ГОДИШНИК НА МИННО-ГЕОЛОЖКИЯ УНИВЕРСИТЕТ “СВ. ИВАН РИЛСКИ”, Том 56, Св. II, Добив и преработка на минерални суровини, 2013 ANNUAL OF THE UNIVERSITY OF MINING AND GEOLOGY “ST. IVAN RILSKI”, Vol. 56, Part ІI, Mining and Mineral processing, 2013 EVALUATION OF ACTIVATED CARBON „NORIT CA1“ SORPTION AS A METHOD FOR HEAVY METAL IONS REMOVAL FROM WASTEWATER Georgi Nikolov, Gospodinka Gicheva University of Mining and Geology “St. Ivan Rilski”, 1700 Sofia, e_gospodinka@yahoo.com ABSTRACT. The Heavy metal pollution is one of the most serious problems concerning environment. Release of heavy metals is contributed mainly to mining industry thus making it a major concern to industrially developed countries. Heavy metals pose a great hazard to human health due to their acute and chronic toxicity, tendency for bioaccumulation and carcinogenicity. One of the industrially used methods for the removal of the ions from wastewater is the process of sorption. Here we present the investigation of sorption capacity of activated carbon Norit CA1 toward Cd(II) and Zn(II) as a method for their removal from wastewater. The effect of pH of the media was studied as a way to evaluate the optimal conditions for water treatment process. ОЦЕНКА НА СОРБЦИЯТА ВЪРХУ АКТИВЕН ВЪГЛЕН „NORIT CA1“ КАТО МЕТОД ЗА ПРЕЧИСТВАНЕ НА ОТПАДНИ ВОДИ ОТ ЙОНИ НА ТЕЖКИ МЕТАЛИ Георги Николов, Господинка Гичева Минно-геоложки университет “Св. Иван Рилски”, 1700 София, e_gospodinka@yahoo.com РЕЗЮМЕ. Замърсяването с тежки метали е един от най-сериозните проблеми засягащи околната среда. То се отдава главно на минната индустрия и поради тази причина е основен проблем в развитите страни. Тежките метали представляват сериозна заплаха за човешкото здраве поради тяхната остра и хронична токсичност, канцерогенност, както и склонността им към биоакумулиране. Един от най-разпространените методите за отстраняване на йони от отпадни води е процеса сорбция. В това изследване е определен сорбционният капацитет на активен въглен Norit CA1 спрямо йони на Cd(II) and Zn(II), като метод за тяхнотот отстраняване от отпадни води. Изследвана е и зависимостта от и йонната сила на средата, за да се оценят оптималните условия за пречистване на замърсените води. Ключови думи: тежки метали, сорбция, активен въглен Introduction been developed – photocatalysis (Lazar et al., 2012; Nakata, K. et al., 2012). Although there are a large number of research papers in the past ten years regarding the advantages and the prospects of this method it is still not employed as an industrially applied water treatment process. Heavy metal pollution is one of the most pressing problems presenting a challenge in engineering a cost effective as well as efficient process for their removal from contaminated waters. Pollution with heavy metals is a problem emerging in industrially developed countries with well pronounced mining industry. Heavy metals are usually a waste accompanying the process of metal extraction, mineral processing, metal plating. Although there isn’t a uniform (unanimous) definition of heavy metal it is usually associated with elements with metallic properties and high atomic weight. Heavy metal ions are well known for their toxicity, both acute and chronic as well as their carcinogenicity. Their release in environment can pose a serious health hazard due to their tendency for bioaccumulation and biomagnification (Paulino et al., 2006; Borba et al., 2006; Oyaro et al., 2007). Each of the above listed methods has its advantages and disadvantages regarding their cost, efficiency and selectivity towards heavy metal removal from wastewaters. Adsorption as a process for water purification is probably one the most widely applied worldwide due to its cost efficiency, versatility and high removal efficiency. Different types of adsorbents have been applied for water purification – both synthetic and naturally occurring. Amongst the ones that have attracted the attention of researchers due to their excellent qualities are zeolites (ElKamash et al., 2005; Kocaoba et al., 2007; Jamil et al., 2010; ), activated carbon (Kang et al., 2008), clays (kaolinite and montmorillonite: Bhattacharyya et al., 2008) as well as polymer-based materials (Liu et al., 2010; Kiani et al., 2011; Ma et al., 2012). Activated carbon is meso- and microporous material obtained mainly from wood and coal. It can be activated by chemical or physical methods and depending on that the properties of activated carbon can vary significantly. The origin and the