides phosphorique (3N) à un rapport

massique égal à 2g d’acide/g de matériaux,

pendant 3 heures. La température de la solution

est maintenue à environ 100°C avec un reflux

total des vapeurs. Après traitement, le solide est

séparé par filtration simple, lavé plusieurs fois

avec de l’eau distillée à chaud pour éliminer les

phosphates résiduels jusqu’à stabilisation du pH

de la solution d’épuisement à une valeur neutre et

enfin séché à 105C° jusqu’à poids constant

II.2. Caractérisation des adsorbants à

différentes proportions préparés

II.2.1. Analyse structurale par spectroscopie

FTIR

La spectroscopie IR est l’une des méthodes

spectrales. Elle permet l’identification des

groupements fonctionnels.

Les analyses de spectroscopie I.R ont été effectuées

au niveau de laboratoire de la faculté des sciences,

université de Boumerdès à l’aide d’un spectromètre

à transformée de Fourrier de type ‘’Nicolet 560

FTIR’’couplé à un calculateur digital permettant le

tracé des spectres entre [4000 et 400 cm -1

].

II.2.2. Essais d’adsorption du cadmium

II.2.2.1. Influence du temps de contact sur la

capacité d’adsorption du Cadmium:

Les essais sont réalisés en batch à température

ambiante dans des béchers, par agitation (au moyen

d’un agitateur magnétique) d’une masse fixe de

0.2g d’adsorbant dans un volume de 15 ml de la

solution de métal à 350 tr/min jusqu’à que

l’équilibre est atteint. La concentration de la

solution synthétique du cadmium était d’environ 17

mg/l et le pH initial est de 5.6. Les échantillons sont

prélevés à des intervalles de temps prédéterminés et

sont séparés du solide par filtration sur un papier

filtre en cellulose de 0.45 µm de diamètre pour

l’analyse de la concentration du métal qui est

effectuée par spectroscopie d’absorption atomique

(SAA).

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La quantité du métal adsorbé par le poids sec

d’adsorbant est calculée comme suit :

Qt = (Ci – Ct) × V / M

Où :

V : est le volume de la solution en (L).

Ci et Ct : sont respectivement, la concentration du

métal à « t » initial et à l’instant « t » en (mg/ l).

M : est le poids sec d’adsorbant en (g).

II.2.2.2. Influence de la concentration initiale en

métal L’effet de la concentration initiale en métal a été

étudié par la même procédure que précédemment en

variant la concentration initiale entre 17 mg//l et

81.85 mg/l et en fixant le temps de contact à

120mn. Le pH initial est de l’ordre de 5.6

II.2.2.3. Modélisation des isothermes

d’adsorption

Nous avons étudié les isothermes d’adsorption du

Cadmium sur les différents adsorbants à l’aide des

models simples à savoir le model de Langmuir et le

model de Freundlich ainsi que le model de Temkin.

II.2.2.4. Influence du pH

Les essais sont réalisés en batch à température

ambiante dans des béchers, par agitation (au moyen

d’un agitateur magnétique) à 350 tr/min d’une

masse fixe de 0.2g d’adsorbant dans un volume de

15 ml de la solution synthétique du cadmium à une

concentration de 17mg/l jusqu’à que l’équilibre est

atteint après un temps prédéterminé de 120mn. Le

pH initial est ajusté au moyen des solutions de

NaOH (1N) et HCl (0.1N), pour les différentes

valeurs de pH étudiées (2, 3, 4, 5, 6, 7 et 9).

III. RÉSULTAT ET DISCUSSION

III.1. Caractérisation des adsorbants à

différentes proportions préparés

Après avoir obtenu les adsorbants à différentes

proportions, on procède à leur caractérisation par

Analyse structurale par spectroscopie FT I R. Les

spectres d’analyse par IR obtenus sur les différents

adsorbants montre la présence de différentes

bandes de vibrations correspondant aux

groupements hydroxyles C-N, C=O, C-H,

-COOH, N-H… (Tableau 3).

Ces résultats nous permettent de conclure que les

ions métalliques vont se lier aux adsorbants par des

interactions avec les groupements actifs OH et -

COOH

Figure 1 : spectre IR de 100% NDN (1) et 100%

NDI (2)

Figure 2 : spectre IR de 100% GON (1) et 100%

GOI (2)

Figure 3 : spectre IR de 50% GON (1) et 50%

GOI (2)

III.2. Influence du temps de contact sur la

capacité d’adsorption du Cadmium

6

N. Babakhouya et al


Le temps de contact choisis était entre 10 et

420min à une température ambiante de 20°C. Le

pH initial mesuré était de 5.6 et il a été maintenu

constant durant tout l’essai. La concentration

d’adsorbant était de 17mg/l.

D’après les figures 8et 9 on constate que

l’adsorption du Cd (II) par les différents adsorbants

était initialement faible et l’équilibre pour les

différentes concentrations était atteint après 60min.

Donc le temps de contact de 120min était considéré

comme un temps idéal pour la rétention du Cd(II)

sur les différents adsorbants.

La cinétique d’adsorption était initialement très

rapide, ce qui peut être expliqué par la disponibilité

des sites actifs sur la surface des différents

adsorbants. Ensuite elle est devenue plus lente

jusqu’à atteindre l’équilibre et cela peut être dû à la

diminution de la surface de contact après

occupation de la majorité des sites actifs par les

ions de Cd(II) et donc les ions restant en solution

deviennent concurrents entre eux mêmes.

En comparant entre les proportions d’adsorbants à

l’état natif et ceux traités chimiquement on constate

que les quantités maximale adsorbée était obtenu

dans le cas des proportion à l’état natif mais on ne

peut pas se baser sur ces résultats vue que les

adsorbants ont une forme hétérogène et des

caractéristiques instables dépendant de l’origine la

période de récolte et le temps de stockage de la

matière première alors que le traitement chimique

permet d’avoir une structure homogène et des

caractéristiques stables. Aussi on peut noter l’effet

du mélange sur l’amélioration de la capacité

d’adsorption qui est nettement remarqué dans le cas

des proportions d’adsorbants traités chimiquement.

Figure 4 : Capacité d’adsorption du cadmium en

fonction du temps de contact (adsorbant à l’état

natif) (Co=17mg/l, pH =5.5, T°=20°C, w = 350 tr/

mn).

Figure 5 : Capacité d’adsorption du cadmium en

fonction du temps de contact (adsorbant à l’état

imprégné) (Co=17mg/l, pH =5.5, T°=20°C, w =

350 tr/ mn).

III.3.Influence de la concentration initiale en

métal

Les résultats présentés par les figures 10 et 11

indiquent qu’avec l’augmentation de la

concentration initiale en Cd(II), le pourcentage de

réduction de cet ion métallique diminue alors que

sa quantité adsorbée par unité de masse d’adsorbant

(qe) augmente. L’augmentation de la capacité

d’adsorption avec l’augmentation de la

concentration initiale en ions de Cd (II) peut être

due à l’augmentation de la surface spécifique

d’adsorption. D’après les résultats obtenus dans le

cas d’adsorbant non traités chimiquement on

constate que le mélange des deux adsorbants

permet d’améliorer leur capacité adsorptive,

Figure 6 : Isothermes d’adsorption du cadmium

sur des adsorbants à l’état natif.(T° = 20°C, t =

120 mn, w = 350tr/mn, pH = 5.5).

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Figure 7 : Isothermes d’adsorption du cadmium sur des adsorbants à l’état imprégné

(T° = 20°C, t = 120 mn, w = 350tr/mn, pH = 5.5)

III.4. Modélisation des isothermes d’adsorption

L’isotherme obtenue est du type L correspondant

à une adsorption d’une couche monomoléculaire,

d’où la possibilité d’appliquer aussi bien la loi de

Langmuir que celle de Freundlich. Les paramètres

d’isothermes de Langmuir, de Freundlich et de

Temkin sont calculés de la même manière que les

travaux de recherches cités dans la littérature

[15,16]. Les paramètres de Langmuir, Freundlich et

Temkin sont récapitulés dans le tableau 3

III.5. Influence du pH

Le pH joue un rôle important dans le processus

d’adsorption, en particulier sur la capacité

d’adsorption. Les figures 40 et 41 nous montre

l’effet du pH sur l’adsorption du cadmium. On

constate d’après ces deux figures que la capacité

d’adsorption pour les différents types d’adsorbants

augmente avec l’augmentation du pH de la

solution. Les résultats montrent que le pH acide est

défavorable pour l’adsorption des ions de

cadmium. Ces résultats corroborent les travaux

menés par Francesca Pagnanelli et al [8] qui ont

fait l’étude de la biosorption des métaux sur un

déchet d’agriculture, le grignon d’olive.

A pH acide, la charge positive domine la surface de

l’adsorbant. Ainsi, une répulsion électrostatique

sensiblement élevée existe entre les charges

positives de la surface de l’adsorbant causées par

les protons H+ et les charges positives du cadmium

[12,14]. Entre pH 5 et 7 on remarque une

augmentation en capacité d’adsorption des ions

métalliques ce qui peut être expliqué par la

dissociation des sites actif sur la surface de

l’adsorbant et qui deviennent chargés négativement

ce qui cause l’attraction des métaux chargés

positivement présents dans la solution. Au delà du

pH 7 on constate une diminution de capacité de

rétention du cadmium due à la précipitation des

ions de cadmium sous forme de Cd (OH)2. Aussi

on constate que le mélange des deux adsorbants

permet l’amélioration de leur capacité adsorptive.

IV. Conclusion

Notre travail a montré que Le mélange entre les

deux matériaux au moyen d’un traitement chimique

par l’acide phosphorique (H3PO4) a permis de créer

une nouvelle solution solide homogène avec des

caractéristiques adsorptives plus performantes.

L’étude de l’adsorption en système batch, nous a

permis de constater que l’élimination du Cadmium

par les différents proportions d’adsorbants, est

meilleure aux pH compris entre 5 et 7, la capacité

maximale d’adsorption est notée dans le cas du

mélange d’une petite fraction de grignon d’olive

avec les noyaux de dattes (90% de noyau de dattes

et 10% de grignon d’olive). L’isotherme de

Langmuir ainsi que l’isotherme de Freundlich sont

favorable pour l’adsorption du Cadmium sur les

différentes proportions d’adsorbants alors que

l’isotherme de Temkin n’a pas donné des résultats

fiables que pour les échantillons à l’état naturel

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N. Babakhouya et al


Figure 8 : Effet du pH sur l’adsorption du

Cadmium sur des adsorbants à l’état natif

(Co=17mg/l, t = 120 mn, w = 350tr/mn, T°=20°C)

Figure 9 : Effet du pH sur l’adsorption du

Cadmium sur des adsorbants à l’état imprégné

(Co=17mg/l, t = 120 mn, w = 350tr/mn, T°=20°C)

Tableau 3 : Paramètres de Langmuir, Freundlich et Temkin pour les différents types d’adsorbants utilisés

V. Références bibliographiques

1. Yakup Arica, M., Tuzun, I., Yalçin, E., Ince, O.,

Bayramoglu, G., 2005. Utilisation of native, heat and acid-

treated microalgae Chlamydomonas reinhardtii

preparations for biosorption of Cr(VI) ions. Process. Biochem. 40. 2351-2358

2. Srivastava, V. C., Mall, I. D., Mishra, I. M., 2006.

Characterisation of mesoporous rice hus ash (RHA) and adsorption kinetics of metal ions from aqueous solution

onto RHA. J. Hazard. Mater. 134 (1-3). 257-267. 3. Bailey, S. E., Olin, T. J., Bricka, R. M., et Adrian, D. D.

