ISSN : 0976-7045
EISSN : 0976-7053
EL FADEL H.1, MERZOUKI M.2*, FAOUZI M.3, LAAMAYEM A.4, NAJEM M.5, BENLEMLIH M.6
1Faculty of Science, Dhar El Mahraz, PO Box: 1796, Atlas-Fez, University Sidi Mohammed Ben Abdellah, Fez, Morocco.
2Faculty of Science, Dhar El Mahraz, PO Box: 1796, Atlas-Fez, University Sidi Mohammed Ben Abdellah, Fez, Morocco.
3Faculty of Science, Dhar El Mahraz, PO Box: 1796, Atlas-Fez, University Sidi Mohammed Ben Abdellah, Fez, Morocco.
4Laboratory of Environmental Physics, Faculty of Science, PO Box: 24000, El Jadida, Morocco.
5Laboratory of Environmental Physics, Faculty of Science, PO Box: 24000, El Jadida, Morocco.
6Faculty of Science, Dhar El Mahraz, PO Box: 1796, Atlas-Fez, University Sidi Mohammed Ben Abdellah, Fez, Morocco.
* Corresponding Author : merzoukimo@yahoo.fr
Received : 12-12-2012 Accepted : 15-01-2013 Published : 11-03-2013
Volume : 4 Issue : 1 Pages : 51 - 59
J Biotechnol Lett 4.1 (2013):51-59
Conflict of Interest : None declared
This study focuses on the slow filtration of leachates by marine sands and matrix formed by clays A1 and fly ash which have already given a satisfactory reduction of physicochemical pollution for the same leachate [1]. The determination of sand particle sizes and the mineralogical characterization of sand is an essential step to choose the best samples of sand filter. The filtration device selected allowed us to reach high removal rate for all parameters. The removals rates of COD, BOD5; SS; TP; Electrical conductivity and TKN were 78,46%; 96,13%; 90,23%; 98,54%; 81,53% and 44,82% respectively, according to Moroccan norms of indirect discharges. The metallic ions Al, Cd, Cr, Cu, Fe, Mn, Ni, Pb and Zn are strongly retained with the concentrations less than Moroccan norms of direct discharges, especially for iron with an abatement rate of 99,32% and a concentration < 0,1 mg/L and chromium with an abatement rate > 97,8% and a concentration of 0,2 mg/L. The fecal coliforms and fecal streptococcus are effectively reduced with respective rates of 96% and 92,80%. The use of this filtration technique using dropouts materials, whose investment costs are lower and the sustainability is more great both technically and financially, seems the best convenient solution for developing countries.
Leachate, Filtration, Fly ash, Clay, Sands.
Since always the water was inseparable from human activity, the depletion of water resources and the degradation of their quality is a major challenge. Indeed, one of the factors that govern the development of human society is the concern to obtain and maintain an adequate supply of water.
In Morocco, the increasing production of household and industrial waste causes critics pollution problems. The increasingly complex and heterogeneous nature of waste involves difficulties for their treatment and management. Much is landfilled without precautions, which is a real and continuing threat to the environment. The controlled dumping site of Fez in Morocco receives more than 800 tons per day of waste of any kind and could reach 950 tons per day in the summer season.
Indeed, since the deposition phase, the waste is submitting to degradation processes associated with biological and physicochemical complex reactions. The water seeps and produces leachate charged of organic and mineral substances that cause a mainly organic and metallic pollution type. These leachates are a source of surface water and groundwater contamination if they aren’t properly treated. Apart to their often substantial pollution load, the leachate must undergo purification treatment before being discharged into the natural environment.
There are various methods of intensive treatment type, requiring energy sources for their running and heavy maintenance loads, the choice of sand filtration technique is often the most economical method in developing countries such as Morocco and offers advantage of high efficiency and simple operation. Thus, it accorded the needs of improving water quality while offering the opportunity to involve the community in the management, maintenance and plant operation.