type of activation determine the specific area, pore size and volume, as well surface functionality. It is one of the most widely used sorbent due to his high sorption capacity combined with its versatility and cost efficiency. A lot of methods for heavy metal ions removal were developed including chemical precipitation (Huisman et al., 2006), ion-exchange (Petruzzelli et al., 1995), membrane filtration (Shaalan et al., 2001; Landaburu-Aguirre et al., 2009), reverse osmosis (Mohsen-Nia et al., 2007; Muthukrishnan et al., 2008), dialysis (Mohammadi et al., 2005), adsorption (; Mohan et al., 2006; Liang et al., 2010; Liu et al., 2011), electrochemical methods (Roundhill et al., 2002) and etc. Recently a promising new method for a water treatment has 135 Experimental part metal ion removal. In that case the predominant is electrostatic interaction between the functional groups on surface of AC and the metal ion. Norit CA1 is referred as so called L carbons (low temperature activation), which is associated with the formation of acidic groups on their surface and negative zeta potential as well as their ability to adsorb metal ions (Corapcioglu et al., 1987). This interaction is dependent on the pH of the media, ionic strength and temperature. Chemicals. Activated charcoal Norit® CA1 was purchased from Sigma-Alrdich and used as obtained (without any further treatment). Cd(CH3COO)2, KCl, CH3COONa, Zn(NO3)2.6H2O (purum) were obtained by Valerus, Bulgaria. Solutions. Solutions of heavy metal ions were prepared by dissolving the heavy metal ion containing compound in media with different pH in order to obtain a solution of heavy metal ion at different pH with concentration 0.2 M (mol/l) to use as a starting solution, respectively. The selected buffer solutions used in our experiments were with pH value of 2.7 (KCl/HCl), 4.8 (AcOH/ NaOH) and 0.1 M ionic strength and distilled water (pH 6.5) and natural water (pH 7.8). Concentration of Cd2+ and Zn2+ ion in the experiments were determined by complexonometric titration. Here is presented the pH and ionic strength dependence of the adsorption of Cd(II) and Zn(II) ions onto Norit CA1. Four different pH media with two different ionic strength were tested. The results from obtained from adsorption of the metal ions were processed using the linear form of Freundlich isotherm, where q is the mass concentration of the adsorbed metal ion per mass of sorbent (q) and its concentration in the solution at equilibrium (CM). Material characterization. The surface morphology of the activated carbon was revealed by scanning electron microscopy SEM (JEOL JSM-6390) – Figure 1. The analysis of the specific surface was conducted by the express method (Klyachko-Gurvich) with N2 sorption at low temperature. It has been determined to be 980 m2/g. Usually parameter K (intercept) is associated with the sorption capacity of the material while 1/n (slope) is connected to the sorption rate. Fig. 1. SEM image of activate carbon of Norit® CA1 Fig. 2. Linear plot of Freundlich isotherms for adsorption of Cd(II) ions onto Norit CA1 at different pH values log( q) 1 log CM log K n (1) As it is shown on Figure 2 the adsorption capacity of Cd(II) ions onto Norit CA1 is practically not affected by the pH media (with slight exception of pH 7.8-mineral water). The parameters K and 1/n are the same for the pH 2.7; 4.8 and 6.5, meaning that Cd(II) are adsorbed with the same rate and amount onto Norit CA1 at that conditions. Adsorption onto Norit CA1. The adsorption isotherms were studied under static conditions in series of six samples. Exact amount of Norit CA1 was placed in each of the six vials and then a solutions of heavy metal ions (Zn(II) and Cd(II)) with increasing concentration (from 0.001 to 0.01 M) were added in the vials with the activated carbon present and then the vials were closed. After 24 hours at room temperature the samples where filtered to remove AC and the equilibrium concentration of the metal ions after the adsorption was determined by complexonometric titration with EDTA (ethylenediaminetetraacetic acid) as a titrant and metal indicator xylenol orange. In order to investigate the effect of pH and ionic strength of the media all other parameters (variables) in the experiments were kept constant. Results and discussions Norit CA1 is chemically activated carbon (with phosphoric acid) with highly developed surface. Depending on the method of activation there can be a different type of functional groups on