DEVELOPMENT OF A NEW ADSORBENT MATERIAL BASED ON MARINE SPONGES OF THE GENUS IRCINA: APPLICATION OF THE EXPERIMENTAL DESIGN METHODOLOGY \ SCREENING AND OPTIMIZATION\ .

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In this work, activated carbon was prepared from the by- product of marine sponges. The objective of this study is summarized in the development of an adsorbent material with a very interesting adsorption capacity, hence the interest to control the parameters influencing the functioning of the development process by exploiting it The screening plan \ Factoriel Complet\ . This technique minimizes the experiments and allows detecting the factors influencing the quality and the quantity which are: temperature, time and mass. Then the next step in this study was devoted to the optimization of the process of elaboration, using the response surface methodology ?Composite centered plan?. The optimal conditions with 55% of methylene blue adsorption capacity are obtained with 180.9minas activation time, 118.9?C as activation temperature and 7.33g for the mass of the raw material.
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  ISSN: 2320-5407 Int. J. Adv. Res. 5(8), 1725-1733 1725    Journal Homepage: -  www.journalijar.com   Article DOI:  10.21474/IJAR01/5237 DOI URL:  http://dx.doi.org/10.21474/IJAR01/5237 RESEARCH ARTICLE DEVELOPMENT OF A NEW ADSORBENT MATERIAL BASED ON MARINE SPONGES OF THE GENUS IRCINA : APPLICATION OF THE EXPERIMENTAL DESIGN METHODOLOGY SCREENING AND OPTIMIZATION . * Zineb Rhandour 1 , Meriem Tarbaoui 1 , Mina Oumam 2 , Belkassem El Amraoui 3,4, Ahmed Bennamara 1  andAbdelmjid Abourriche 1 . 1.   Biomolecular And Organic Synthesis Laboratory, Faculty Of Sciences Ben M’sik   University Hassan II- Casablanca, Casablanca, Morocco. 2.   Limat (Engineering Materials Laboratory), University Of Hassan II-Casablanca, Casablanca, Morocco. 3.   Faculty polydisciplinary of Taroudant, university ibn Zohr, Agadir, Morocco. 4.   Control quality in bio-control industry & bioactive molecules laboratory, faculty of sciences El jadida, Morocco. …………………………………………………………………………………………………… ....  Manuscript Info Abstract …………………….   ………………………………………………………………    Manuscript History Received: 21 June 2017 Final Accepted: 23 July 2017 Published: August 2017 Key words:- Marine sponge, Adsorbent material, screening, Experimental design, Optimization In this work, activated carbon was prepared from the by- product of marine sponges. The objective of this study is summarized in the development of an adsorbent material with a very interesting adsorption capacity, hence the interest to control the parameters influencing the functioning of the development process by exploiting it The screening  plan Factoriel Complet . This technique minimizes the experiments and allows detecting the factors influencing the quality and the quantity which are: temperature, time and mass. Then the next step in this study was devoted to the optimization of the process of elaboration, using the response surface methodology “Composite centered plan”. The optimal conditions with 55% of methylene blue adsorption capacity are obtained with 180.9minas activation time, 118.9°C as activation temperature and 7.33g for the mass of the raw material. Copy Right, IJAR, 2017,. All rights reserved. …………………………………………………………………………………………………… .... Introduction:- Liquid industrial effluents present a great danger to the aquatic environment which is the main site of industrial and urban waste. Industrial wastewater is causing enormous damage to the environment and health (Oumam et al.,2003)  . These releases have different degrees of harmfulness and this pollution is all the more dangerous because it is not known. In order to combat this dissolved pollution, several studies have been oriented towards economically acceptable processes using several techniques (Souabi et al., 1993 and Altinbas et al., 1995) . These techniques could be divided into three types of treatment, namely biological, dielectric and physico-chemical treatments (Wanassi et al., 2017 ). These include adsorption and ion exchange ( Tzvetkova et al., 2016) .The aim of this work is to develop adsorbent materials having an adsorption capacity from the extraction residues of the  Ircinia  marine sponge, adopting the experimental design methodology in first the screening plan in order to master the influence of factors on the process of elaboration, followed by an optimization of the process by adopting a composite plan centered. This study has guided us in translating the evolution of the performance of the materials developed according to the different operating factors influencing the process.   