• A physicochemical characterization of raw leachate ;
• A mineralogical analysis and a determination of particle sizes sands for choose the best samples for the leachate filtration;
• An assessment of the treatment performance of the filter device selected through the physicochemical and bacteriological filtrate analysis.
Materials
The apparatus listed in [Table-1] were used.
Physicochemical parameters
The physicochemical parameters which have been the subject of this study are: Chemical Oxygen Demand (COD), Biological Oxygen Demand (BOD5) Total Kjeldahl Nitrogen (TKN) Total Phosphorus (TP), Suspended Solids (SS), Electrical conductivity and colour removal from leachate. The latter parameter was obtained using the following formula:
Where DOi and DOf are the initial and final optical density of the colour from leachate, respectively, assayed at 455 nm [2] .
Two types of bacteria were analysed for to evaluate the treatment performance of the filtration system in terms of germs reduction. These are fecal coliforms (FC) [3] and fecal streptococcus (FS), indicators of fecal pollution. The bacteriological analyses were performed according to the method described by Marchal and Maury [4,5] .
Analysis Technique of Filter Substrates
Different analyses techniques are performed for filter substrates including:
• Analysis particle size: the size distribution curves were established by passage through sieve columns according to standardized method NF P 18-560;
• Chemical analysis by X-ray fluorescence technique;
• Mineralogical analysis by X-ray diffraction (XRD);
• Analyses by inductively coupled plasma atomic emission spectroscopy (ICP-AES).
For to determine the heavy metals concentrations, a taking of sample test to be analyzed is submitted to acid attack. The acids used are HNO3 and HCl. After the dissolution of all the elements, the solution is filtered and then analysed by ICP. ICP analyses were performed in the laboratory REMINEX Marrakech (Morocco).
Our experimental device is constituted of a glass column with a dimension of 6 cm in diameter and 50 cm in height. The effective height of the filter bed is 36 cm (Hs), 14 cm is used for the raw leachate (HE), which is maintained constant along the experiments in order to keep the same load of leachate on the filter bed [Fig-1] .
The leachate is collected from the controlled dumping site of Fez, located southeast of the city of Fez, in Ouled Mhamed Sidi Harazem road, it spreads over an area of ​​120 hectares. The general collector leachate records a flow rate of 15 l/min.
The filter bed consists of five marine sands samples chosen from nine. These sand samples are collected along the coast of the city of El Jadida, washed with distilled water and then dried in an oven at a temperature of 50°C for 24 h. These sands are then added to the matrix formed by natural clay designated A1 and fly ash.
The method is based on the following principle: a slow filtration, the leachate passes under a constant load (14cm of leachate) through the filter bed, the load is kept constant along the experiments.
Physicochemical Characterization of Leachates
It is difficult to accurately determine the leachates properties because they evolve in time and space [6] . The volume of leachate required for this work was taken from a storage tank leachate. This sample was transported directly to the laboratory and stored at 4°C for 1 day before use. All the tests were performed in triplicate and the average values ​​are determined according to AFNOR standard techniques.
[Table-2] summarizes the main physicochemical properties of leachate from controlled dumping site of Fez with the Moroccan norms of indirect discharges.
As to the landfill aged and the waste stabilised, the organic load reduces and the volatile fatty acids scarce (20 to 30% of the load of leachate) in favor for compounds of high molecular weight. The emergence of these compounds tends to decrease the biodegradability of leachate. Therefore, the pH is near neutral generally corresponding at the stable methanogenic phase [7] .
The contents in COD and BOD5 are respectively 5200 mg/L and 1375,12 mg/L, these are indicators of organic pollution of leachate. This polluting power of leachate comes mainly from the domestic use of detergents, pesticides, solvents, and also from storm water: runoff on agricultural land, on road network, etc. It can also come from industrial discharges or even from disinfection treatments of effluent by chlorine (haloforms) [8] .