1999. A Review of potentially low-cost sorbent for heavy

metals. Water Res. 33 : 2469-2479. 4. Fiset,J. F., Ben Cheikh, R., et Tyagi, R. D. 2000. Revue sur

l’enlevement des métaux des effluent par adsorption sur les

5. sciures et les écorces de bois. Rev. Sci. Eau, 13(3) : 323-

347.

6. Randall, J. M., et Hautala,E. 1975. Removal of heavy metal ions from waste solutions y contact with agricultural by

products. Proc. Ind. Waste conf. 30 : 412-422.

7. Fiset, J. F., Tyagi, R. D., et Blais, J. F. 2002. Cocoa shells as adsorents for metal recovery from acid effluent. Water

Pollut. Res. J. Can. 37(2) : 379-388.

8. Bosinco, S., Roussy, J, Guibal, E., et Lecloirec, P. 1996. Interaction mecanisms etween hexavalent chromium and

cornocob. Environ. Technol. 17 : 55-62.

9. Pagnanelli, F., Mainelli, S., Veglio, F., Toro, L., 2003. « Heavy metal removal by olive pomace: biosorbent

types d'adsorbants

Paramètres de Langmuir Paramètres de Freundlich paramètres de Temkin

qm (mg/g)

b R2 RLx 10

4 KF 1/n R

2 aT bT R2

100% NDN 0,589 6,089 0,9731 20,025 0,876 0.368 0,9945 2,148 3544,229 0,9544

100% GON 3,199 0.996 0,9464 121,179 1,708 0.187 0,9561 90,377 6372,199 0,9824

90% GON 2,361 1,309 0,7587 92,471 1,684 0.107 0,3761 101,19 7312,83 0,937

10% GON 2,072 1,598 0,9196 75,875 1,518 0.222 0,9744 37,713 5768,914 0,9925

100%NDI 0,486 9,633 0,9021 12,667 0,957 0.378 0,7847 3,221 3578,573 0,7274

100%GOI 0,575 6,769 0,9783 18,017 0,961 0.352 0,9194 3,117 3769,512 0,8791

90%GOI 1,41 2,47 0,9763 49,226 1,539 0.217 0,8207 17,601 4801,746 0,8363

10%GOI 1.266 2,578 0,986 47,158 1,32 0.250 0,9953 8,281 4465,677 0,9928

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characterisation and equilibrium modelling». Chemical

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Please cite this Article as: Babakhouya, N., Boughrara, S., Abed, F., Abai, N., Midoune, S., Etude du potentiel d’utilisation des déchets agroalimentaires, les grignons d’olives et les noyaux de date pour

récupération et adsorption des métaux lourds, Algerian J. Env. Sc. Technology, 1:1 (2015) 4-10

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Biodegradation of diclofenac by activated sludge and membrane bioreactor-A review

D. Cherik, K. Louhab

Laboratory of Alimentary Technology, Faculty of Engineering Sciences,

University of Boumerdes, Boumerdes 35000, Algeria


ARTICLE INFO ABSTRACT

Article History:

Received : 01/01/2015

Accepted : 25/04/2015

Diclofenac (DCF) is a pharmaceutical residue of therapeutic class of

non-steroidal anti-inflammatory which is often detected in the

wastewater treatment plants (influent and effluent) and surface waters.

This review focuses its elimination by biodegradation with activated

sludge (CAS) or bioreactor membrane (MBR) in which

microorganisms plays a key role in the elimination of diclofenac and in

which a lot of factors can affect the efficiency of the removal as

physicochemical properties of diclofenac, sludge retention time (SRT),

temperature, pH, redox conditions and sludge characteristics.The

objective of this study was to describe a review of the literature by

recent publications on the biodegradation of diclofenac. We inspect the

performance of biodegradation using biological process technology by

activated sludge and membrane bioreactor in the elimination of

diclofenac.

Key Words:

Biodegradation,

Membrane bioreactor,

Conventional activated

sludge,

Bacterial community

I. Introduction

Diclofenac (DCF), a polycyclic non-steroidal anti-

inflammatory drug [1- 3] is one of the most

extensively studied pharmaceuticals, for his

potential toxic effects on no-target organisms [4].

Diclofenac was detected in wastewater [5, 6] in a

number of countries such as China [7, 8], Serbia

[9], Spain [10, 11, and 12], Greece [13, 14],

Portugal [15, 16], Brazil [17], USA [18] and South

Africa [19]. According to published documents, the

concentrations of this drug varied in a range from

0.01 to 8.5μg/l [20, 21] and the rate of his

elimination in sewage treatment plants is low (up to

40%) [22, 23]. Table 1 presents physicochemical

properties and molecular structure of Diclofenac. It

was considered very toxic anti-inflammatory due to

the death of birds recorded shortly after scanning

the infected farm in India and Pakistan [24, 25]; he

centre de recherche scientifique et technique en analyses physico-chimiques showed potential influence of

endocrine disruption by delaying and reducing the

success of fish eggs and hatching low

concentrations damage the digestive organs [25].

Sewage treatment plays an important part in

removing contaminants from reclaimed water but

it’s known that conventional wastewater treatment

plants (WWTP) do not remove all the pollutants

[26], especially the persistent polar pollutants due

to their physicochemical properties such as

diclofenac [27, 28, 29]. Most treatment methods of

pharmaceuticals wastewater are biological

processes [30, 14 and 31] in which microorganisms

such as ammonia-oxidizing bacteria for the removal

of ammonium [32], Escherichia coli [33] and

nitrite-oxidizing bacteria [34] are applied for

removal of organic contaminants [35, 25, and 36].

Most WWTPs used are activated sludge processes

[37, 38] and membrane bioreactors [39, 40, and

24]. Biodegradation by these two processes can be

influenced by various factors namely; the

physicochemical properties of diclofenac [41], the

biological operating conditions (sludge retention

time, temperature, pH and redox conditions) [42-

44, 45] and sludge characteristics [46, 47]. In this

context, this study is a literature review of recent

publications and studies to full and small scale on

biodegradation of diclofenac to study the

performance of activated sludge and membrane

bioreactor in the elimination of diclofenac.

11


D. Cherik et al


Table 1: Main characteristics of diclofenac

Structure a Molecular weight (g/mol)a Log KOW a, b pKa a

296.14

0.7-4.51

4.15

a : [48], b: [49]

II. Biodegradation of diclofenac

Biodegradation is the process most usually used to

eliminate the pharmaceutical residues persistent as

the diclofenac [50, 51 and 52, 53]. This process

decomposes and mineralizes these pollutants by

bacteria or mushrooms in simpler compounds [47,

54]. Diclofenac is a polar pharmaceutical

compound mostly used as the sodium salt

diclofenac-Na in human and veterinary medicine to

reduce inflammation and pain [5, 17 and 55]. Many

studies have evaluated the biodegradation of

diclofenac by conventional activated sludge and

membrane bioreactors.

2.1 Conventional activated sludge

Microbial degradation of diclofenac by activated

sludge does not lead to its complete elimination but

produces other metabolites which are also

considered such as pollutants [56], these authors

investigated the repartition of diclofenac in

activated sludge, they detected 7 diclofenac

transformation products among them 1-(2,6-

dichlorophenyl)-1,3-dihydro-2H-indol-2-one and

2,3-dichloro-N-(phenyl)aniline. The fungus

Trametes versicolor can be utilized in activated

sludge for the elimination of diclofenac [57], in this

study the removal rate was 64% which leads to a

production of less toxic sludge, these authors

concluded that fungal process can be an effective

mean for biodegradation and diclofenac reduction

in polluted waters. Activated sludge is the most

used in the biological treatment and the rate of

elimination of diclofenac by this process was

insignificant and does not exceed 50 % [6, 43, 58,

59, 60, 61, 62 and 63]. Biodegradation of

diclofenac can be estimated on measuring COD

(Chemical Oxygen Demand) in polluted water and

treated water [64], [60] have illuminated this point

and studied the elimination of diclofenac by

activated sludge suspended in 2 reactors; ASR1 and

ASR2. The removal rate was 48±19% and the

concentrations of DCO decreased from 976±39

mg/l and 707±14 mg/l to 47±48 mg/l and 54±55

mg/l in ASR1 and ASR2, respectively. The

hydrophobicity property defines the compound

when the latter is insoluble in water [47], [65]

studied the effect of the molecular features of

diclofenac in activated sludge in lab-scale

experimental; they confirm that the functional

groups can influenced the biodegradability. Among

the biological process conditions; the sludge

retention time SRT which may have an effect on the

biodegradation and also affects microbial activity

[29], [51] evaluated the biodegradation of

diclofenac in activated sludge of two wastewater

treatment plants, Mamer and Boevange which

differed in size, layout and sludge retention time

(SRT). They observed that the biological

degradation of diclofenac was significantly better in

sludge from WWTP Mamer compared to sludge

from WWTP Boevange and the removal rate

decreases with increasing of SRT due to a lower

active biomass presence. [66] reported the influence

of SRT on diclofenac removal for more than seven

months in denitrifying semi-continuous reactors

operated at 10, 20, and 40 days by using two culture

series (diclofenac free-control and diclofenac-

acclimated); the results showed that the elimination

rate for diclofenac-acclimated culture was lower

than 15% a nitrate removal rate increased with

increasing SRT but for diclofenac free-control this

rate decreases with increasing SRT at 10, 20, 40

days with 48, 63, 79 mg NO-3-N/L day and 122, 55,

54 mg NO-3-N/L day, respectively. [67]

investigated the biodegradation of diclofenac by

nitrifying activated sludge and established the no

removal of diclofenac with this process, these

results are consistent with those of [68] who have

studied the removal of diclofenac by nitrifying

activated sludge in large scale (WWTP) and small

scale (laboratory level) at a temperature of 12°C,

the authors found that diclofenac is not

biodegradable in large scale and the reaction rate

constant (k′) and biodegradation constant (kbiol)

were 1.7 d-1

and 0.6 l gss-1

d-1

, respectively in

WWTP. In laboratory scale the biodegradation rate

showed a difference between the reactors where

with 10ug / l of diclofenac the biodegradation rate

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was 86% in the reactor 1, whereas in the other

reactors was 90%. The authors explained this

difference by the amount of active nitrifying

bacteria in the reactors which was influenced by

temperature. [69] studied the removal of diclofenac

in two lab-scale conventional activated sludge

reactors under nitrifying (aerobic) and denitrifying

(anoxic) conditions for more than 1.5 years, they

found that the removal by the biological treatment

with nitrifying or denitrifying bacteria was not

significant (<25%). Diclofenac in anoxic conditions

(kbiol< 0.04 Lgss-1

d-1

) is persistent with respect to

aerobic conditions (kbiol= 1.2 Lgss-1

d-1

) [69]. [65]

found a similar partition coefficient (kd) under

aerobic and anoxic conditions (0.319 and 0.303

L.gSS-1

, respectively).