the activated carbon surface. This is of significant importance when one uses the activated carbon (AC) for heavy Fig. 3. Linear plot of Freundlich isotherms for adsorption of Zn(II) ions onto Norit CA1 at different pH values 136 Conclusions Here on Figure 3 is shown the corresponding dependence of the adsorption of Zn(II) ions onto Norit CA1 at different pH. One can see from it that there is no apparent effect of pH onto adsorption properties of Zn(II) onto the AC. They are practically indiscernible. Activated carbon is one the most widely applied sorbent for water and wastewater treatment. That is due to its high sorption capacity, chemical resistance and versatility. It can be successfully applied for removal of both organic and inorganic substances (pollutants). By comparing the results obtained from the linear plots of Freundlich isotherms for adsorption of Cd(II) and Zn(II) ions (Figure 2 and Figure 3) onto Norit CA1 one can summarize that there is not any well pronounced dependence of the adsorption from pH media, both for Cd and Zn ions. This can be attributed to the chemical modification of activated carbon with phosphoric acid. That allowed the formation of a surfaced with relatively strong acidic groups that doesn’t affect from pH of the media in a tangible way. That makes Norit CA1 a very attractive choice when one needs to remove heavy metal ions, because it gives the opportunity to adsorb the same amount of metal ions regardless of pH of the media. The experiments conducted in this research revealed that activated carbon Norit CA1 is very suitable for heavy metal ions removal from waters and wastewaters. The results has shown that there is not any significant decrease of adsorption capacity at different pH media. That makes Norit CA1 useful for wastewater treatment since the low pH will affect much the adsorption of heavy metal ions onto surface of the activated carbon. The other fact that recommends it is versatility – it was shown that adsorption capacity of Zn(II) ions was as high as the Cd(II) ions. This leads us to believe that it can remove a large number of different metal ions from polluted waters with the same efficiency. There is no significant difference in the adsorption capacity and rate regarding Zn(II) and Cd(II) ions. This means that Norit CA1 is not selective adsorbent, at least not in respect these two metal ions. But this fact also makes it a versatile adsorbent for different types of substances. Overall activated carbon (in this particular case Norit CA1) has shown excellent adsorption properties to the tested heavy metal ions, one of his major advantages being the nonpronounced pH dependence as well as its versatility. The fact that adsorption in this case is mainly due to the electrostatic interaction between metal ions and AC surface makes it preferable to establish the effect and the ionic strength dependence since it is expected to be one of the parameters which will influence the adsorption capacity. Acknowledgements The authors thank to project MTF-120/ 07.07.2013 of UMG “St. Ivan Rilski” for the financial support and to IPC-BAS for SEM images of Norit CA1. On Figure 4 data are presented for adsorption of Cd(II) and Zn(II) ions onto Norit CA1 ot pH=4.8 and ionic strength – 0.1M and 0.01 M. Here can see the way that adsorption is affected by ionic strength of the media. In the case of Cd(II) ions when we increase the ionic strength from 0.01M to 0.1M the adsorption capacity and rate does not change significant which is also the case of Zn (II) ions adsorption. Overall we can observe from Figure 4 that ases as expected while the adsorption rate (slope) does not change significantly. In the case of we observe that Zn(II) ions have higher adsorption capacity onto Norit CA1 than Cd(II) at the same other conditions. References Bhattacharyya, K.G., Gupta, S.S., 2008. Adsorption of a few heavy metals on natural and modified kaolinite and montmorillonite: a review. – In: Adv. Colloid Interface Sci. 140, 114-131. Borba, C.E., Guirardello, R., Silva, E.A., Veit, M.T., Tavares, C.R.G., 2006. Removal of nickel(II) ions from aqueous solution by biosorption in a fixed bed column: experimental and theoretical breakthrough curves. – In: Biochem. Eng. J. 30, 184-191. Corapcioglu, M.O., Huang, C.P., 1987. The adsorption of heavy metals onto hydrous activated carbon. – In: Water Res. 21(9), 1031-1044. El-Kamash, A.M., Zaki, A.A., Abel El Geleel, M., 2005. Modeling batch kinetics and thermodynamics of zinc and