The COD/BOD5 ratio gives information about the biodegradability of waste. Applied at leachate from controlled dumping site of Fez, the COD/BOD5 ratio is 3,78 indicating that these leachates are stabilized and poorly biodegradable [9] .
The kjeldahl nitrogen comprises nitrogen in ammoniacal and organic forms, excluding nitrous forms (nitrites) and nitric form (nitrate). The origin of organic nitrogen may be the decomposition of organic waste, the human or animal organic waste (urea), adjuvants of some detergents.
Kjeldahl nitrogen concentration detected in the landfill leachate from the city of Fez achieved 3146,5 mg/L, which is comparable to the results obtained on landfill leachate from the city of Mohammedia: 3000 mg/L [10] .
For the phosphates released into the environment, they are partly responsible for the eutrophication of watercourse. However, the N/P ratio indicator of eutrophication state [11] shows the values ​​exceeding the threshold of 29, which indicates the possibility of the presence of cyanobacteria. This low content in total nitrogen and in total phosphorus of landfill leachate from Fez is explained by their consumption by the biomass with the production of CO2 and H2 [12] .
The electrical conductivity is closely related to the dissolved substances concentrations and to their nature. The leachate studied have a very high electrical conductivity in the order of 37,9 ms.cm-1, due to the highly mineralised landfill leachate [13] .
Results of Sands Analysis
Particle size analysis
Curves from [Fig-2] to [Fig-10] represents the particle size distribution of each sand sample according to its size.
The results of particle size analysis indicate that the sands 1, 3, 4, 5, 8 and 9 have the predominant size of 160 µm, while the sands 2 and 7 have the same major size of 250 µm. On the other side, the sand 6 has a different size of 500 µm, so generally formed by crushed shells. This particle size distribution allowed us to deduce the Uniformity Coefficient (UC = d60/d10) characterizing each sand sample.
The sands 3, 4, 5, 8 and 9 are chosen for the leachate filtration because of:
• Their low particle size (160 µm) so they will have the best treatment performance of leachate into increasing the adsorption surface, due to the decrease of grain size of adsorbent;
• Their Uniformity Coefficient UC which is and must be less than 1,5 [14] knowing that more the value of UC is close to 1, the homogeneity for the filter bed is better [14] ;
These five sand samples were subsequently analysed by ICP, firstly for to know their exact chemical composition and secondly for to determine if there is a probable contamination by the heavy metals, knowing that these sand samples will be used as the filter substrates for the leachate.
The results of this mineralogical analysis by ICP are shown in the histogram of [Fig-11] .
The five sand samples contain various chemical elements. The most significant concentrations concern the silica (SiO2) and the lime (CaO). The lowest value was recorded for the titanium dioxide (TiO2).
Chemical Analysis
[Table-3] summarizes the medium values ​​expressed at an oxide percentage of different elements contained in fly ash and in the clay soil A1 [1] .
For the clays A1, the sum of the oxides proportions identified is 100%. It consists principally by the silica in the quartz form (46,27%). It also contains a substantial content in alumina (12,7%) and in calcium oxide (12,5%).
For the fly ash, the sum of the elements percentages: SiO2, Al2O3, and Fe2O3 is 94,4%, which can be classified among the silico-aluminous ash.
For the clays A1, this analysis allows to highlight the different mineral phases of soil A1, according to their interplanar spacings. The result of X-ray diffraction is shown in [Fig-12] .
The X-ray spectra analysis shows that the soil A1 is mostly composed by quartz followed by the magnesium calcite. These minerals types are the origin of the clays basicity.
For fly ash, the X-ray diffraction analysis revealed the existence of two peaks: the quartz and the mullite. This result is explained by the coal mineralogy used which is generally composed by the crystallised silica in quartz form and the phyllitic minerals of the clays group (shales) [1] .
Cheriaf et al [15] studies showed that the fly ash are pozzolanic, that means when they are mixed with lime, they tend to react and form stable calcium silicate hydrates CSH as shown in [Fig-13] . This property is called pozzolanicity. The pozzolanic power is manifested by two successive phenomena: the combination with the lime to form the insoluble compounds then the curing.