Sludge characteristics may influence the sorption

diclofenac. These characteristics vary depending on

the operation of treatment plants as activated sludge

[70]. [71] Studied the biodegradability of the

diclofenac on two types of sludge; sterilized and

activated. Results of batch adsorption experiments

via sterilized sludge showed that the removal

efficiency was 40.1% at 6 hours and 19.7% for

activated sludge where the contributions of sludge

adsorption and biodegradation were 14.9% at 6

hours and 4.8%, respectively, The authors

suggested that this difference in removal efficiency

by sterilized and activated sludge is due probably

by the sterilizing effect of the activated sludge

which can be caused changes in the characteristics

of the sludge and improves the elimination of

diclofenac and also suggested that the structure of

diclofenac (the electronic withdrawing groups)

namely its functional groups (amine, halogen, and

carboxylic groups) causes the resistance of

diclofenac in its biodegradation.

2.2 Membranes bioreactors

Recently, the membrane bioreactor process has

become the most effective process for the removal

of diclofenac compared to activated sludge [72],

where the authors have demonstrated that the

removal rate of diclofenac by membrane bioreactor

process was 65%. The molecular features of

diclofenac can affect the rate of his elimination by

membrane bioreactor on the scale of laboratory

[73]. In this study, the authors observed a very low

rate of elimination (17 %) and they justified this

behavior of diclofenac in the MBR system by the

presence of chlorine group and also the electron

withdrawing functional groups generates an

electron deficiency[74] investigated the degradation

of diclofenac by a white-rot fungus-augmented

membrane bioreactor (MBR) with and without

addition of a redox mediator (1-hydroxy

benzotriazole, HBT); the results showed that the

addition of a redox mediator (1-hydroxy

benzotriazole, HBT) improve the removal

efficiency of diclofenac from 70% to 95%. On the

other hand anaerobic MBR system has not shown

an effective elimination rate for diclofenac (<10%)

[75], these results are consistent with those of [76]

these authors worked on a process of anaerobic /

anoxic / aerobic membrane bioreactor in a large

scale and observed removal rate below 20% for

diclofenac. The full-scale MBR showed

significantly better removal of hydrophilic

compound (log D < 3) [77]; they explained the

greater removal by the existence of preand post-

anoxic tanks and the combination of aerobic zones

with different levels of DO (Dissolved Oxygen)

relative to a pre-anoxic and one aerobic tank in the

pilot MBR. In contrast in another study [28] where

they used an anaerobic system by anaerobic

fluidized membrane bioreactor (AFMBR) using

granular activated carbon (GAC) as carrier medium,

78% was the removal rate of diclofenac and the

elimination rate of COD was 95% at total HRT of 5

h. It can be concluded that the use of GAC helps

eliminate diclofenac in the anaerobic system. In

non-sterile conditions studied by [72] the removal

rate of diclofenac was 55% in an MBR system with

a hydraulic retention time of two days [78] have

shown that increasing the biomass concentration in

the MBR system due to the long retention time

favors the elimination of diclofenac and can be

influenced by microbial activity according to [79].

These authors found that the reduction of microbial

activity in the MBR system induces a decrease in

the rate of elimination of diclofenac which indicates

that the latter is eliminated by biological

degradation and not by the sorption process only.

[80] investigated the elimination of diclofenac by

MBR under different temperature (10-45°C) in

laboratory-scale and demonstrated that the

temperature has an effect on the microbial activity.

The results showed that the maximum and

minimum removal rate were at 10 ° C and 20°C,

respectively.

As regards the influence of pH, [81] explain the

relationship between physicochemical properties of

diclofenac and his efficiency removal by a

laboratory scale MBR at mixed liquor pH values of

5, 6, 7, 8, and 9. At pH 5 the rate of removal was

highest; this result is due to the physicochemical

properties of this ionisable compound under acidic

conditions wherein the pKa value is 4.15 [82] so at

pH 5 diclofenac is neutral which makes it a

hydrophobic compound. The increase of the made

pH decreases log D and consequently the

hydrophobicity of diclofenac what makes decrease

also the efficiency elimination. [83] confirmed the

11 13

D. Cherik et al


results found by [81] with their study where they

assessed the biotransformation of diclofenac by

laccase in an enzymatic membrane reactor, DCF

biodegradation was better at acidic pH (3 and 4.5),

and decreased with increasing pH.

3. Conclusion

The elimination of diclofenac was demonstrated to

large and small scale with two process treatment of

polluted water; biological process or biodegradation

using conventional activated sludge (CAS) and

membrane bioreactor (MBR) where the

microorganisms are responsible for its degradation.

Discussion of studies and publications used in this

review demonstrated that biodegradation by

membrane bioreactor is the most effective process

for the removal of a resistant and persistent

contaminant such as diclofenac with complete

retention of suspended solids, thus reducing

emissions to the dissolved fractions, but this

removal may be influenced by various factors:

Chemical structure where the presence of

chlorine group and functional groups can

influence the biodegradability of diclofenac.

Sludge retention time (SRT) where the increase

in this factor increasing the biomass

concentration and therefore improves

elimination of diclofenac.

The temperature can affect the microbial

activity in sludge and the maximum removal of

diclofenac was seen at low temperatures.

At acidic pH eliminating diclofenac was

considered very favorable where the

Hydrophobicity plays a very important role.

Redox conditions: aerobic conditions in the

elimination of diclofenac were better compared

to the other conditions.

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A review, , Algerian J. Env. Sc. Technology, 1:1 (2015) 11-17

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Contribution of Anhydrous Milk Fat to environmental impacts generated by the dairy processing

F. Younsi

Food Technology Research Laboratory, University of Boumerdes, 35000 - Boumerdes, ALGERIA


ARTICLE INFO ABSTRACT / RESUME

Article History

Received : 14/12/2014

Accepted : 11/02/2015

Milk constitutes an important ingredient in the Algerian population diet. it is

obtained by recovering process from milk powder or the recombination-based

milk powder and anhydrous milk fat (AMF). These are the two main processes

in place in Algerian dairies. In this study, carried out in a dairy processing

situated in Boudouaou (Algiers), a comparative analysis of these two

processes was conducted in order to determinate the contribution to

environmental impacts of different basic elements of manufacturing milk. The

approach used was based on the life cycle assessment (LCA), which is a

standardized method (ISO 14040-14044). Results showed that the milk

powder is the main hot spot in almost all the categories under assessment.

Furthermore, adding the AMF has allowed the reduction of all impacts of the

order of 3 to 6% resulting in a decrease of 4.74 E-02 kgCO2eq of Global

Warming Potential, 0.21MJ of the consumption of non-renewable energy, a

reduction of 2.60 E-03kg SO2eq for terrestrial acidification/nitrification

potential. A decrease of 0.16kg TEGsoil is recorded to terrestrial ecotoxicity

and 2.80 E-05kg PM2.5eq to respiratory inorganics.

Key Words / Mots clés Milk; LCA; Algeria ; Global

Warming ; Eco toxicity

I. Introduction

The focus on sustainable development in recent

years in the food industry mainly environmental

aspects has motivated the emergence of several

evaluation studies in this sector in particular the

dairy industry. The most used tool was the Life

Cycle Assessment (LCA) witch is a performing tool

for environmental management that provides

knowledge about the environmental impacts

associated with a product or human activity.

Several authors assessed the environmental impacts

generated by milk production have used this

method [1-5]. Various authors [6,7] used the LCA

method to compare the modes of production of

milk. LCA was also used by some other authors [8-

12] in plants transformation. LCA was also used to

measure the environmental impact of dairy

derivatives such as cheese [12,13], yogurt [14] and

butter [15] and to compare the impact of different

methods of cleaning in place (CIP) in dairies. The

Algerian dairy industry mainly operates on the

basis of imported raw materials i.e. milk powder

and anhydrous milk fat (AMF). Technologically,

two transformation processes allow us to obtain

pasteurized milk: reconstitution and recombination.

The first process consists in rehydrating the whole

milk powder while in the second process; the

finished product is obtained from a mixture of

reconstituted milk, based on skim milk powder and

AMF. A lack of studies on the environmental

analysis of reconstituted milk powder was

observed, hence the interest of this approach to

determine the impacts of various basic elements of

this product. The study was carried out at a dairy

processing plant in Algeria to assess the

environmental impacts of the main constituents of

pasteurized milk, especially the AMF used in the

process of recombination.

18


F. Younsi


II. Materiels and methods

The method used in this study was LCA, an

environmental assessment tool standardized

according to ISO 14040 (ISO, 2006a) and 14044

(ISO, 2006b). LCA methodology includes four

major stages: goal and scope definition, life cycle

inventory (LCI), life cycle impact analysis (LCIA)

and interpretation of the results (ISO, 2006a). In the

goal and scope phase, a functional unit, system

boundary and allocation procedures are defined,

depending on the subject and intended use of the

study. For the LCI, all input and output processes

are defined, quantified and summarized. The LCI is

linked to environmental impact categories and

indicators by the LCIA, and interpreted relative to

the FU. SimaPro7.1.5 was used as support software

in this study. System boundaries of this study

encompass production of raw materials (milk

powder, raw milk, AMF), milk processing, packing

production (polyethylene, metal drums), and

transportation of the raw materials to the milk plant.

The delivery of final product from the dairy factory

to retailers was excluded from the system

boundaries as well as the consumption phase of the

product [9,12]. Production of capital goods

(machinery and buildings) was excluded from the

study in accordance with several studies [7,8].

Production, transportation and use of detergents and

disinfectants were also excluded from this study [3]

as well as the different scenarios of waste

management.

Inventory analysis

The inventory analysis involves the collection of

data concerning resource use, energy consumption,

emissions, and products resulting from each activity

in the system studied. In this study, inventory data

for the dairy factory were collected by means of

surveys, interviews and visits to the plant. The data

processing steps, transportation, energy and

packaging were collected from the Boudouaou

dairy plant which refers to 2013.

III. Results and discusion

The results for the characterization step are shown

in Table 1 referred to the functional unit. The

values of impacts related to the production of

reconstituted milk are higher than those of the

recombined milk and in order to determine the

origin of these impacts, we will discuss the

contribution of both systems to main categories of

impact.

Respiratory inorganics

This type of impact (Fig.1) represents the health

hazards caused by breathing inorganics particles

released into the air, in kg equivalent PM2.5. Table

2 shows that for 1 liter of milk, this impact in

scenario1 is more important than the scenario2 of

the order of 0.17 E-4kg PM2.5eq. This difference is

attributed to the milk powder which is the main

contributor in both scenarios (76% vs. 65.5%). The

adding of the AMF in scenario2 will decrease this

value of the order of 0.713 E-4kgPM2.5eq (9.12%).

The amount of raw milk in the scenario2 was

higher than in Scenario1, this will play a role in the

reduction of the order of 0.071 E-4kgPM2.5eq of

this impact. The production of steam also plays a

role in this impact category where it intervenes at

10% of the overall impact at both scenarios,

because milk reconstitution requires large amounts

of hot water and steam (It takes about 1 to 12 liters

of water heated to 400°C to reconstitute 1 liter of

milk). The steam was used mainly in the processing

operations including milk pasteurization. These two

energy sources are generally produced in boiler fuel

(fuel used in the dairy industry) resulting in the

emission of carbon dioxide (CO2), sulfur dioxide

(SO2) and nitrogen oxides (NOx). According to the

operation of the boiler, unburned can be produced,

giving rise to the emission of solid particles. A

contribution of 6.88% of transport by ship was

noted at both scenarios. Indeed, the environmental

impact of shipping was accompanied by emissions

of different gases (CO2, NOx, SO2 and CO) and

fine particles smaller than 2.5 microns. The PE

packaging production intervenes at 2.17 and 2.25%

respectively in both scenarios. In fact, the

production of 1kg of PE generates 12g of NOx, 9g

of SOx, 16.6 g of NMCOV and 3g of particles

(BUWAL 250, 1996). The contribution of the

remaining elements was <1% of the overall impact.