cadmium ions removal from waste solutions using synthetic zeolite A. – In: J Hazard Mater B127, 211-220. Huisman, J.L., Schouten, G., Schultz, C., 2006. Biologically produced sulphide for purification of process streams, effluent treatment and recovery of metals in the metal and mining industry. – In: Hydrometallurgy 83, 106-113. Jamil, T.S., Ibrahim, H.S., Abd El-Maksoud, I.H., El-Wakeel, S.T., 2010. Application of zeolite prepared from Egyption kaolin for removal of heavy metals: I. Optimum conditions. – In: Desalination 258, 34-40. Kang, K.C., Kim, S.S., Choi, J.W., Kwon, S.H., 2008. Sorption of Cu2+ and Cd2+ onto acid- and base-pretreated granular activated carbon and activated carbon fiber samples. – In: J. Ind. Eng. Chem. 14, 131-135. Fig. 4. Linear plot of Freundlich isotherms for adsorption of Zn(II) and Cd(II) ions onto Norit CA1 at pH=4.8 and two different ionic strengths – 0.1M and 0.01M 137 Kiani, G.R., Sheikhloie, H., Arsalani, N., 2011. Heavy metal ion removal from aqueous solutions by functionalized polyacrylonitrile. – In: Desalination 269, 266-270. Kocaoba, S., Orhan Y., Akyuz, T., 2007. Kinetics and equilibrium studies of heavy metal ions removal by use of natural zeolite. – In: Desalination 214, 1-10. Landaburu-Aguirre, J., Garcia, V., Pongracz, E., Keiski, R.L., 2009. The removal of zinc from synthetic wastewaters by micellar-enhanced ultrafiltration: statistical design of experiments. – In: Desalination 240, 262-269. Lazar, M., Varghese, S., Nair, S.S., 2012. Photocatalytic water treatment by titanium dioxide: Recent updates. – In: Catalysts 2, 572-601. Liang, S., Guo, X., Feng, N., Tian Q., 2010. Effective removal of heavy metals from aqueous solutions by orange peel xanthate. – In: Trans. Nonferrous Met. Soc. China 20, 187191 Liu, C., Bai, R., Hong, L., Liu, T., 2010. Functionalization of adsorbent with different aliphatic polyamines for heavy metal ion removal: Characteristics and performance. – In: Journal of Colloid and Interface Sci. 345, 454-460. Liu, Q., Li, Y., Zhang, J., Chi, Y., Ruan, X., Liu, J., Qian, G., 2011. Effective removal of zinc from aqueous solution by hydrocalumite. – In: Chem. Eng. Jornal 175, 33-38 Ma, X., Li, L., Yang, L., Su, C., Wang, K., Jiang, K., 2012. Preparation of hybrid CaCO3-pepsin hemisphere with ordered hierarchical structure and the application for removal of heavy metal ions. – In: Journal of Crystal Growth 338, 272-279. Mohammadi, T., Moheb, A., Sadrzadeh, M., Ramzi, A., 2005. Modeling of metal ion removal from wastewater by electrodialysis. – In: Sep. Purif. Technol. 41(I), 73-82. Mohan, D., Pittman Jr., C.U., 2006. Activated carbons and low cost adsorbents for remediation of tri- and hexavalent chromium from water. – In: Journal of Hazardous Materials B137, 762-811. Mohsen-Nia, M., Montazeri, P., Modarress, H., 2007. Removal of Cu2+ and Ni2+ from wastewater with a chelating agent and reverse osmosis processes. – In: Desalination 217, 276-281. Muthukrishnan, M., Guha, B.K., 2008. Effect of pH on rejection of hexavalent chromium by nanofiltration – In: Desalination 219, 171-178. Asenov, A. 1991. Fundamentals of Geology. Nauka i Izkustvo, Sofia, 234 p. (in Bulgarian) International Tables for X-ray Crystallography. Vol. 1. Symmetry Groups. 1969. International Union of Crystallography, Kynoch Press, Birmingham, 588 p. Nakata, K., Fujishima, A., 2012. TiO2 photocatalysis: Design and applications. – In: Journal of Photochemistry and Photobiology C: Photochemistry Reviews 13, 169-189. Oyaro, N., Juddy, O., Murago, E.N.M., Gitonga, E., 2007 The contents of Pb, Cu, Zn andCd in meat in Nairobi, Kenya. – In: Int. J. Food Agric. Environ., 5, 119-121. Paulino, A.T., Minasse, F.A.S., Guilherme, M.R., Reis, A.V., Muniz, E.C., Nozaki, J. 2006. Novel adsorbent based on silkworm chrysalides for removal of heavy metals from wastewaters. – In: J. Colloid Interface Sci. 301, 479-487. Petruzzelli, D., Passino, R., Tiravanti, G., 1995. Ion exchange process for chromium removal and recovery from tannery waters. – In: Ind. Eng. Chem. Res. 34, 2612-2617. Roundhill, D.M., Koch, H.F., 2002. Methods and techniques for selective extraction and recovery of oxoanions. – In: Chem. Soc. Rev. 31, 60-67. Shaalan, H., Sorour, M., Tewfik, S., 2001. Simulation and optimization of a membrane system for chromium recovery from tanning waters. – In: Desalination 14, 315-324. Vasilev, O. 1999. Geochemical content of coals. – In: European Coal Geology and Technology. Geol. Soc. Spec. Publ., 125, 141–149. 138