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ADSORPTION OF INDIGO BLUE DYE AND SOME TOXIC METALS BY ACTIVATED CARBONS FROM COCONUT SHELLS
C.E. GIMBA*1 MUYIWA TUROTI2 , P.A EGWAIKHIDE3 AND E.E AKPORHONOR4 Department of Chemistry, Ahmadu Bello University, Zaria, Nigeria. Department of Chemistry, Federal College of Education, Zaria, Nigeria. 3 Department of Chemistry and Centre for Biomaterials Research, University of Benin, Nigeria 4 Department of Chemistry, Delta State University, Abraka, Nigeria gimbace @ yahoo.com
ABSTRACT At the activation temperature of 8000C, activated carbons of different particle sizes were produced from carbonized carbon that was previously obtained from coconut shells at carbonization temperature of 5000C. The activating salts were anhydrous FeCl3, ZnCl2, CaCl2 and K2CO3 at varying concentrations. Samples of a textile effluent containing indigo blue dye were used and the levels of dye adsorption were determined by colorimetry. Amongst the activated carbons the results showed that the particle size of 250µm of ZnCl2 – activated carbon was most effective adsorbing the dye up to 98%. The adsorption of lead (II), cadmium (II) and mercury (II) by the activated carbons was determined using atomic absorption spectrometry (AAS). The results show that the FeCl3 – activated carbon was most effective in adsorbing 70% Pb while the K2CO3 – activated carbon was most effective in adsorbing 81 and 83% of Cd and Hg respectively. KEYWORDS Adsorption, Activated Carbon, Indigo blue dye, colorimetry, atomic absorption spectrometry (AAS).
It is therefore very important to reduce or remove the level of dyes in such effluents before discharge.C. bacteria present in water convert organometallise mercury into dimethyl mercury compounds which bind tenaciously to the proteins in fish tissue . would be in the selective recovery of the adsorbed metals for industrial and laboratory uses. lack of coordination. would not only reduce the level of hazards but the recovery of the dye after adsorption will enhance recycling of the dye in such textile industries. cadmium for production of pigments e. loss of sensation in fingers and toes. The present work reports on the quantitative determination of the concentration of indigo dye adsorbed onto four different activated carbons each of eight different particle sizes unlike the two sizes used in the earlier study . These could include lead productions for vehicle batteries and solder. referred to herein as IB. Gimba. 425 500. Porcelain crucible. The effluents containing the excess dye are finally discharged into soils and rivers constituting pollution particularly to the aquatic lives.5. Lead accumulation yields chronic intoxication manifesting in encephalopathies in the central nervous system (CNS). different particle sizes.et al. and dissolved food substances containing these toxic metals. were of analytical grade.g. reproductive problems. Pb (NO3) 2. Cadmium (Cd) and mercury (Hg) are soil and water pollutants arising from waste waters. Cd(NO3) 2 and Hg (NO3)2. 850. such as indigo blue. was obtained as an industrial chemical from a chemical company in Kaduna. FeCl3. The highly toxic organomercury compounds eventually reach the higher animals and human beings through the food chain. coma and possibly death [8. Nigeria. Indigo blue dye. Lead (II). Anhydrous ZnCl2. 1400 and 2000µm of the activated carbon were obtained. CaCl2.10]. MATERIALS AND METHODS Materials Coconut shells were obtained locally.  gave an estimate of colours of effluents and showed that this dye can be adsorbed unto activated carbons from coconut shell. E. Therefore the major objective of this work is to find out the adsorption capacity of the activated carbons for Pb. BamfordSheffield. hearing loss. England. road traffic with leaded petrol. disturbance in kidney and liver functions progressing as far as necrosis. Lead and cadmium are typical cumulative  poisons. Access of cadmium into animals and human beings through feeding on plants containing absorbed Cd causes stomach irritation resulting in vomiting and diarrhea . The adsorption of dyes. 250. cadmium yellow 37 and metal coatings as well as mercury used in electrical engines and production of pigments. prepared and carbonized at 5000C as previously described by Gimba . According to a recent report. A certain level of Hg can damage the CNS causing memory loss. EJEAFChe.6]. 8 (11). Cd and Hg from contaminated waters. slurred speech. from textile effluents. 150. K2CO3. 1195 . With appropriate sieves. It is envisaged that the procedure used to adsorb indigo dye in this study can be effective in reducing the amount of the dye from the effluent of any textile industry using indigo blue. et al.9. industrial processes and their emissions. Gimba. in future. sintered glass crucible and other glass wares were thoroughly washed with distilled water and dried in the oven at about 1050C. 355. 2009. damage of the reproductive systems as well as anaemias and many metabolic deficiency symptom [4. [1194-1201] INTRODUCTION The use of dyes in the textile industries is mandatory. Muffle furnace model GLM 3 + PD/ND manufactured by Carbolite. An important extension of this study. CORNING–252 digital colorimeter.