Physicochemical Results of Leachate Filtration
The [Table-4] shows the results obtained after the passage of raw leachate through the filter material bed. At the bed surface, a thin layer is formed called "biological membrane" or biofilm. This thin layer is essential, because this is where the purification process takes place.
The results of [Table-4] revealed the removal rates of different physicochemical parameters with the concentrations strongly less than the Moroccan norms of indirect discharges.
The COD reduction rate achieved 78,46% which is comparable to the result obtained for the leachate from AL Hoceima [16] . The content in COD obtained is estimated at 1120 mg/L close to the Moroccan norm of indirect discharge (1000 mg/L).
We also find a BOD5 removal rate estimated at 96,13%, a removal rate strongly higher than that founded for the leachate from AL Hoceima [16] : between 60% and 67% at the exit of the bed sands. The content in BOD5 obtained is 53,12 mg/L, significantly less than the Moroccan norm of indirect discharge (500 mg/L).
These COD and BOD5 reductions are explained by the physicochemical characteristics of sands:
• The richness in silica exceeding 51% for each sand, it is a strong adsorbent with high electrical polarity ;
• The low sand size not exceeding 160 µm, which permitted to increase the specific adsorption surface;
• Iron ions contribute to neutralise the negative charges of organic matter of leachate.
The organic load reduction of COD and BOD5 affects the leachate colour. This colour reduction of leachate achieved 97,80% with a pale yellow colour, it’s a discolouration accompanied by a deodorization which explained by the high adsorption capacity of sands and clays.
There is also a maximum reduction of suspended solids up to 90, 23% with a concentration of 42 mg/L, significantly less than Moroccan norm of indirect discharges (600 mg/L). This elimination of SS could be explained by the physical characteristics of sands filters with UC < 1,5 which permitted to reduce load losses and get a retention in depth of suspended solids [14] .
The organic matter has ceased to be available in mass and spawned a series of cascade reactions: the first effect, a decrease of microbiological activity causing a drop of amounts of organic material degraded (BOD5 and COD), thus limiting the mineralization of inorganic substances. Therefore, a significant decrease of the electrical conductivity is recorded up to 81,53%. This high reduction of the electrical conductivity can also be explained by the retention of dissolved salts contained in the leachate (sulphates, calcium, sodium, magnesium, chloride ...) by sandy and clayey materials of the filter bed.
We also note that there's almost total reduction of total phosphorus to 98,54%, with a concentration of 9,51.10-3 mg/L in the leachate filtered. This large reduction is due to the richness in ferric oxides, aluminum oxides and lime contained in marine sands (exceeding 27% for each sand), in fly ash (CaO + Σ% Al2O3 + Fe2O3 = 47,4%) and in clay soil (exceeding 30%). These oxides are considered as precipitating for the physicochemical removal of phosphorus giving insoluble precipitates of metallic phosphates.
The Kjeldahl nitrogen reduction is estimated to 44,82% with a concentration of 1736 mg/L in the filtered leachate. Indeed, the pH of the filtrate 7,8 is into the optimum range of pH (7,5 to 8,5) favoring the ammonia nitrification which is converted to nitrate, through bacteria of the genus of Nitrobacter, Nitrocystis, Nitrospira, Nitrococcus.
We analyzed the metallic elements (Al, Cd, Cr, Cu, Fe, Mn, Ni, Pb and Zn) in the raw leachate and the filtrate. Each value is the medium obtained after four sampling [Table-5] the concentrations of heavy metals in raw leachate which revealed considerable concentrations of iron, chromium, aluminum, manganese and zinc. Cadmium level was almost negligible. The iron concentration reached 14,65 mg/L, this metal is considered among the major stainless steel having an important role in numerous areas: daily life, mechanical industry, food processing, chemistry, medicine and surgery [17] .