These values were considered negligible. We can

therefore conclude that this impact category was

attributed mainly to the milk powder and the use of

the AMF contributed to the reduction of 3.46% of

this impact.

Figure.1: Contribution to respiratory inorganics

(for 1l of milk)

19


Global Warming

This effect contributes to the climate change

(Fig.2). It is due to the greenhouse gas (GHG)

emissions such as CO2, CH4, and N2O. It is

expressed in kgCO2eq. As shown in Table 1, for 1

liter of milk, the GWP was higher in the Scenario1

of the order of 2.60 E-02kgCO2eq (4.28%). These

emissions were mainly attributed to the milk

powder, whose the contribution in Scenario1 was

greater than that in scenario2 of the order of 77.10

and 66.78% respectively. This is explained by the

need to use a large quantity of milk for the

production of milk powder (it takes about 7.8 kg of

milk to make 1 kg of powdered milk (LCA Food)

and several studies confirmed that the production of

raw milk is the main source of GHG (Eide, 2002;

Hospido et al, 2003; Castanheira et al, 2010; Fantin

et al, 2012; González-García et al, 2013). In the

same way, the production of raw milk added in both

process intervenes at the rate of 3.34 and 4.29%

respectively. The manufacture of PE packaging and

transport ship, come at a same rate (≈ 2.63%) in

both scenarios. The production of PE emanated

several GHG (per 1 kg of PE, 2.32 kg of CO2 4.4 g

of CH4 and 12g of NOx were emitted)

(BUWAL250, 1996). The impact of thermal energy

was important for both scenarios (13.28 and

13.87%) respectively, this was observed in the

various processing operations, because the

pasteurization of milk requires great amount of

steam. The production of the latter requires natural

gas, which generates greenhouse gases both in its

production than consumption (boiler). The impact

of other Process was considered negligible (<1% of

the total impact). For 1 liter of milk, the use of the

AMF in the second scenario contributed at 8.16%,

this allowed the reduction of the order of 4.28% of

the impact.

Terrestrial acidification/nitrification

The terrestrial acidification (Fig.3) is mainly caused

by atmospheric deposition of acidifying compounds

such as SO2, NOx, NH3,.... etc.. It is expressed in

equivalent kgSO2. For one liter of milk, the total

contribution to the terrestrial acidification and

nitrification was 6.64E-02 kgSO2eq in Scenario1

and 6.38E-02 kgSO2eq in scenario2 (Table 1). The

difference between the two scenarios was mainly

due to the milk powder which represents 89.91% of

the impact in scenario1 and 77.43% in scenario2.

The impact of raw milk in both scenarios was about

4.55 and 5.83% respectively. Its production was the

main contributor to acidification [1,4,8,12]. The

production of steam followed by ship transport,

contributed in both scenarios up to 2.50% and

2.06% respectively. The AMF contributed in

scenario2 with 6.97E-03kg SO2eq (10.92%), hence

a reduction of this impact of about 2.60 E-03 kg

SO2eq.

Figure.2: Contribution to the global warming

potential (for 1l of milk)

Figure.3: Contribution of two processes in

terrestrial acidification (for 1l of milk)

Availability of data

The inventory data is a crucial step in any LCA

study. However, accurate inventory data are not

always available [7]. Most LCA on the dairy

industry are focused on the primary production of

milk "cradle-to-farm-gate" [1-7]. There are very

few studies on the impacts of milk processing

plants [8,9-12] and no studies have addressed the

reconstitution milk production or milk powder.

Hence the difficulties in comparing our study to

those mentioned above. It is important to note that

few authors have included in their studies

respiratory inorganics and ecotoxicity categories,

mostly due to the lack of available information

[7,17].

20

F. Younsi


Table.1: Comparison of the two scenarios "characterization" for 1l milk

RI (kg PM2.5eq)

GWP (kg CO2eq)

NRE (MJ) TE (kg TEG soil) TA (kg SO2eq)

Scenario 1 Scenario 2 Scenario 1 Scenario 2 Scenario 1 Scenario 2 Scenario 1 Scenario 2 Scenario 1 Scenario 2 Milk Powder

6,18E-04 5,12E-04 4,68E-01 3,88E-01 2,82 2,33 2,11 1,75 5,97E-02 4,94E-02 Raw Milk

3,08E-05 3,79E-05 2,03E-02 2,49E-02 8,70E-02 1,07E-01 7,83E-02 9,62E-02 3,02E-03 3,72E-03 AMF

/ 7,13E-05 / 4,74E-02 / 2,12E-01 / 1,87E-01 / 6,97E-03 PE packaging

1,76E-05 1,76E-05 1,53E-02 1,53E-02 5,22E-01 5,22E-01 7,38E-03 7,38E-03 4,87E-04 4,87E-04 Paper packaging

8,48E-07 7,78E-07 3,61E-04 3,31E-04 5,72E-03 5,24E-03 2,05E-04 1,88E-04 2,73E-05 2,51E-05 Metal packaging

/ 1,38E-06 / 3,23E-03 / 3,51E-02 / 2,52E-03 / 3,29E-05 Ship transport

5,58E-05 5,38E-05 1,63E-02 1,57E-02 2,32E-01 2,23E-01 3,54E-01 3,42E-01 1,37E-03 1,32E-03 Truck transport

3,20E-06 3,39E-06 2,23E-03 2,44E-03 3,52E-02 3,83E-02 9,59E-02 1,04E-01 9,97E-05 1,05E-04 Electricity

1,24E-06 1,31E-06 4,01E-03 4,22E-03 6,66E-02 7,01E-02 4,48E-02 4,71E-02 5,23E-05 5,51E-05 Steam

8,19E-05 8,19E-05 8,06E-02 8,06E-02 1,16E+00 1,16E+00 7,98E-06 7,98E-06 1,66E-03 1,66E-03 Natural gas

/ 1,61E-06 / 1,00E-03 / 2,02E-02 / 2,14E-05 / 3,22E-05 PE waste

-2,26E-08 -2,26E-08 -1,34E-05 -1,34E-05 -1,23E-03 -1,23E-02 4,32E-05 4,32E-05 -1,22E-06 -1,22E-06 Paper waste

3,13E-08 2,88E-08 -8,11E-05 -7,46E-05 -1,38E-02 -1,27E-03 -1,99E-04 -1,83E-04 1,87E-06 1,72E-06 Metal waste

/ -4,44E-07 / -1,66E-03 / -1,41E-02 / 2,66E-04 / -1,11E-05 Total

8,10E-04 7,82E-04 6,07E-01 5,81E-01 4,91 4,70 2,69 2,53 6,64E-02 6,38E-02

Table. 2: Contribution of the AMF (for 1kg of milk)

Catégorie d'impact Unité Scenario 1 Scenario 2 Ecart %

RI kg PM2.5 eq 8,10E-04 7,82E-04 2,80E-05 3,58

TE kg TEG soil 2,69E+00 2,53E+00 0,16E-01 5,94

TA kg SO2 eq 6,64E-02 6,38E-02 2,58E-03 3,92

GWP kg CO2 eq 6,07E-01 5,81E-01 2,60E-02 4,28

NRE MJ primary 4,91E+00 4,7E+00 2,10E-01 4,27

IV. Conclusion

The application of the LCA procedure to two types

of milk processing, reconstitution and

recombination has made possible the comparison of

their environmental impacts and assessing the

contribution of different components of milk. The

impact criteria selected were quantified according

to the "cradle-to-gate" approach. The consumption

step and waste management were not included in

this study. The result shows that for all impact

categories, milk powder was the main contributor to

the environmental loads in both scenarios, and the

production of raw milk contributed more

significantly due to the large amount of milk

required (7.8 l/ kg of milk powder) (LCA Food).

However, the substitution of a certain amount of

milk powder by the AMF in the recombination

(scenario 2) has reduced the impact of 3 to 6%.

Within this context, it seems optimal to favor the

recombination of milk-based AMF.

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7,115-126. 9. Hospido, A., Moreira, M.T., Feijoo, G., 2003. Simplified

life cycle assessment of Galician milk production. International Dairy Journal 13, 783–796.

10. Berlin, J., Sonesson, U., 2008. Minimizing environmental

impact by sequencing cultured dairy products: two case

studies. J Cleaner Prod 16, 483–98 11. Nutter, D.W., et al., 2012. Greenhouse gas emission

analysis for USA fluid milk processing plants: Processing,

packaging, and distribution, International Dairy Journal http://dx.doi.org/10.1016/j.idairyj.2012.09.011

12. González-García, S., Castanheira, E.G., Dias, A.C., Arroja,

L., 2013. Using Life Cycle Assessment methodology to assess UHT milk production in Portugal. Science of the

Total Environment 442, 225–234

13. Kim, D., Thoma, G., Nutter, D., Milani, F., Ulrich, R.,

Norris, G., 2013. Life cycle assessment of cheese and whey

production in the USA. International Journal of Life Cycle Assessment. DOI 10.1007/s11367-013-0553-9

14. González-García, S., Castanheira, E.G., Dias, A.C., Arroja,

L., 2012. Environmental life cycle assessment of a dairy product: the yoghurt. International Journal of Life Cycle

Assess DOI 10.1007/s11367-012-0522-8

15. Nilsson, K., Flysjö, A., Davis, J., Sim, S., Unger, N., Bell, S., 2010. Comparative life cycle assessment of margarine

and butter consumed in the UK, Germany and France.

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16. van der Werf, H.M.G., Kanyarushoki, C., Corson, M.S.,

2009. An operational method for the evaluation of resource use and environmental impacts of dairy farms by life cycle

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3643–3652. 17. Yan, M.J., Humphreys, J., Holden, N.M., 2011. An

evaluation of life cycle assessment of European milk

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Please cite this Article as: F. Younsi., Contribution of Anhydrous Milk Fat to environmental impacts generated by the dairy

processing, Algerian J. Env. Sc. Technology, 1:1 (2015) 18-22

22

http://dx.doi.org/10.1016/j.idairyj.2012.09.011


o1. (2015)

ISSN : 2437-1114



Toxic effect of surfactants on marine species Mediterranean mussel: Mytilus gallprovinciallis and

evaluation of their aquatic toxicology impact by LCA methodology

M. Belkhir. S. Boughrara. H. Boutiche

Food Technology Research Laboratory, University of Boumerdes, 35000 - Boumerdes, ALGERIA



Article History

Received : 11/01/2015

Accepted : 11/03/2015

The increase of over 500% in ten years, the use of synthetic detergents

explains the high concentrations explain the high concentrations in liquid

effluents. Part of these discharges flow without purification in rivers. Which it

is interesting to assess the impacts thus generated by such a detergent

manufacturing process. In our study we used the tool life cycle assessment

(LCA) methodology to assess the aquatic toxicology impact of liquid detergent

intended multi user. This study needs the use of SimaPro7.1 software and

EDIP 2003method.In order to explain aquatic toxicology impact was chosen

by selecting a type of marine species Mediterranean mussel Mytilus

gallprovinciallis.In our study we determined the toxic effect of anionic

surfactants (LAS, AES) characterization of liquid effluents generated by one of

the leading Algerian companies in detergents. Comparing the toxicology of

two anionic surfactants is obtained after determining the lethal concentrations

of fifty percent (LC50) of the individuated simmering with forty-eight hours

(48h), Ensuring living conditions (temperature, O2, pH, TH, TA, TAC). In an

aquarium. Any and controlling various pollution parameters (BOD5, COD,

Nitrate, Nitrite, Phosphate, Sulfate, Dissolved Oxygen.