Gimba.50.0M solution of ZnCl2 was prepared and appropriate aliquots were diluted with distilled water to give a range of 0. Metal and Moisture content in activated carbons These parameters were determined for the activated carbons using the same procedure described for the carbonized product elsewhere .025M solution were measured into a glass crucible using a pipette. 1. rinsed several times with distilled water and dried in an air – circulated oven. 2.0g of the carbonized product and the different particle sizes of the activated carbons were dispensed into 250cm3 conical flask followed by 50cm3 of standard indigo blue solution in chloroform (5%v/v). 1.0g of the carbonized carbon of a particular particle size (150. 2.2000µm) were weighed into the crucible and mixed thoroughly with the ZnCl2 solution to form a paste and then allowed to dry up at room temperature to constant weight. Activation Temperature. 0.0cm3 of 0. FeCl3. [1194-1201] Activation of Carbonised Carbon About 2.0cm3 of the 0. 2009. Thereafter. Determination of the Amount of Adsorbed Indigo Blue Dye The method described by Mkayula and Matumbo  was used. Thereafter the mixture in each flask was filtered by sunction through sintered glass crucible and the different filtrates were collected and analysed. This was followed by filtration through a glass crucible of porosity 4.5 and 2. The activated product was allowed to cool and then washed with 0. 0.5M solution of ethanoic acid.0M solutions.C.075. per sec. et al. Determination of Ash. 0. using an electric shaker for 1 hour each at room temperature. 8 (11). RESULTS AND DISCUSSION Preliminary investigation (Table 1) showed that the most effective activation temperature is 8000C. 1. Table 1.Effect of Activation Temperature on Adsorption (%) of indigo blue dye onto Activated Carbons. 1. 0C % Indigo blue adsorbed 500 60 600 65 700 75 800 78 900 62 1196 .025 – 2.2. The filtrate was then analysed for Pb using AAS so as to obtain the quantity of metal adsorbed unto each activated carbon by difference.0g of the carbonized carbon. the dry samples was heated in the Muffle furnace for 5 min at 8000C. Determination of the Amount Lead (Pb). The concentrations of the indigo blue filtrates were determined photometrically at λmax of 602nm against pure chloroform using a digital CORNING – 252 colorimeter.0. The activated product was kept in a dessicator.05. E. This procedure was repeated with each of 2. The above procedure was repeated using the same volume and concentrations as well as 2. Cadmium (Cd) and Mercury (Hg) Adsorbed. The standard solution of lead (II) containing 2x103ppm was agitated with the activated carbon of 500 µm particle size for 1h using an electric shaker. The above procedure was repeated using standard solution of 2x103ppm each of Cd (II) and Hg (II) salts. Absorbances of standard solutions of indigo blue were used for the calibration curve.0M solutions of ZnCl2 separately with 2.0. EJEAFChe.0g of the carbonized product and activated with the other activating salts. CaCl2 and K2 CO3. This was stoppered and agitated at a fast speed of 5 rev.