Corresponding Author:- Zineb Rhandour. Address:- Biomolecular And Organic Synthesis Laboratory, Faculty Of Sciences Ben M’sik   University Hassan II- Casablanca, Casablanca, Morocco.    ISSN: 2320-5407 Int. J. Adv. Res. 5(8), 1725-1733 1726 Materials and methods:- Sample: The marine sponges were collected in winter 2015 at the littoral Atlantic of El-Jadida (Morocco). All the sponges were identified by Dr. Maria-Jesús Uriz, Research Professor at the Centro de Estudios Avanzados de Blanes (CEAB) and Consejo superior de investigaciones científicas (CSIC) Spain. The collected materials were immediately frozen for one night prior to extraction  (Rhandour et al., 2016). Preparation of samples:- The extraction residues obtained from these sponges were chemically activated using (phosphoric/ sulfuric) acid 2M. The samples were baked overnight at 120 ° C. and heat-treated in air, in a muffle furnace, at different temperatures, the treatment time varied. The samples are then washed with distilled water in a Soxhlet for 72 hours, in order to extract the excess acid and the soluble material and then dried in the oven at 120 ° C. The products are ground (granulometry less than 100 µm)  (Tarbaoui et al., 2014). Experimental design methodology:- Screening plan  :- The first problems which experimental design can give the solution are these of screening parameters “Complete factorial plans “. This study permitted to deter  mine easily, among a large number of factors (k), those are significantly influenced to improve extraction process. This study will allow determining the effect of each level and for every factor, in objective to classify them in ascending order   (Fadil et al., 2014). The table (tab.1) presents the factors studied with real and coded level   . Table 1: Factors and their coded levels Factors Levels Coded Levels Temperature (°C) 180 -1 350 +1 Time (mn) 90 -1 180 +1 Mass (g) 5 -1 10 +1 Type of acid sulfuric -1  phosphoric +1 Pretreatment yes -1 no +1 Optimization plan:- Response surface methodology (RSM) is a statistical method that uses quantitative data from appropriate experiments to determine regression model equations and operating conditions ( Alam et al., 2007) . RSM is a collection of mathematical and statistical techniques for modeling and analysis of problems in which a response of interest is influenced by several variables ( Chaudhary et al., 2014 ). A standard RSM design called central composite design (CCD) ( Tarbaoui et al., 2015). Which allow solving the optimization problems by determining the optimal levels of the factors giving rise to a desired response. They constitute a second stage of the study after screening plans designed to identify the most influential factors  (Oumam et al., 2003). In order to optimize the  production conditions of our adsorbent material, the composite centered plane was used in order to reduce the number of experimental tests necessary for the evaluation of the parameters determined by the screening plan (activation temperature, time, and the treated mass of the material) and their effects on the adsorption capacity of methylene blue ( Marouane et al., 2012) . Statistical analysis:- The treatment of the results for the experimental models was carried out using experimental design software JMP. The adsorption capacity was compared with the ANOVA test, the Fisher Snedecor test and the student test. All statistical analyzes were carried out in P values (P <0.05).  ISSN: 2320-5407 Int. J. Adv. Res. 5(8), 1725-1733 1727 Results and discussion:- Screening plan:-  The Complete factorial plan is a pre-established plan in the JMP software. The experiment matrix is a table L8 (Tab. 2) which allows establishing the experimental plan . Table 2:- Experiment matrix of the material produced from the sponge  N° Test code Temperature (°C) X 1  Time (mn)X 2  Mass (g)X 3  Acid X 4  Pretreatment X 5  Adsorption capacity % 1 +−−++  350 90 5 phosphoric no 75.8 2 +++++ 350 180 10 phosphoric no 55.3 3 −−−− + 180 90 5 sulfuric no 55.196 4 −++−+  180 180 10 sulfuric no 21.41 5 −+−+−  180 180 5 phosphoric yes 13.4 6 −−++−  180 90 10 phosphoric yes 9.13 7 ++−−−  350 180 5 sulfuric yes 13.17 8 +−+−−  350 90 10 sulfuric yes 7.3 Validation of the model :- The quality of the adjusted model was expressed by the