Key Words / Mots clés Aquatic toxicology impact,

Mytilus gallprovinciallis,

LCA methodology, anionic

surfactant, LC50.

I. Introduction

With the growing awareness of environmental

issues, the integration of sound environmental

management practices in our industry is growing in

importance. In response to this reality, various

environmental assessment tools have been

developed, such as environmental risk analysis,

analysis of material flow, the ecological footprint.

According to the article Finnveden, G., Hauschild,

MZ, Ekvall, "Recent developments in Life Cycle

Assessment" pull Journal of Environmental

Management, these players end up saying that

environmental tools provide some answers for

decision informed decisions, both for those in the

public and private sectors [1]. LCA appears as an

appropriate tool to measure and certify the

improvement of its production cycle or ease of

waste treatment. In fact, some organizations rank

companies based on their impact on the

environment [2]. This methodology has taken place

within ISO 14040 series [3-6]. The control of the

environmental impact of activities in the detergents

manufacturing industries is now essential for their

durability, as well as the reduction of production

costs or improving product quality. It also affects

the image of the products from the consumer and

also intervenes in their "quality"[7]. Surfactants are

an important part of the composition of detergents

in 1995, the Health Research Institute and safety at

23


M. Belkheir et al


work of Québec, Montreal shows that global

production is about 3106 tons or increased in the

past ten years is over 500%, this increase explains

their high concentrations in industrial effluents and

sewage, or they flow without purification in rivers.

In our study we determined the toxic effect of three

kinds of surfactants (LAS, AES and NI07) that fall

within the composition of a multi user detergence.

LAS: Linear Alkyl benzene sulphonate (anionic)

AES: Alkyl Ether Sulfate (sulphonate) (anionic)

NI 07: Fatty Alcohol Ethoxylate (nonionic)

And for the purpose of an environmental

assessment of their impacts aquatic toxicology, we

applied the approach Life Cycle Assessment to

justify of results obtained by their ecotoxicity tests.

II. Materiels and methods

The methods used in our study are:

The determination of the lethal concentrations of

fifty percent (LC50) of three surfactants on

mussels

The potential ecotoxicity was addressed by

performing a toxicity test (acute effects) assets

tensions LAS, AES and NI07 on an aquatic

organism Mediterranean mussel Mytilus

galloprovincialis causing mortality 50% of the

population exposed to a fixed concentration of a

24H and 48H surfactant with mid renewal.

Experimental Protocol

More than 200 species of mussel Mytilus

galloprovincialis were collected in July 2013, in a

Sghirate site, it is located 5km from the center

wilaya of Boumerdes (east of Algiers). The molds

were kept in seawater and transported to the

laboratory in coolers. Before moving to the

toxicological test should be allowed mussels an

adjustment period in aquariums, with a dozen

mussels in 10L water ensuring ventilation the one

hand and avoiding their toxicity nitrate comes from

their nitrogenous waste.

Preparing the aquarium

The main difficulty in setting up an aquarium is to

recreate the best conditions for living environment

mussels (sea water), either the temperature, the

hardness of the water, the nitrate problem etc. The

molds are placed in the tank (food plastic basin) at a

temperature entre14 ° C and 16 ° C (temperature of

sea water).

The Life cycle assessment

LCA is a method for environmental analysis

identifies the major sources of environmental

impacts and avoiding further transfer of pollution

from one phase of the life cycle to another. It is

therefore essential to cover the entire life cycle so

that improving the overall rendering is not reflected

on another scale.[8]. These steps are more

commonly referred to as "cradle to grave". During

each of these steps, products and processes interact

with the environment.

Goal and scope of the study

The goal of the present study is to assess the

environmental performance of detergent. The

model focuses on production of detergent liquid

form that is: multi user liquid, the production

processes include the mixture of all compounds in

aqueous solution. The functional. Unit of analysis

in this study is the production of one ton of this

detergent.

Inventory analysis

To establish LCA for the multipurpose workshop,

we tried to collect all the theoretical and

experimental data from the various analyzes carried

companions. These data include those relating to

the consumption of raw materials (surfactants,

fragrances, dyes, packaging material) and energy

consumption (water, electricity). Which are related

to the functional unit defined above.

Balance incoming

The raw material consumption and energy is

presented in Table 1.

Tab.1: Consumption of raw materials and energy Inputs consumption

(kg)

LAS (alkyl benzènesulfonâte ) 21.207

AES (alkyl ethoxy sulfate ) 26.414

NaoH 0.526

NaCl 4.260

Parfum 1.230

Formol 0.662

NI LT07 3.787

Dye 0.153

acetic acid 0.037

Dequest 0.568

Packaging material consumption

(kg)

cellulose Cards (Kg) 50

Labels (plastic) (Kg) 3.60

caps (PEHD) (Kg) 4.80

bottles (PET) (Kg) 48

Energy Consumption

Electricity (KWh) 32.14

Water (m3 ) 941.18

Out going balance

Outgoing balance consists of rejecting liquid

(water) and solid (packaging waste), including

pollution parameters are measured and calculated

according to standardized methods of water

analysis. (See the book by Rodier ) [4]. But the

concentrations of the surfactants (LAS, AES and

NI07) are determined by the chromatographic

method using a (HPLC).

24


Tab. 2: Analysis methods HPLC (In mobile phase at high ionic strength) [5]

with :

Fig.1: Chromatogram of surfactants

SPE : Solid phase extraction.

SM :Mass Spectrometry.

REA: anion exchange resin

LD: limit dedétection.

CTMA: cetyltrimethylammonium.

G: gradient.

I: isocratic.

Tab.3:physicochemical parameter of rejecting

liquid

Outputs

physicochemical parameter Results

temperature (°C) 20

Ph 9.07

COD (mg of o2/l) 983.00

BOD5 (mg of o2/l) 103.33

LAS (g/l) 1.96

AES (g/l) 0.600

NI07 (g/l) 0.068

salinity (g/l) 3.50

turbidity (NTU) 71.11

The O2 below (mg/l) 13.32

Phosphates (mg/l) 76.00

Sulfates (mg/l) 800.00

Nitrates (mg/l) 30.00

TDS (g/l) 3.45

Solid waste

cellulose Carton 5

Label plastic 2

25

M. Belkheir et al


III. Results and discusion

Ecotoxicity tests surfactants on mussels

1st test :

The experiments were usually performed in

continuous flow aquaria. In order to assure natural

conditions, the aquarium is alimented by sea water

at a constant continuous flow with variation of

temperature between 14C° to 18C° and Ph varies

between 7 to 8 for each 10 animals in 10L of sea

water for 48 Hours for each experience. The

standard sample is taken in sea water, that its

characteristics are summarized in table 3. It’s

remarked that no mortality of animals (see table 4).

Tab .4: Physicochemical characteristic of standard

sample (only sea water) Physicochemical parameter Results

O2 (mg/ l) 8,60

Ph 7,42

Salinity (g/l) 29

Turbidity (NTU) 8 ,11

Total of dissolute Salt (TDS (F°) 26,4

Sulfate (mg/l) 0,02

Nitrate (mg/l) 2,72

TH (F°) 1060

Tab. 5: Mortality of mussels in 1nd

test (see water) Day of

contact

1st

Da

y

2nd

Da

y

4th

Da

y

6th

Da

y

8th

Da

y

9th

Da

y

10th

Da

y

% Mortality 0 0 0 0 0 1 3

Tab. 6: Physicochemical characteristic of standard

sample after the 1nd

test

Contact time

Physicochemical

parameters

1st

Day

4th

Day

9th

Day

10th

Day

O2 (mg/ l) 8.46 8.10 7.89 7.72

Ph 7.41 7.38 7.40 7.42

Salinity (g/l) 30 29.8 29.8 28.7

Turbidity (NTU) 9.30 11.8

2

20.87 30.61

Total of dissolute Salt (TDS

(F°)

28.5 28.3 28.4 28.3

Sulfate (mg/l) 0.02

2

0.01

8

0.024 0.019

Nitrate (mg/l) 59.3

6

75.4

4

133.2

1

195.3

8

TH (°F) 105

6

104

0

1048 1051

2nd test

The mussels are taken in three aquariums

sea water, with addition for each one a surfactant

that it’s concentration is taken in the reject of Eagle

factory (see table 3). These animals are taken

contact with each solution for 48 Hours, that the

results are summarizes in table 7.

Tab.7: Mortality of mussels in contact with the

actual concentrations.

Concentration surfactant

Mortality%

LAS

(1,98

g/l)

AES

(0,65g/l)

NI07

(68mg/l)

24h 60 80 70

48h 100 100 100

These results show that the:

- LAS LC50 for mussels is <1.98g / l.

- AES LC50 for mussels is <0.65g / l.

- NI07LC50 for mussels is <68mg / l.

The characteristic of solution after contacts are

summarized in table 6

The characteristic of the environment solution of

the 2nd

experiment after contact is summarized in

table 8

Tab.8. physicochemical characteristic after the 2nd

test Physicochemical

parameters

LAS AES NI

07

O2 (mg/ l) 9,73 9,57 9,75

Ph 6,80 6,68 6,83

Salinity (g/l) 32 32,5 32,4

Turbidity (NTU) 801 30,3 13,2

Total of dissolute Salt (TDS (F°) 29,8 30 30,2

Sulfate (mg/l) 710,20 689,79 0,026

Nitrate (mg/l) 5112,76 139,14 84,27

TH (°F) 850 870 700

3rd test

The animals are taken in one aquariums of sea

water, with addition a mixture of three surfactant

that it’s concentration is taken in the reject of Eagle

factory (see table 3). These animals are taken

contact in this environment for 48 Hours, that the

results of mortality are summarizes in table 9 and

the characteristics of this environment after contact

are summarized in table 10.

Tab. 9: Mortality of mussels for the 3rd test Time of contact % of mortality

24 H 90

48 H 100

Tab: 10. Physicochemical characteristic after the

3rd test Physicochemical parameter Results

O2 (mg/ l) 9.70

Ph 6.80

Salinity (g/l) 32.5

Turbidity (NTU) 830

26


4th

test

The animals are taken in four aquariums of sea

water, with addition different concentrations

(table11 of the anionic surfactant (LAS) contacting

the animals for 48 Hours. The results of mortality

are summarizes in table 11 and figure 2, the

characteristics of this environment after contact are

summarized in table 12

Tab: 11: Mortality of mussels in contact with the

concentrations of LAS

Concentration of LAS

Mortality %

10

mg/l

50

mg/l

75

mg/l

100

mg/l

24h 10 20 40 60

48h 40 80 100 100

Fig.2: Mortality of mussels on function

concentration of LAS

Tab.12: physicochemical characteristic after the 4th

test

Concentration

of LAS

Physicochemic

al parameters

10

mg/l

50

mg/l

75

mg/l

100

mg/l

O2 (mg/ l) 7 7,10 7,05 6,90

Ph 7,20 7,24 7,30 7,10

Salinity (g/l) 29,8 29,8 29,7 28,6

Turbidity (NTU)

22 101 135 182

Total of

dissolute Salt (TDS (F°)

28,3 28,4 28,3 28,2

Sulfate (mg/l) 3.51 17.5

9

26.3

9

143.31

Nitrate (mg/l) 644.68

861.70

1161.70

1440.42

TH (°F) 830 810 750 700

5th

test

The mussels are taken in four aquariums of sea


(table12) of the anionic surfactant (AES) contacting

the animals for 48 Hours. The results of mortality

are summarizes in table 13, the characteristics of

this environment after contact are summarized in

table 13.