The order of moisture content is FeCl3 .11 9. Gimba. With respect to metal content the percent metal content follows the order CaCl2 . E. Table 2: Ash.54 CaCl2 5.> ZnCl2 -> CaCl2 .42 5. Figures 1 – 4 show the percent adsorption of the indigo blue dye with varying concentrations of the salts used for the adsorptions. This tends to suggest that the total ash content and metal content depends on the specific chemical interaction of the activating salt and the carbonized carbon during the activation process.90 0. Interestingly. This should be expected since the activation temperature (8000C) was higher than the carbonization temperature (5000C) and could have led to further removal of chemisorbed water in the carbonized product during the activation process. Table 2 shows that both the ash and metal contents of the activated carbons are higher than those of the precursor (carbonized carbons).> FeCl3 . The order of these two parameters (ash content and metal content) did not follow a particular trend (that is either increasing or decreasing) based on the physical constants of the Mn+.> K2CO3 .C. et al.49 5.91 3. 2009.93 ZnCl2 8. 8 (11).70 10. This is not surprising as the intermolecular association between water and M n+ depends on the polarizing power of the latter. This explains why the tripositively charged and smallest Fe3* in FeCl3 has the highest moisture content and least for K2* in K2CO3 .05 5. Metal and Moisture Content (%) of Different Activated Carbons (AC) at 150µm particle size.25 0. The order of ash content is ZnCl2 . Activating salts Parameters Ash content of carbonized carbon Ash content of Activated carbon Metal content of carbonized carbon Metal content of Activated carbon Moisture content of carbonized carbon Moisture content of Activated carbon FeCl3 2.> FeCl3 .01 K2CO3 5.71 5.> ZnCl2 -> K2CO3 – activated carbon. 1197 . EJEAFChe.8 0.35 3.> K2CO3 – activated carbon.35 This suggests that the activating salts were bonded to the activated carbons.> CaCl2 – activated carbons at 150µm particle size.01 5. This power depends directly on magnitude of the ionic charge and indirectly on the size of M n+ . The moisture contents of the activated carbons are much lower than that of the carbonized product as can be seen in Table 2.27 10. ionic size increases as Fe3+< Zn2+< Ca2+< K+ while ionic charge follows as Fe3+> Zn2+= Ca2+> K+ in the activating salts.25 4. [1194-1201] This is the optimum activation temperature for adsorbing this dye for all the different activated carbons used in this study.
Gimba. EJEAFChe. [1194-1201] 1198 . et al. E.C. 2009. 8 (11).
In addition.4) there could be higher adsorption for the dye at higher concentrations of K2CO3 which might not be economically viable due to larger amount of the salts that will be needed. This may explain why the highest concentration of 2.0 mol dm-3 concentration of the activating agent.0 2. This view is in agreement with the findings of [17. It is most probable that the hot CO enhances removal of moisture from the K2CO3-activated carbon.activated K2 CO3 . 2009. This is coupled with the fact that less moisture associates with K + due to its relatively big size and small positive charge. is capable of penetrating in between the hexagon plates of the crystallites normally found in the carbonized product of most cellulosic materials . Gimba. The increasing consumption of K2CO3 demands higher concentration of the salt resulting into greater effectiveness as more CO would be produced.5 1. 8 (11). The coconut shell is a cellulosic material containing bonded – OH group and H atom which can easily be removed as water by ZnCl2 particularly at the high activation temperature (8000C).activated ZnCl2 .C.15].0 0. develop greater porosity and leave the remaining atoms of the carbon matrix in a configuration that has specific affinities for particular adsorbates. The effectiveness of the ZnCl2 – activated carbon for IB could be attributed to the well recognized fact that ZnCl2 is a good dehydrating agent [14.activated CaCl2 . E. The concentration dependent effectiveness of K2CO3-activated carbon (AC) could be explained from the redox reaction producing carbon (II) oxide (CO) as earlier recognized . K2 CO3(s) + 2C(s) 2 K(s) + 3CO (g) The hot CO generated during the activation process would aid the formation of porous structure by burning the by–product blockages in the precursor. From the results obtained using the ZnCl2 – and K2CO3 . These are summarized in Table 3. et al. unto the activated carbons at 250µm particle size. increases the surface areas. The K in this position could spread the crystallites apart thereby aiding surface erosion of the unexposed carbonized product (due to closed pores) at the end of carbonization. the high ash content and low moisture content should be considered for effective adsorption of dyes. Most Effective particle size (µm) 150 150 250 250 Table 3:Adsorption Characteristics of Indigo blue Most Effective concentration (mol dm-3 Activated Carbon type )of Activating salts) FeCl3 . The presence of ZnCl2 will therefore enhance activation process and increase the adsorption efficiency of the ZnCl2-activated product.0mol dm-3 of ZnCl2 is employed. the reduced product.0 Maximum Adsorption of IB (%) 92 93 98 97 It is now probably clear that ZnCl2 – activated carbon at 250µm particle size is most effective in adsorbing 98% of IB when 1.1] that oxidation (as in the above reaction) selectively erodes the surface of carbonized carbon. EJEAFChe. there are optimum adsorption occurring at a particular particle size of each of the different activated carbons using particular concentrations of the activating salts. according to these authors.. 1199 .activated carbons. From the trend of the curves (Fig.0 mol dm-3 of k2CO3 used in this work resulted into high adsorption efficiency for IB. such as indigo blue. potassium metal. The K2CO3 – activated carbon at 250µm particle closely followed with 97% IB adsorption but at 2. [1194-1201] As it can be seen. This..activated 1.
