Performance evaluation of industrial by-product phosphogypsum in the sorptive removal of nickel(ii) from aqueous environment

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1 Performance evaluation of industrial by-product phosphog in the sorptive removal of nickel(ii) from aqueous environment M.M. EL-Tyeb & S.R.Zeedan Sanitary and Environmental Engineering Department, Housing& Building National Research Center, Giza, Egypt. Raw Materials and Processing Department, Housing& Building National Research Center, Giza, Egypt. address: : Abstract: - The removal of Ni(II) ions from aqueous medium by phosphog was examined. The removal capacity of phosphog for Ni(II) ions was studied as a function of solution ph, contact time, adsorbent dosage and adsorbate concentration. The maximum adsorption of the Ni(II) ions on the phosphog was observed at the ph values between 9.5 and. The equilibrium time was attained after 3 min. and the maximum removal percentage was achieved at an adsorbent loading weight of gm/ml. The equilibrium adsorption capacity of adsorbent used for nickel was measured and extrapolated using linear Freundlich, Langmuir and Temkin isotherms and the experimental data were found to fit the Temkin isotherm model. Key-words: - Adsorption; Batch; Phosphog; Nickel; Wastewater; Isotherm. Introduction silver refineries,, zinc base casting and storage battery industries []. Higher concentration of nickel causes cancer of lungs, nose and bone. Dermatitis (Ni itch) is the most frequent effect of exposure to Ni, such as coins and jewelry. Acute poisoning of Ni(II) causes headache, dizziness, nausea and vomiting, chest pain, tightness of the chest, dry cough and shortness of breath, rapid respiration, cyanosis and extreme weakness [3]. According to World Health Organization (WHO) guidelines for drinking water [], the permissible level Ni(II) is. mg/l. Therefore, it is necessary to decrease the concentration of heavy metals to their permissible limits before their discharge to the environment. The EPA requires nickel in drinking water not to exceed. mg/l [5]. The permissible Brazilian limit for Ni (II) in wastewater discharge is. mg/l []. In recent years, various removal methods have been developed for the treatment of heavy metal containing wastewaters. Chemical precipitation, solvent extraction, reverse Nowadays, various metals are discharged into the water bodies. The sources of trace metals are associated with human activities. One of the metals released to the environment from a number of sources is nickel. Among the predominant aqueous forms of nickel in natural waters are Ni(II) and Ni(OH)3-. Nickel is an essential element but the levels required by both plants and animals are very low. At higher concentrations, it is known to be toxic to both plants and animals, whereas at very high levels of exposure, nickel salts are known to be carcinogenic []. Electroplating is one important process involved in surface finishing and metal deposition for better life of articles and for decoration. Although several metals can be used for electroplating, nickel, copper, zinc and chromium are the most commonly used metals, the choice depending upon the specific requirement of the articles. During washing of the electroplating tanks, considerable amounts of the metal ions find their way into the effluent. Ni(II) is present in the effluents of ISSN: ISBN:

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3 Table : Chemical composition of phosphog as oxides. concentrations. The stock solution ( mg/l) was acidified with drops of concentrated HCl to ph. The concentrations of Ni(II) ions in the supernatant were analyzed for metal content colorimetric according to standard methods for the examination of water and wastewater [], using the spectrophotometer (CECIL-CE 3), providing a light path of cm or longer. All chemicals used for preparing reagent solutions for analysis of metal ions were analytical grade reagent. Element.3 Batch experiments Adsorption experiments were carried out in 5mL capacity Erlenmeyer flasks. Given amounts of phosphog were added to ml of Ni(II) solutions in Erlenmeyer flasks and shacked at rpm and room temperature (GFL 3 Model Shaker). After agitating the solutions were filtered through whatman no. filter paper and the concentrations of Ni(II) ions in the filtrate were analyzed for metal content. The ph of each solution was adjusted to the desired value with.5n HCl and.5n NaOH solutions before the contact of adsorbent with metal ion solution. Each experiment was performed twice under identical conditions. Adsorption efficiency was expressed as a percentage of adsorbed metal compared to initial metal concentration, whereas adsorption capacity was expressed as amount of Ni adsorbed per mass unit of phosphog using the following equations, respectively: removal efficiency (%) = Co Ce /Co () qe (mg/g)= (Co Ce)V W () where Co and Ce are the initial and equilibrium concentrations of Ni(II) ion in the solution, respectively (mg/ L), V is the volume of solution (L) and W is the weight of the adsorbent (g). ;Q uartz G G G Q uartz ;Q uartz Û íñãíñ æ Þ ;Q uartz Counts/s Quantitative Composition (%) FeO3. CaO 3.9 MgO.53 NaO. K O. SO TiO.3 P O5. L.O.I.. TOTAL LOI*= Loss on ignition. 3 5 Position[ Theta] Fig.: x ray diffraction of raw PG.. Preparation of nickel solutions and analytical methods Metal solution hase been prepared and used in the laboratory. Simulated stock solution of Ni(II) ( mg/l) was prepared by dissolving required quantity of analar grade of nickel sulfate NiSO.HO (.7 g) salt in the distilled water. The stock solution was further diluted with distilled water to desired ISSN: Adsorption isotherm models 3 ISBN:

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5 Where B =RT/b () Temkin isotherm contains a factor that explicitly takes into the account adsorbing species adsorbent interactions. This isotherm assumes that (i) the heat of adsorption of all the molecules in the layer decreases linearly with coverage due to adsorbent adsorbate interactions, and that (ii) the adsorption is characterized by a uniform distribution of binding energies, up to some maximum binding energy [3]. A plot of qe versus ln Ce enables the determination of the isotherm constants B and AT from the slope and the intercept, respectively. AT is the equilibrium binding constant (l/g) corresponding to the maximum binding energy and constant B is related to the heat of adsorption. an increase in Zn (II) uptake with the increase in solution ph was reported by N. Balkaya and, H. Cesur, []. Ni(II) adsorption by phosphog increased with the increase in ph and reached a maximum in the ph range of Effect of contact time Figure (3) shows the effect of contact time on the removal of Ni(II) ions from aqueous solutions by PG. The metal uptake is rapid in the first 5 min. of contact period. Beyond the 3 min. contact time, the amount of Ni(II) adsorbed on the PG remains constant as shown in Figure (3) These data indicate that, the equilibrium is attained after 3 min. The nature of adsorbent and the available adsorption sites affect the rate of adsorption of Ni(II). The mechanism of solute transfer to the solid includes diffusion through the fluid film around the adsorbent particle and diffusion through the pores to the internal adsorption sites. In the initial stages of adsorption of Ni(II), the concentration gradient between the film and the available pore sites is large, and hence the rate of adsorption is faster. The rate of adsorption decreases in the later stages of the adsorption probably due to the slow pore diffusion of the solute ion into the bulk of the adsorbent. 3 Results and Discussion 3. Influence of process variables 3.. Effect of ph The ph of the aqueous solution is an important controlling parameter in the sorption process [33], and metal removal typically increases with increasing ph values. Solution ph controls (a) the solubility of metal hydroxides; (b) hydrolysis behavior of metals; and (c) surface charge of the sorbent. The effect of ph on Ni(II) adsorption by PG was given in Figure (). It can be seen from this figure that the minimum Ni (II) adsorption occurs in the ph range of 7.The low Ni (II) adsorption at low ph may be due to high acidity of solution, and the competition between the H+ and Ni (II) ions for the adsorption. The H+ ions are preferentially adsorbed over adsorbent surface. Thus, it hinders the positively charged metal ions to reach to the binding sites of the adsorbent. It is known that the solution ph affect both the solution chemistry and the surface binding sites of the PG [9]. Similarly, ISSN: Effect of adsorbent dosage Figures (a) and (b) show the effect of adsorbent dosage on Ni(II) adsorption. As it can be seen from (Figure a) that while the removal percentage of Ni(II) increased with the increase in adsorbent dosage, but the amount of Ni(II) adsorbed by unit weight of the adsorbent decreased (Figure b) and the maximum removal percentage was achieved at an adsorbent loading weight of gm/ml. It can be said that the decrease in the adsorbed amount with the increase in adsorbent dosage may result from the electrostatic interactions, interference between binding sites, and reduced mixing at higher adsorbent densities [3 3]. This 3 ISBN:

6 finding agrees with those of Gong et al. [37] for Cr(VI) removal by intact and pre-treated Spirulina maxima biomass, Yabe and de Oliveira [3] for metal removal by sequential adsorbent treatment (using solid adsorbents such as sand, silika, coal and alumina), Montanher et al. [3] for Zn(II) removal by rice bran, and Kwon et al. [39] for Zn(II) removal by scoria and for Zn(II) removal by phosphog [5]. q(mg/g) Time (min) Fig.3: Effect of initial contact time (initial concentration of Ni(II), mg/l; PG dosage, g/l; ph 9.5). 3.. Effect of adsorbate concentration The effect of initial adsorbate concentration on the adsorption was investigated by varying the initial concentration of Ni(II) between and. mg/l. The experimental data were illustrated in Figure 5. The results show that, with an increase in the Ni(II) concentration from to mg/l, the percentage removal decreases from 97.7% to 9.7% and the adsorption capacity increases from.97 to 9 mg/g. The decrease in the percentage removal of Ni(II) can be explained with the fact that, all the adsorbents had a limited number of active sites, which would have become saturated above a certain concentration. The increase in adsorption capacity with an increase in the Ni(II) concentration may be due to the higher adsorption rate and the utilization of all the active sites available for the adsorption at higher concentration [39,]. 9 (a) W eig ht ( g / ml) (b) 5 3. q (mg/g) W eig ht ( g / ml). Fig.: Effect of PG dosage: (a) Ni(II) removal (%) and (b) adsorbed Ni(II) (mg/ g) (initial concentration of Ni(II), mg/l; contact time, 3 min; ph 9.5). ph Fig.: Effect of initial ph (initial concentration of Ni(II), mg/l; PG dosage, mg/l; contact time, 3min.). ISSN: ISBN:

7 was. for similar adsorption on phosphog for Zn(II) [].Figure (7c) shows the Temkin plot. Values of Temkin parameters AT and B have been calculated from the curves and listed in Table (). The correlation coefficients of Langmuir, Freundlich and Temkin models are.959,.93, and.9 respectively. Therefore, the langmuir isotherm is well fitted with the experimental Data based on the negative values for the Langmuir isotherm constants obtained it can be seen from the obtained data that, Temkin equation can be fitted with a desirable R =.9. q(mg/g) 5 Concentration(mg/l) Fig. 5: Effect of initial Ni(II) concentration; PG dosage, g/l contact time, 3 min; ph 9.5). ISSN: qe mglg 3. Adsorption isotherms Adsorption isotherm for Ni(II) adsorption from aqueous solution on the PG is presented in Figure. The adsorption constants and correlation coefficients of the Langmuir,Freundlich and Temkin isotherms were given in Table. Figure (7a) shows the Langmuir plot. Values of Langmuir parameters B and (A/B) which corresponds to the maximum adsorption capacity (qmax) have been calculated from the curves and listed in Table () which indicate that, negative values for the Langmuir isotherm constants indicate the inadequacy of the isotherm model to explain the adsorption process [].Figure (7b) shows the Freundlich plot. Values of Freundlich parameters KF and n have been calculated from the curves and listed in Table (). Freundlich parameters (KF and n) indicate whether the nature of sorption is either favorable or unfavorable []. The intercept KF [(mg/g)/(mg/l)/n] is an indicator of sorption capacity and the slope /n is an indicator of sorption strength and a measure of the deviation from linearity of the adsorption. Smaller values of n(< ) (i.e. /n> a steep slope) mean that, sorption intensity is good or (favorable) at high concentrations but much less at lower concentrations [3], the adsorption bond is weak, a physical adsorption rather than chemical is probably dominant in Ni(II) adsorption by phosphog. The value of n Ce mgll Fig.: Equilibrium curve for the adsorption of Ni(II) on PG (PG dosage,g/ L; contact time, 3 min; ph 9.5). Table : Isotherms parameters for Ni(II) removal using PG. Langmuir parameters Qmax (mg/g) -.3 B (l/mg) R Frendlish parameters Kf n R AT (l/g) B R Temkin parameters 3 ISBN:

8 crystals. This indicates that it has a more complex composition than natural g, from figure b after adsorption of Ni(II),nickel ions appeared to cover the surface of PG and penetrate into the crystals (a) Ce/qe.5 y = x R = (a).5 Log qe (b) y = 3.9x -.37 R =.93 (b) Ce m g/l... Log Ce. y =.97x -.7 (c) R =.9 qe Fig.: SEM imaging of PG (a) before (b) after adsorption of Ni(II) (initial concentration of Ni(II), 5 mg/l PG dosage,g/ L; contact time, 3 min; ph 9.5). Conclusion.5 lnce.5 The present study showed that phosphog without any pretreatment seems to be an efficient and economical adsorbent for the removal of Ni(II) ions from aqueous solution. ph was a critical parameter for the Ni(II) uptake. Maximum adsorption was found to occur in the ph range of 9.5 and. The adsorption isotherms fitted well by the Temkin equation. It can be concluded that phosphog can be considered as an alternative approach for treatment of aqueous solutions polluted by Ni(II). Indeed, this method can be considered as a simple way in respect of handling and economical point of view since phosphog is a waste material.5 Fig.7: isotherm models for Ni(II) adsorption on PG (a) langmuir plot (b) Frendlish plot (c) Temkin plot. 3.3 The morphological characteristics The morphological characteristics of the adsorbent were evaluated by using a scanning electron microscope. SEM images for PG before and after adsorption of Ni(II) are shown in Figure (a,b). As shown in figure a PG has a well defined crystalline structure with the majority of rhombic and hexagonal shape ISSN: ISBN:

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