Tab.13: Mortality of mussels 5th

test

Concentration of AES

Mortality %

10 mg/l 50

mg/l

75

mg/l

100

mg/l

24h 40 50 70 80

48h 50 90 100 100

The AES LC50 for mussels is 10 mg / l.

Tab.14: physicochemical characteristic after the 5

th

test

Concentration of

AES

Physicochemical

parameters

10

mg/l

50

mg/l

75

mg/l

100

mg/l

O2 (mg/ l) 8,01 7,10 6,87 6,70

Ph 7,27 7,08 7,03 7,10

Salinity (g/l) 30,00 29,8 29,8 28,7

Turbidity (NTU) 59,5 63,8 122 163

Total of dissolute

Salt (TDS (F°)

28,5 28,3 28,4 28,3

Sulfate (mg/l) 3.51 17.59 26.3

9

35.19

Nitrate (mg/l) 379.68 407.75 778.

72

1040.42

TH (°F) 900 870 850 830

6

th test

The animals are taken in four aquariums of sea


(table15) of the nonionic surfactant (NI 07)

contacting the animals for 48 Hours. The results of

mortality are summarizes in table 15 and figure 3,

the characteristics of this environment after contact

are summarized in table 16

Tab.15: Concentration surfactants and animals

mortality in 6th

test

Concentration of NI 07

Mortality %

1

mg/l

5

mg/l

10

mg/l

24h 10 70 100

48h 20 100 100

It is found that the nonionic may cause 100%

mortality of the population at a concentration of 10

mg/l. The CL5048h of NI07 is between 1 mg / l and

5 mg / L, and it is possible to graphically determine

the mortality curve as a function of the

concentration of NI07.

27

M. Belkheir et al


Fig.3: Mortality of mussels on function

concentration of NI O7

Tab.16: physicochemical characteristic after the

6th

test Concentration of NI 07

Physicochemical

parameters

1

mg/l

5

mg/l

10

mg/l

O2 (mg/ l) 6.95 7.01 10.40

Ph 7.01 7.02 6.85

Salinity (g/l) 29 ?8 30 30?9

Turbidity (NTU) 30 64 86.5

Total of dissolute Salt (TDS (F°)

28.5 28.3 28.6

Sulfate (mg/l) 0.019 0.024 0.020

Nitrate (mg/l) 191.48 408.51 552.12

TH (°F) 910 870 800

Based on the results, a 48H of contact with different

surfactants is sufficient to cause a mortality rate of

100% of the population, we note that the LAS 24H

has a concentration [LAS] = 1.98g / l to cause 60%

mortality, AES has de0.65g / l causes 80%

mortality and the mortality rate of NI07 is 70% to

68mg / l.

Rather, the mixture of the three surfactants caused a

mortality rate of 90% of the population after 24

hours of which we can conclude that the

assemblement of these surfactants is more toxic

than mètrent separately, something that does not

happen in the manufacture of cleaning products.

It is noted that the hardness decreases with increase

in the concentration of the LAS, the decrease is due

to the ions of the complexities of the reactions with

sulphate ions Mg ++

and Ca ++

forming precipitates:

Ca (LAS) 2

and Mg (LAS) 2. 48 hours after contact,

mussels with different concentrations of the AES,

we find that:

- pH decreases slightly, and this due to the

acidification caused by the presence of sulphate

ions in the aquatic environment by keeping the

neutral medium.

-The reduction of dissolved O2 is due to the

breathing of the mussels, it is one of the nutrients

necessary for survival and growth of the mussels.

In the control, test there's no real change in the

water body except a slight decrease in hardness and

dissolved O2 that due to consumption by mussels

and a nitrate concentration increased from

nitrogenous waste mussels.

To compare the ecotoxicity of three surfactants with

each other, a determination was performed per

class, depending on the CL5048H each surfactant.

Fig.5: Comparison ecotoxicity of three surfactants

Finally we will justify the results of the tests of

Ecotoxicological these three surfactants by applying

the LCA approach that will allow us to make a

toxicological classification of the three surfactants

and assessing their impacts aquatic toxicity.

Application of life cycle assessment on multi

user liquid detergent

Impacts assessment

The EDIP2003 method is used to assess the

environmental impacts.

The impacts considered in this study are shown in

figure 4 and summarized in table 17:

Aquatic eutrophication EP(N) expressed on kg N

Aquatic eutrophication EP(P) expressed on kg p

Human toxicity water expressed on m 3

Bulk waste expressed on Kg

Tab.17: Impact generated by detergent liquid multi

user-EDIP 2003 method

Impact categories Unit Results

Aquatic eutrophication EP(N) Kg N 4.07 E-6

Aquatic eutrophication EP(P) Kg P 2.21 E-5

Human tocxicity water m3 0.105

Bulk waste Kg 7.00

y = 8,5246x + 27,8690

20

40

60

80

100

120

0 5 10 15

mo

rtal

itè

en

%

concentrations en mg/l

0

20

40

60

80

100

120

1 5 10 50 75 100m

ort

alit

y %

concentration mg/l

NI07

AES

LAS

28


Contribution of components to the impacts

generated

Edip2013 method allows us to explain the origin of

some important impacts : human toxicity by the

water. Which we are interested in their origins.

Tab.18: Contribution to Human toxicity water

impact generated

Impact

categories

Element

contribution

Unit Results

Human toxicity

water

Alkyl Ether Sulfate

(sulphonate)

m3 1.78 E-4

Fatty alcohol ethoxylate

m3 0.103

Linear Alkyl

benzene sulfonate

m3 5.28 E-4

The aquatic toxicity has received particular

attention in the regulatory context, as the aquatic

compartment is a typical sink for industrial

pollution due to direct releases and indirect

emission pathways. This impact category is

primarily influenced by the emission of the

surfactants in the various processes for the

production of detergents

The multi pollutant in use is the impact of human

toxicity by the water with a large contribution of

NI07 surfactants, LAS and AES.

The surfactants are responsible aquatic human

toxiicity, explain what these surfactants

concentrations accumulated by aquatic species and

transformation to the human food chain

Conclusion

Reviews conducted environmental toxicity of

certain assets tensions in several marine species,

and to complete these studies and to provide

knowledge in the same perspective, our study was

performed on a species called mussels , there was

little toxicological studies in this context.

In The practical part, we tried to vary the

concentrations of three active tension, two of which

are anionic (LAS, AES) and one non-ionic (NI7),

and put it in contact for a definite time with mussels

and monitored physiological variations and the

number of deaths of the species.

This study followed the results of the LCA

approach that has allowed us to make an assessment

of the impact of human aquatic toxicity of liquid

detergent (multi use) and to determine the

contribution of components to these impacts.

The ecotoxicity of the aquatic species studied

shows that the nonionic is more toxic than anionic

because it caused the death of all individuals

contacted in time less than 24heurs with behavioral

disturbance and physiology of this species.

Through this research we can propose the

replacement of the most polluting power assets

(non-ionic) with oils play an important role in

detergents such as essential oils or ethoxylated oils

that are low in toxicity.

Finally, wishing us by this research that will result

in the initiative, and it will serve as a reference for

future research.

V. References

1. ANDRE, P., DELISLE, C., REVERET, J.P.,

L’évaluation des impacts sur l’environnement :

processus, acteurs et pratique, Presses internationales Polytechnique, ISBN 2-553-2003, 519 p.

2. 01132-6,

3. Directive du Conseil n° 85/337/CEE du 27 juin 1985 concernant l'évaluation des incidences de certains

projets publics et privés sur l'environnement,

article 3 tel que modifié par la Directive n° 97/11/CE du 3 mars 1997, Journal Officiel de la

Communauté Européenne n° L 175 du 5 juillet 1985. 4. ISO Systèmes de management environnemental :

spécifications et lignes directrices pour son

utilisation, norme française AFNOR en ISO 14001,

1996, 15 p.

5. Olivier Jollet, Myriam Saade, Pierre Crettaz, Analyse

du cycle de vie : comprendre a réalisé un écobilan , 2010.

6. ADEME, Note de synthèse externe, "Introduction à

l'analyse du cycle de vie (ACV)," 2005. 7. Organisation Internationale de Normalisation,

"Norme ISO 14040 ‐ Analyse du cycle de vie ‐ principes et cadre ,2006.

8. Sebastien Renou, Analyse du cycle de vie appliquèe

aux systemes de traitement des eaux usées, thèse de doctorat de l’institut national polytechnique de

Lorraine .2006.

9. Rodier.J,Legube.B,Merlier.N et Coll, L’analyse de l’eau, Edition 9, entire mise a jour, Dunod Paris, 2009

10. Morris, M.; Wolf, K. (1998) Water-Based Repair and

Maintenance Cleaning: Case Study Conversions. Institute for Research and Technical Assistance's

Pollution revention Center, Santa Monica, CA.

Please cite this Article as: M. Belkhir., S. Boughrara., H. Boutiche., Toxic effect of surfactants on marine species Mediterranean mussel: Mytilus gallprovinciallis and evaluation of their aquatic toxicology impact by

LCA methodology, Algerian J. Env. Sc. Technology, 1:1 (2015) 23-29

29


o1. (2015)

ISSN : 2437-1114



Reaction in water under microwave: rapid and convenient synthesis of N-hydroxymethylimides and N-hydroxymethyl

lactams

M. Hachemi

Faculté des Sciences de l’Ingénieur-UMBB- Boumerdes


ARTICLE INFO ABSTRACT

Article History:

Received : 11/01/2015

Accepted : 11/02/2015

N-hydroxymethyl imides and N-hydroxymethyl lactams were obtained

by the reaction of formaldehyde with imides or lactams in water under

microwave irradiation (15 min., 240 W).

.

Key Words:

Microwave,

Water,

Formaldehyde,

N-Hydroxymethy

I. Introduction

Actually chemical synthesis employs

large amounts of hazardous and toxic

solvents. In last decade, there has been an

incredible growth in research involving

water as a green, environmentally benign

replacement for a wide range of organic

solvents.1 The water is a no toxic, non-

flammable, non-polluting and inexpensive

solvent. It is an ideal solvent for synthesis

on condition that the organic compound

can be dissolved.2 It has also a high

dielectric constant so their molecules are

very well activated under microwave

irradiation.3

We have been interested in the synthesis of

a series of related compounds belonging to

the following families: the N-

hydroxymethyl lactams and N-

hydroxymethyl imides

We report herein the reaction of

an aqueous formaldehyde solution under

microwave irradiation for the

transformation of amides into N-

hydroxymethyl lactams without use of any

catalyst (Scheme 1)

OH

O

NH

O

N

240 W, 15 min.

microwaves

HCHO, H2O

Scheme 1: Synthesis of N-hydroxymethyl

imide or N-hydroxymethyl lactam

Morever the application of N-

hydroxymethyl imides or N-hydroxymethyl lactams

has been of great interest in the field of

agropharmaceutical manufacturing ( potential

antipsychotic4, agents for modification of textile

material5, precursor of surface-active ethers, in the

synthesis of insecticides (tribenuron)6, proteolytic

enzyme inhibitors and so on. They are also used in

active energy-curable varnishes for coatings7, inks

and adhesives for protecting wood surface,8 as

corrosion inhibitors, and as flame-protection agents.