The chromium concentration in the leachate reached 4,554 mg/L such as the concentration detected in the landfill leachate from Mohammedia (5mg/L) [10] and remains higher than the value measured in Akreuch dumping (35-120 µg/L) [18] . This is because many industrial units of tannery are installed in Fez. The chromium ion may originate from other types of waste collected with household waste such as cardboard paper and wood (total Cr = 25 mg/g of paper and 80 mg/g of wood) [19] .
It should be noted that the dumping site of Fez receives all variety of urban waste and some industrial waste like food industrial waste into absence of regulation leading a rigorous management for dumping site.
The lead concentration reached 0,215mg/L, it is related to the industrial waste, particularly in the printing areas and the paint manufacture of [Table-5] shows that the leachate treatment by this filtration process further reduces heavy metals with concentrations less than the Moroccan norms of direct discharges and with removal rate higher than those founded after 7 days of leachate treatment by aeration [20] .
The variability of removal rate of metals is due to the ionic form of each metal, the ability of each bacterium to accumulate the metal and the physicochemical conditions that differ from one organism to another for ensure the metals abatement.
Iron ions which recorded the highest concentration in the raw leachate and persisted at the treatment by aeration [20] , are now strongly reduced with the high reduction rate of 99, 32% and a concentration < 0,1 mg/L strongly less than the norm (3 mg/L).
Chromium ions has an abatement rate > 97,8% with a concentration of 0,2 mg/L, strongly less than the norm of directs discharges (2 mg/L). This metal has always presented a major problem for the leachate from Fez, caused by industrial solid waste (tannery) of the city without any prior treatment.
After filtration, the contents in heavy metals of leachate accorded the Moroccan norms of direct discharges. Indeed, with the richness in silica of sand, the surface hydroxyl groups are formed by hydration which allows the adsorption of metallic cations [21] . The pozzolanic fly ash used react with lime of sands, this reaction produces stable calcium silicate hydrates CSH and further allows the stabilization of heavy metals [22] by various mechanisms:
• Mechanical trapping: the metallic contaminants can react as nucleation center and remain trapped in the hydrate thus formed [23,24] .
• Integration into hydrates: CSH can incorporate metallic contaminants by substitution (especially for aluminum and iron) in the crystalline lattice and have the ability to trap these contaminants in their interlayer space [25] This explains the high elimination of iron and aluminum of raw leachate;
• Adsorption: CSH have a good adsorption capacity [26] .
Being good adsorbents, the ferric oxides and aluminum oxides contained in the ash (Σ% Al2O3 + Fe2O3 = 47, 4%) in the clay soil (18%) and in marine sands (9% each sand) have an important role for the retention of metallic ions [22] .
Although rare, the manganese oxides of sands play also an important role because they have a particular affinity for some heavy metals (Cu, Zn, Ni, Pb ...) which they can adsorb in large amounts [27] .
The research of pathogen germs specifically, is too costly and uncertain, which why we seek the fecal contamination germs (fecal coliforms and fecal streptococcus) to estimate the possible presence of pathogen germs. Indeed, there is a correlation between the presence of these indicators bacteria of fecal contamination and the presence of pathogenic bacteria [8] . The results of this analysis are shown in [Fig-14] .
The bacteriological analysis of raw leachate shows that fecal coliform (FC) and fecal streptococcus (FS) are present at low concentrations in the order of 1,65x104/100 ml and 1,39x104/100 ml, respectively. The survival of fecal bacteria in these waters may be several months [28,29] . The reduction rate of fecal coliforms and fecal streptococcus are 96 % and 92,80 %, respectively. The medium number of FC is 660 bacteria per 100 ml, this low content reflects a good bacteriological quality of treated leachate because the water containing 4,3x105 FC per 100 ml reached the bacteriological quality required for unrestricted irrigation [30] . The medium number of FS showed also a significant decline with 1000 bacteria per 100 ml in the treated leachate, but as in most cases, the mortality of FC was higher than that of FS according to the results of other studies [31,32] . However, the FC/FS ratio can provide information about the fecal contamination origin [33,34] although the significance of this ratio is sometimes disputed [34] .