> CaCl2 > ZnCl2 .> FeCl3 – activated carbon. Gimba.0 mol dm-3 of the activating salt. adsorbed unto the activated carbon containing a transition metal ion. CaCl2 ZnCl2 and K2CO3 at activation temperature of 8000C have the following characteristics. Cadmium and Mercury Adsorbed unto Activated carbons at 500µm particle size.110 nm) is slightly better adsorbed (83%) than the slightly smaller Cd2+ (0.2 50. for example. For both Cd (II) and Hg (II) the order of adsorption by the adsorbents is the same but the reverse is the case for Pb (II). using these activated carbons could be utilized for their recovery and sold as laboratory 1200 .3 80 75 81 60. Particle sizes 150 and 250µ are required for IB adsorption of over 90% using any of the four activated carbons employed in this study. Metal Adsorbed Lead Cadmium Mercury Initial concentration (ppm) 2000 2000 2000 Concentration ( %) of each metal Adsorbed FeCl3 – activated CaCl2 – ZnCl2 – K2CO3 – activated carbon Activated activated carbon carbon carbon 70 57.C. The earlier work . The bigger Hg2+ (0. Some of these metals are very expensive and their adsorption from wastewaters. Fe3+. 2. This probably suggests that the nature of the adsorption is dependent on the similarity of electronic structure of the Cd(II) and Hg(II) which are successive group II B transition metals In the periodic table.8 45. lead (II) _ cadmium (II) and mercury (Hg) . The adsorption is different with Pb2+ a group IVA metal.activated carbon. showed that the highest adsorption of indigo blue by carbonized carbon at 500µm particle size and carbonization temperature of 5000C was only 37%.097 nm) of 81% adsorption unto the same K2CO3 . The 250µm particle size of the ZnCl2 activated carbon produced at 8000C had the highest IB adsorption of 98% using 1. The smaller particle sizes of the activated carbons generally have higher adsorption propensities for IB. E. which is better. Toxicity levels due to the presence of Pb(II). EJEAFChe. Table 4:Concentration (percentage) of Lead. This shows that effective adsorption of indigo blue is generally dependent on the surface area of the activated carbons. Cd(II) and Hg(II) in aqueous medium can be reduced using FeCl3-activated carbons for Pb(II). et al. 3. [1194-1201] Adsorption of Metals Our preliminary experiments involving the four activated carbons showed that 500µm particle size is most effective for adsorption of the three toxic metals. 1. Similar view had been recognised earlier .1 82 68. The order of increasing size and decreasing charge follows (Fe3t < Zn2+<Ca2+ < K+ ) and (Fe3t > Zn2+>Ca2+ >K+ ) respectively. 8 (11).1 83 CONCLUSION The results contained in this report showed that coconut shell previously carbonized at 5000C and subsequently activated using FeCl3.7 63. K2CO3 . Greater ash and metal content as well as smaller moisture content than the carbonized form. 2009. The relatively high affinity for IB adsorption was generally dependent on high ash content and low moisture content of the activated carbons. that is. and K2CO3 for Cd(II) and/or Hg(II) adsorption at 500µm particle size . Table 4 shows that the order of adsorption of lead from the solution by the carbons is FeCl3 -AC > ZnCl2 -AC > CaCl2 -AC > K2CO3 -AC.
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