coefficient of determination R  2 , and its statistical significance was verified by an F test (analysis of variance) at the significance level of 5%. The linear regression of the model:- R  2  measures the proportion of the total change in the mean response explained by the regression, it is the correlation  between the observed and predicted response (Franco ., 2008) . The goodness of the model is judged if the linear of regression coefficient is equal to or higher than 0.80 (Rhanzi. N et al., 2015) . The linear analysis of regression as established by the experimental design JMP software are shown in the Figure 1. The calculated values of the coefficients of determination of the multilinear regression R2 equal to 0.99 is close to 1 and adjusted R  2A  which is 0.97 (Tab.3) make it possible to confirm the validity of the model. Figure 1:-  Linear regression of Adsorption capacity  Table 3:- Adjusted regression analysis of adsorption capacity.   R square 0.99 Adjested R square 0.97 Root of square error of average 4.73 Average of the reponse 31.33 Observations (or weighted sums) 8  ISSN: 2320-5407 Int. J. Adv. Res. 5(8), 1725-1733 1728 Variance analysis:- The variance analysis is based on the comparison of the variance of the established model with the variance of the residue, using the Fisher Snedecor test. For the model to be very significant at 95% , it is necessary that: Fexp >> Fα,  ν mod , ν res   where α = 0.05. The results of the ANOVA given by the JMP software are shown in Table 4. The results of analysis of the variance between the established model and the residue give an experimental factor Fexp (variance of the model / variance of the residue) = 43.75. From the results, we have Fexp = 43,75 >> Fthéo, the condition of the Fisher Snedecor test is verified, so the regression is significant with a confidence threshold of 5%. The probability Prob> F is the P-value associated with F value given by the statistical software JMP. It was compared to the risk α = 0.05, then the P - value is strictly less than α = 0.05, this model is significant.   Table 4:- ANOVA test Study of selected factors:- Factors Statistically not negligible:- Table 5 shows an increase in the adsorption capacity of methylene blue from low temperatures to high temperatures, while with the increase in processing time and mass a decrease in adsorption capacity is observed. The t-test for the temperature, processing time, and mass coefficients showed that these factors influence process operation because their risks are significant (<0.05). Factors Statistically negligible:- The pretreatment and the type of acid are the factors which do not affect the process of production of adsorbent, and therefore will be removed from the study. The screening plan helps to demonstrate the parameters which have little influence on the adsorption capacity and therefore choose those which appear to be more influential. These will be studied more precisely in the next section to allow better control of the process. Table 5:- Significant effects  Optimization of the conditions for the preparation of adsorbent materials by the experimental design method Composite centered plan :- The results obtained in the previous part of this study allowed to choose the most influential variables on the adsorption capacity of the prepared material namely temperature, treatment time and mass. The next step of this study will be devoted to the optimization of the process of elaboration. The easiest way is to choose a plan of experiments with faces centered whose matrix and the experimental values of adsorption capacity are represented in Table 6.The exploitation of the results obtained for the response was carried out with the same approach. The evaluation of the overall quality of the postulated model makes it possible to know whether it adequately summarizes the results of the tests of the experimental design. The evaluation of the overall quality of the postulated model allows knowing if it adequately summarizes the results of the tests of the experimental design. Source Degrees of freedom Sum of squares Average square F value Modele 5 1224.22 244.84 43.75 Residue 2 11.19 5.59 Prob. > F Total 7 1235.42 0.0225 Terme Estimation Standard deviation T value T value Prob.>|t| Temprature -10.29 0,83 -12.31 0.0065 Time -4.026 0.83 -4.81 0.04 Mass -3.53 0.83 -4.23 0.05 Acid (sulfu) 3.27 0,83 3.92 0.0594 Pretraitement (yes) -2.75 0.83 -3.30 0.0809
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