Although, a large number of synthesis of these

products is described, only few are really effective

and generally, the assistance of catalysts is

necessary.9

03


M.Hachemi


Previously, it has been reported the formation of

aromatic hydroxymethyl imide by action of the

paraformaldehyde on amides in DMF10, (the use of

aqueous formaldehyde leads to very bad results).

Unlike of our case, a kitchen microwave oven was

used without reflux cooler, in these conditions, the

formaldehyde formed escape quickly with the water

and can’t react sufficiently with the reagent.On the

other part, the insufficient coupling with a

multimode irradiator does not allow to obtain good

and reproducible results with water.

In our case, the aqueous solution formed with

formaldehyde and lactam or imide was irradiated

under reflux with a microwave monomode

irradiator. The main advantage of this procedure is

to carry out reactions which would be impossible

to do correctly in a kitchen microwave oven.

It is also possible to follow the rise in temperature

in the reactor (use an infrared thermometer).

Reactional mixtures were irradiated for 15 minutes,

but reaction is generally ended after 4-5 min. The

curve of evolution of the temperature shows an

inflection point followed by a landing temperature

showing the end of the reaction. By cooling the

reaction mixture, the products N-hydroxymethyl

lactams crystallize. A further crystallization (for the

solvent, see table 1) was not always necessary to

obtain the pure product. The yield of the reaction

was almost quantitative. Results with different

imides and lactams are reported in the table 1.

The products obtained were characterised by

their 1H and 13CNMR spectra and their

quantitative analysis.

In conclusion, the synthesis under focused

microwave irradiation of N-hydroxymethyl imides

or N-hydroxymethyl lactams is fast and efficient

from a commercial available aqueous formaldehyde

without the assistance of any catalyst.

II. Experimental part

Reactions were carried out with a monomode

microwave irradiator Prolabo Synthewave 402 at

2450 MHz monitored by a microcomputer. The

power of irradiation was fixed and the temperature

was recorded in direct.

General procedure (N-hydroxymethylimide or N-

hydroxymethyllactam) ex: Phthalimide

In a quartz tube surmounted with a reflux cooler,

the phthalimide (100 mmol) and an aqueous

solution of of formaldehyde (37%, 3 ml) were

irradiated for 15 min with power 240 W. A

homogeneous solution was obtained and by

cooling, crystallised in a heap of colourless crystals.

The product was recristallised in a acetone Mp=

149°C (lit=149).

All N-hydroxymethlimides crystallised

spontaneously. In the case of N-

hydroxymethyllactams, liquids were first obtained.

The pyrrolidin-2-one derivative was crystallised in

ethanol, in the case of the piperidin-2-one

derivative, we have not obtained crystallisation.

III. References

1. D. J. H. Clark and D. Macquarrie, Handbook of Green

Chemistry and Technology, Clark, Blackwell Publishing

Ld , Oxford, 2002. 2. R. Breslow, Acc. Chem. Res., 2002, 35, 9; C. J. Li, Chem.

Rev.,1993, 93, 2023; A. Lubineau, J. Auge and Y.

Queneau, Synthesis, 1994, 741; C. J. Li, Tetrahedron, 1996, 52, 5643; C.J. Li and T.H. Chen, Tetrahedron, 1999,

55, 11149 ; C. J. Li and H. T. Chang, Organic Reactions in

Aqueous Media, Wiley, New York, 1997; P. A. Grieco,

Organic Synthesis in Water, Blackie Academic and

Professional, London, 1998.

3. B. L. Hayes, Microwave Synthesis-Chemistry at the Speed of Light, CEM publishing, Matthews, 2002.

4. M. K. Scott, E. W. Baxter, J. Bennett, , R. E Boyd, P. S.

Blum, E. E. Codd, M. J. Kukla, E. Malloy and B. E Maryanoff, J. Med. Chem., 1995, 38, 4198.

5. S. L. Vail, Textile Res. J. ,1972, 42, 360; S. L. Vail and

A.G. Pierce Jr, Textile Res. J. ,1973, 43, 294 . 6. K. Nishimura, T. Kitahaba, Y. Ikemoto and T. Fujita,

Pesticide Biochem. Physio. 988), 31, 155.; A.K.

Bhattacherjee and P. Dureja, Pesticide Sc. ,1999, 55, 183. 7. Y. Inaba, G. Urano, T. Kobayashi, U.S. Pat. Appl. Publ.

(2005), US 2005014924, Chem. Abs., 2005, 142:135564 .

8. T. Watanabe, (Sekisui Chemical Co. Ltd., Japan), Jpn. Kokai Tokkyo Koho (2002), JP 2002080509, Chem.

Abs., 2002 136, 248414.

9. B. Jouglet, S. Oumoch and G. Rousseau, Synth. Commun., 1995, 25, 3869.

10. K. Kacprzak, Synth. Comm., 2003, 33, 1499.

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Table 1: Synthesis of N-hydroxymethyllactams or N-hydroxymethylimides under microwave irradiation (15 min,

240 W).

Product Starting product Yield

(%)

mp °C

Solvent

Mol formula C Found (required)%

H

2a phthalimide 98 149 (acetone) C9H7NO3 60.97(61.02) 3.96(3.98)

2b saccharin 97 125 (EtOH) C8H7NO4S 45.10(45.07) 3.27(3.31)

2c maleimide 96 104-106 (EtOAc) C5H5NO3 47.34(47.25) 4.03(3.97)

2d succinimide 98 64-66 (EtOAc) C5H7NO3 46.58(46.51) 5.51(5.46)

2e pyrrolidin-2-one 88 82 (EtOH) C5H9NO2 52.22(52.16) 7.82(7.88)

2f piperidin -2-one 85 liquid C6H11NO2 55.61(55.8) 8.68(8.58)

Reaction in water under microwave: rapid and convenient synthesis of N-hydroxymethylimides and N-hydroxymethyl lactams

Please cite this Article as: Hachemi, M., Reaction in water under microwave: rapid and convenient synthesis of N-hydroxymethylimides and N-hydroxymethyl lactams, Algerian J. Env. Sc. Technology, 1:1 (2015)

30-32

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Study of dispersion of brine water into coastal seawater by using a pilot

Laboratory of Food Technology, Faculty of Engineering Science, university of Boumerdes Algeria.



Article History:

Received : 11/01/2015

Accepted : 11/04/2015

Les technologies utilisées dans le dessalement des eaux de mer sont

accompagnées par diverses impacts sur l’environnement. Plusieurs

effects considérés dans les unites de dessalement tells que les imacts

marins et la pollution marine. Les unites de dessalement des eaux de

mer sont localisées pour apporter un supplement d’eau aux

populations et aux diverses applications. La construction des unites

dessalement et les infrastructures installées sur les côtes affectent le

milieu marin. La grande salinité de la saumure et les produits

chimiques utilizes sont dévérsés dans le milieu marin. Ainsi, plusieurs

impacts sont causes par la décharge de la saumure. Dans cet article,

l’objectif de ce travail consiste d’étudierl’influence de different

parameters de dispersion de la saumure comme la position du rejet, le

déplacement et le temps. Different points de rejet de la saumure ( P1,

P2, P3) sont étudiés horizontalement et verticalement en fonction de la

température de l’eau de mer. Les resultants expérimentaux obtenus

montrent que la dispersion de la saumure , la meilleure pposition est

celle la plus loine et la plus profonde (P3).

The technologies used in water desalination are accompanied by

adverse environmental effects. There are several effects to be

considered in desalination plants, such as the use of the land, the

groundwater, the marine environment and noise pollution. Seawater

desalination plants are located by the shoreline, to supply desalted

water to the population of the main cities and for other uses. The

construction of both the desalination plants and all the required

infrastructure in coastal areas affects the local environment. For

instance, the high salt concentration in the brine and several chemical

products used in the desalination process are returned to the sea. Most

impacts on the marine environment arise as a consequence of the brine

discharge. In this paper, the objective of this work consists to study the

dispersion of the brine discharges and its impact into marine

environment. Then, a pilot used to study the different parameters of

dispersion such as position of brine and depth and time of dispersion.

Different points of brine (P1, P2, P3) were studied horizontally and

vertically according to the ambient sea water. Experimental results

obtained show that dispersion of brine in best then position of brine

point is far and in down sea (P3).

Key Words:

Desalination,

Environment,

brine,

sea water,

pilot.

L. Habet*, K. benrachedi

33


L. Habet et al


I. Introduction

Algeria with a semi-arid climate and with its

limited water resources already intensively utilized,

suffers from temporary water shortages, with a high

level of utilization of its water resources, water

demand increasing due to repeated drought. The

government of Algeria has decided to construct a

number of desalination plants based on reverse

osmosis. Reverse osmosis is a physical process in

which contaminants and the undesirable

compounds are removed by using pressure on the

feed water by forcing it through a semi permeable

membrane [1]. Provision of potable water by

seawater desalination is generally considered a

benefit despite high construction and operating

costs of plants. This is especially true when

conventional sources of freshwater are absent or

cannot be exploited without severe environmental

damage. Whoever is familiar with the situation in

arid countries such as Algeria knows that

desalination plants are often large industries

facilities, which consume space and emit

substantial amounts of combustion gases. It is also

knows that potable water production means

emitting a concentrate into the sea or into the

ground. However, a generally less noticed fact is

that this concentrate contains not only the contents

of the seawater taken in, but also additives

necessary for the desalting process and corrosion by

products [2, 3]. The response of the impacted

marine ecosystem depends on its sensitivity [4] and

the magnitude of the impact, which in turn depends

on factors such as distance, transport direction and

dilution. Most impacts on the marine environment

arise as a consequence of the brine discharge and its

effects could be worse in the Mediterranean sea

than in other areas. So our purpose is to study

desalination of sea water impact into marine

environment, using a pilot dispersion of brine into

marine environment.

II. desalination of sea water impacts into

environment

Desalination of seawater is thus the technology

predominantly used for alleviating the problem of

water scarcity in coastal regions. Although

desalination of seawater offers a range of human

health, socio-economic and environmental benefits

by providing a seemingly unlimited, constant

supply of high drinking water without impairing

natural freshwater ecosystems, concerns are raised

due to potential negative impacts. These are mainly

attributed to the concentrate and chemical

discharges, which may impair coastal water quality

and affect marine life, and air pollutant emissions

attributed to the energy demand of the process. The

list of potential impacts can be extended, however,

the information available on the marine discharges

alone indicates the need for a comprehensive

environment evaluation [5, 6].