Filters sand can reduce the fecal contamination germs. Indeed, the soil has an important purifying power whatsoever on the physicochemical and microbiological plane [35-38] .
The major decontamination in bacterial load of leachate is ensured by the particle size characteristics, the thickness of the clogging layer, the thickness of the layer of filtered water, the frequency and periodicity of water inputs at the sand filters [39] . Thus, the bacteria retained by filtration or adsorption undergo a decline ensured by the soil microflora [40] . Also, the biological mechanisms namely predation of bacteria by the soil protozoa seems to have a significant effect on the bacterial load elimination [36,40,41] .
Summarizing, the leachate filtration by marine sands added to the matrix formed by clay A1 and fly ash, allowed us to identify the following points:
• The richness in silica of sands allows a higher reduction of COD and BOD5 in a respective order of 78, 46 % and 96, 13% and a good adsorption of metallic cations;
• Sands used have uniformity coefficients UC< 1,5 which allowed a retention in depth of suspended solids;
• The pozzolanic reaction between fly ash and lime of sands promotes the stabilization of heavy metals of leachate with contents less than Moroccan norms of directs discharges;
• The richness in metallic oxides in substrates filter allows the total phosphorus reduction;
• Sands filter allows an important reduction of fecal contamination germs ;
• The filter substrates selected can be used for the landfill leachate treatment in big scale.
Al- Aluminum
Al2O3- Aluminum oxide
BOD- Biological Oxygen Demand
CaO- Lime
Cd- Cadmium
COD- Chemical Oxygen Demand
Cr- Chromium
CSH- Calcium Silicate Hydrates
Cu- Copper
FC- Fecal Coliforms
Fe- Iron
Fe2O3- Ferric oxide
FS- Fecal Streptococcus
ICP- AES-Inductively Coupled Plasma - Atomic Emission Spectroscopy
K2O- Potassium oxide
MgO- Magnesium oxide
MnO- Maganese oxide
Mn- Manganese
Ni- Nickel
Pb- Lead
SiO2- Silica
SO3- Sulfur trioxide
SS- Suspended Solids
TiO2- Titanium dioxide
TKN- Total Kjeldahl Nitrogen
Total P- Total Phosphorus
UC- Uniformity Coefficient
XRD- X-ray diffraction
Zn- Zinc
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 | Fig. 1- Experimental Device |
 | Fig. 2- Particle size Distribution Curves of Sand 1 |
 | Fig. 3- Particle size Distribution Curves of Sand 2 |
 | Fig. 4- Particle size Distribution Curves of Sand 3 |
 | Fig. 5- Particle size Distribution Curves of Sand 4 |
 | Fig. 6- Particle size Distribution Curves of Sand 5 |
 | Fig. 7- Particle size Distribution Curves of Sand 6 |
 | Fig. 8- Particle size Distribution Curves of Sand 7 |
 | Fig. 9- Particle size Distribution Curves of Sand 8 |
 | Fig. 10- Particle size Distribution Curves of Sand 9 |
 | Fig. 11- Results of ICP analysis of sand samples |
 | Fig. 12- X-ray Diffraction Pattern of the Clay Soil A1 |
 | Fig. 13- Enlarged Image of the Pozzolanicreaction of fly ash |
 | Fig. 14- Evolution for Fecal Coliforms Counts (FC) and for Fecal Streptococcus Counts (FS) of Leachate after Filtration |
 | Table 1- Apparatus Used |
 | Table 2- Physicochemical Characteristics of Landfill Leachate from Fez |
 | Table 3- Chemical Composition of Clay A1 and Fly Ash Expressed in Weight Percentage (%). |
 | Table 4- Physicochemical Characteristics of Leachate before and after Filtration |
 | Table 5- Heavy Metals Analysis of Leachate before and after Filtration |