III. Matériel et méthodes

1. Study of dispersion for brine into laboratory

pilot

The brine is a reject of desalination process. The

high salt concentration in the brine and several

chemical products used in the desalination process

are returned to the sea. In our research, we have

studied specially dispersion or propagation of brine

into sea water by using laboratory pilot which is

constituted by a sea water basin and a reservoir of

brine (see figure 1)

2-Experimental work

We have used in this study the following

laboratory pilot :

Figure.1: pilot experimental and his accessories

Legend :

1- graduated reservoir of brine (volume = 10 liters)

2- control valve of brine flow

3- flow to measure reject flow

4- conduct of reject in glass or plastic (PVC)

diameter d= 5mm

5- Manometer to measure reject pressure

6- Position of reject point (variable)

7- ventilation point

8- graduated tank of sea water (volume = 760 liters in

glass)

9- Metallic supports

10- brine

11- Sea water

1

0

1

1

2

3

5

6 7

8

9

1

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3. Analysis Method :

3.1. brine and sea water preparation

To study the brine discharge propagation in

seawater, we have used concentration equal at 60

g/l. , salinity of sample for sea water at 32 g/l

(temperature ambiente = 15° C).

Then, we have considered constant flow and

pressure of brine reject.

Experimental Conditions

Sea water ambient

Time of dispersion for brine is 20 minutes.

Reject flow QR = 0,15 l/min.

reject pressure for position (P1 et P2) = 0,07 bar

reject pressure for position (P3) = 0.1 bar

prepared volumes

Vbrine = 10 liters

Vseawater = 300 liters

3.2. Experimental protocol and operation mode :

1- placing brine and sea water in the tank

successively in the basin.

2- Opening the valve (2) for a constant flow.

3- Monitoring over time and space :

- For different positions for reject point (6),

we measure :

- changes in salinity in the basin according

to the time and the directions (x,y,z) ;

salinity (t,x,y,z)

3.3. Point reject situation :

Table 1 : Rreject points situation

Positions sampling on the axis z

( depth, surface level)

P1

- at surface level.

- at 10cm below

- at 20cm below

P2

at 20cm below

P3

at 20cm below

IV. RÉSULTAT ET DISCUSSION

1. dispersion of brine in the sea water according

to the depth of the basin

Figure 2 : evolution for the salinity of brine

discharge into seawater in the basin area at P1,

with sea water stable according to distance and

time (x, y, z=0, t=20 min).

Figure 3 : evolution for the salinity of brine

discharge into seawater at depth 10 cm in the basin

at P1 with sea water stable in function ( x, y, z=10

cm, t= 20 min).

35

L. Habet et al


Figure 4 : evolution for the salinity of the brine

discharge of seawater a depth of 20 cm in the

basin at P1, with seawater stable in function (x, y,

z=20 cm, t=20 min).

From the results shown in the figures 2, 3, 4, we

observe that the point of brine discharge, salinity is

too high. It decreases in sea surface from 10 cm on

axis (x), this has been shown by the work of J.J.

Malfeito and al. [7] in the channel Fantana

desalination plant in Javea in Spain [7]. However, it

forms a plume at the bottom of the sea which

becomes highly saline with a concentration 42g/l.

This is due to the difference in density between the

sea and the brine. Then extends to a distance of 120

cm. So, it causes ongoing damage to the aquatic

flora and fauna, especially in the coastal marine

inhabitants.

For instance, and based on the work of Jacqueline L

Dupavillon and al.[8] brine concentrations 50 g/l

have an inhibitory effect on the growth and

development of embryos apama of Sepia, and on

microscopic bacteria or fungi pathogens.

2. Propagation of brine discharge of function

time

(sampling at depth 20cm)

P1 : position of reject point on coastal

Figure 5 : evolution for salinity of brine discharge

into sea water in the basin at P1, with sea water

stable in function (x, y, z=20 cm, t = 10 min).

Figure 6 : evolution , function de (x ;y ; z=20cm ;

t= 20min), salinity of the brine discharge on the

sea water in the basin at P1, with seawater stable

We observe from the results shown in figures : 5, 6

a gradual increase in salinity in the basin over time.

Indeed, the value of the salinity of seawater

recorded after 20 min brine discharge reaches a

maximum value of 42 g/l. This is due to obstacles

located at the bottom of the basin. This high salt

concentration can affect the local marine

inhabitants. Indeed, these comments were raised by

the work of Jacqueline L Dupavillon and al.[8].

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P2 : position of reject point 40 cm far

for cosatal

Figure 7 : evolution of salinity of brine discharge

on the seawater in the basin at P2, with sea water

stable in function (x,y,z=20 cm, t=10 min).

Figure 8 : evolution of salinity of the brine

discharge on the seawater in the basin at P2, with

seawater stable in function ( x, y , z = 20 cm , t= 20

min).

We observe from the results shown in the figures 7,

8 the salt concentration is still high at the discharge

point and extends over time. The brine can go

further but at low concentrations. This is due to the

great depth from the point of discharge. According

to the work of Villanueva R. and al.[9] growth rates

of cephalopods are affected by the low

concentration of salinity, from where low salinity

brine increases the size of statolith. But also causes

deformities of embryos. This comment has been

removed by the work of Paulij,W.P and al. [10]

According to R. Einav [11], category where worked

on the same conditions, no overview of

environmental impact was observed in the region of

Malta (personal information Domovic Darko).

P3 : position of reject point 40 cm l far for

coastal, situated at bottom basin

Figure 9 : evolution of salinity for brine discharge


stable in function (x , y, z = 20 cm , t = 10min ).

Figure 10 : evolution of salinity for brine

discharge into seawater in basin at P3 with

seawater stable, in function (x; y; z=20cm;

t=20min).

37

L. Habet et al


We note from the results shown in the

figures : 9, 10 salt concentration is still high at

the discharge point. It is decreases with time.

For the discharge of the brine discharge forms

a jet of water, due to the pressure P' = 1,2 bar

(P' > P), and the inclination of the discharge

point upwardly at an angle 30°. This

corresponds to a rapid dilution. In fact, these

comments were raised by the work of T.

Bleninger and al. [12].

According to the work of R. Zimmerman [13]

which he worked on the same conditions, the

jet of brine has a well-defined area (depending

on the flow and speed of the jet). The current

density of the jet can causes erosion at the

bottom, this implies the difficulty of stabilizing

grass prairies and aquatic vegetation (studies in

the Canary Islands – the region of Sardina Del

Norte)

Sandy deposits removed by the phenomenon of

erosion can fill the holes of the rocks, which

are an important marine habitat different fish,

decreasing it with disapperance of aquatic

vegetation and benthos.

3. Effet on temperature on propagation of brine

into sea water in function time (sampling at

profundity 20cm)

P1 : position of reject point on

coastal

Figure 11: evolution for salinity of brine discharge


stable at temperature T=25°C in function ( x, y , z

=20 cm, t = 10 min).

Figure 12 : evolution for salinity of brine discharge


stable at temperature T=25°C in function ( x, y , z

=20 cm, t = 20 min).

We noticed from the results shown in the

figures: 11, 12 that the diffusion of brine is

faster at 25 °C compared to 15 ° C, so we can

say that according the results of Ahmed.

Hashim and al. [14], Gulf countries:

- the increase in temperature of the brine

typically causes an increase in

temperature of the sea water, which

can directly affect the marine

organisms in the discharge zone.

- We go more over, the high temperature

process can affect water quality and

consequently, decrease the

concentration of dissolved oxygen in

seawater

V. Conclusion

Seawater desalination is a solution to the

growing demand for freshwater, but the used

technical processes could damage the

environment, with impacts such as the global

warning due to the increases use of energy,

noise pollution, negative effects on land use

and adverse effects on the marine environment.

Brine reject is always the main environmental

problem and his discharge is usually done

jointly with the discharge of waste water

treatment, thus diluting it. There are some

marine species affected by the salinity of the

brine discharged into the sea, as grass prairies. In this paper, the work is intended to contribute

to the study of the impacts of seawater

desalination on the marine environment in the

Mediterranean through the use of a pilot

spreading brine on sea water and its effect on

marine environment.

The study of the propagation of brine seawater

as a function of time, we concluded that total

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calm sea water, brine goes to the seabed, as it

provides a source of continuous and

cumulative pollution, it would result in

ongoing damage to the flora and fauna in the

vicinity of the discharge point, and would be

linked to the increase of the salt concentration

and temperature. Since the Mediterranean is

characterized by its great depth, the dilution is

faster. It is therefore desirable to place the

brine discharge point far from the beach

(sample P3) and rocky areas which are rich in

organisms

Perspective, it would be interesting to install

diffusers on channel rejection, the performance

of the operation depends on the number of

broad casters and the space between them.

They will improve the dilution.

Another option is the use of lenses pointing at

an angle of 30-90 ° to the seabed, so that the

concentrated brine is pressed in the direction of

the surface of the sea.

VI. Références bibliographiques

1. K.Benrachedi ; K.Bensouali ; H.Houchati ,2009,Coupling

ultrafiltration with adsorption on activated coffee for use as

a reverse osmosis pretreatment” desalination, 239,pp122-

129. 2. Th. Hoepner ; A , 1999,procedure for environmental

impact assessment (EIA) for seawater desalination plants,

desalination,124,pp1-12. 3. D. Subba Rao and F. Al-Yamani, The Arabian Gulf in :

C.Sheppard, 2000,Ed.seas at the millenium Pergamon,

Amsterdam, pp.1-16. 4. K.Wangnik, 2000, IDA Worlwide desalting plants

inventory report No.16 IDA.

5. S. Lattermann ; T. Höpner;2008, environmental impact and impact assessment of seawater desalination.

Desalination,220,pp.1-15.

6. United Nations Environment Programme- Mediterranean

Action Plan MED POL,2003,Sea Water Desalination in the Mediterranean : Assessment and Guidelines, Map

Technical Reports series No.139, UNEP/MAP, Athens.

7. J.J. Malfeito*a, J. Dýaz-Canejaa, M. Farinasa, Yolanda Fernandez-Torrequemadab, Jose M. Gonzalez-Correab,

Adoracion Carratala´ -Gimenez b, J.L. Sanchez-

Lizaso,2005, Brine discharge from the Javea desalination plant, Desalination, Vol. 185, pp : 87–94.

8. Jacqueline L Dupavillon, Bronwyn M Gillanders,

2009,Impacts of seawater desalination on the giant Australian cuttlefish Sepia apama in the upper Spencer

Gulf, South Australia, Marine Environmental Research.

9. Villanueva,R ; Moltschaniwskyj,N.A ; Bozzano A,2007, A biotic influences on embryo growth : statolith as

experimental tools in the squid early life history. Reviews

in fish Biology and Fisheries 17, pp:101-110. 10. Paulij,W.P ; Bogaards,R.H ; Denuce,J.M.1990, Influence

of salinity on embryonic development and the distribution of Sepia Officinalis in the Delta area South Western part of

the Netherlands; Marine Biology 107, pp:17-24.

11. Rachel Einav, Kobi Hamssib, Dan Periyb,2002,The footprint of the desalination processes on the environment,

Desalination, Vol. 152, pp: 141-154.

12. T.Bleninger, G.H. Jirka and V.Weitbrecht.2006, Optimal discharge configuration for brine effluents from

desalination plants, Proc. DME (Deutsche Meerwasser

Entsalzung) – Congress, 04 - 06. 04.; Berlin. 13. R. Zimmerman,1999, The Larnaca seawater desalination

plant, Environmental impact assessment.

14. Ahmed Hashim et Munneer hajjaj.2005, Impact of desalination plants fluid effluents on the integrity of

seawater, with the Arabian Gulf in perspective,

Desalination, Vol.182, pp: 373-393.

Please cite this Article as: Habet, L., Benrachedi, K., Study of dispersion of brine water into coastal seawater by using a pilot,

Algerian J. Env. Sc. Technology, 1:1 (2015) 33-39

33

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