Adsorptive treatment of brewery effluent using activated Chrysophyllum albidium seed shell carbon
© Menkiti et al.; licensee Springer. 2014
Received: 17 January 2014
Accepted: 25 March 2014
Published: 30 April 2014
Chrysophyllum albidium seed shell, an abundant, biodegradable and inexpensive natural resource was used as a precursor to bioadsorbent production for the removal of suspended and dissolved particles (SDP) from initially coagulated Brewery Effluent (BRE). Influence of key parameters such as contact time, bioadsorbent dose, pH and temperature were investigated using batch mode. The thermal behavior studies were evaluated using Thermogravimetric and Differential scanning calorimetric analyses. The morphological observations and functional groups of the bioadsorbents were determined using scanning electron microscopy and Fourier transform infrared spectroscopy, respectively. The adsorption equilibrium, thermodynamics and kinetic of SDP adsorption on H3PO4-treated shell and NH4Cl-treated shell were examined at specified temperatures. Equilibrium data sufficiently fitted the Langmuir isotherm model (R2 > 0.99; SSE < 0.09). The pseudo-second order kinetic model provided the best correlation (R2 > 0.99; SSE < 0.14) with the experimental data. The values of ΔG° and ΔH° indicated the spontaneous and endothermic nature of the process. This study demonstrated that C. albidium seed shell could be utilized as low cost, renewable, ecofriendly bioadsorbent for the uptake of SDP from BRE.
Brewing is an intensive water consuming activity, besides utilizing a wide variety of chemicals. Expectedly, large volumes of effluent is discharged into water courses of brewery bearing communities, leaving in its wake a polluted aquifer (Khuo-Omoregbe et al. 2005; Menkiti 2010). Increasing concentration of these organic/non-organic enriched BRE in the water constitute a severe health hazard to both plants and animals, thus impeding the functionality of the ecosystem. The situation is typical of the BRE receiving aquatic system in Nigeria, where much of the water resources cannot be utilized without a form of treatment, following effluent discharges with negligible consideration for environmental control (Menkiti and Onukwuli 2011a).
BRE, generated from lager beer production, contains large amount of SDP (Menkiti and Onukwuli 2010). Typically, the organic contents of BRE consists of sugars, soluble starch, ethanol, volatile fatty acids and solids which are mainly spent grains, yeast and trub (Driessen and Vereijken 2003). Untreated BRE quantitatively contains suspended solids (100–1500 mg/l), chemical oxygen demand (300–800 mg/l), nitrogen (30–100 mg/l) and phosphorus (10–30 mg/l) (Menkiti et al.2011a World Bank Group 1998).
Over the years, significant attention has been given to the environmental cleanup of such contaminated aqua system using varieties of techniques such as precipitation, ion-exchange, coagulation, reverse osmosis and adsorption (Hameed and El-Khaiary 2008; Larous et al.2005; Menkiti et al.2011b; Menkiti and Onukwuli 2011b). Among the different treatments listed above, adsorption technology is attractive due to its merits of efficiency,even at low concentration of contaminants (Meena et al. 2008; Yakubu et al. 2008), economy, simple operation and insensitivity to toxic substances (Grini 2005; Feng et al.2010; Menkiti and Onukwuli 2011b).
The common adsorbents primarily include zeolite, clays, polymeric materials and natural agricultural materials which provided the focus of this study (Asasian and Kaghazchi 2013; Jiang et al.2012; Amirnia et al.2012). These natural materials have potential to be used as low cost bioadsorbent, as they represent unused resources, abundantly available and known to be eco-friendly (Deans and Dioxn 1992). Progressively, much attention has been focused on techniques of converting these waste materials into useful adsorbents. Among these agricultural wastes are saw dust (Meena et al. 2008) palm ash (Ahmad et al.2007).
Chrysophylum albidium seed shell, considered in this study, is of tropical forest tree of genus chrysophyllum, family of sapotaca e and order of ericales. The fruit is large berry containing 4 to 5 flattened seeds with a hard shell (Bada 1997). Significant quantities of these seeds shells are produced annually in Nigeria without being put to useful ends industrially. However, successful application of adsorbent from C. albidium seed shells for the removal of heavy metals had been reported (Oboh et al.2009; Onwu and Ogah 2010; Ejikeme et al.2011). According to the author’s knowledge, no attempt has been made until now to use this seed shell for the treatment of natural organic aqueous waste, such as BRE. Therefore, it was of interest to experiment with such a promising biomaterial for the adsorptive removal of SDP from initially coagulated BRE by batch technique. The work further seeks to investigate the influence of contact time, adsorbent dosage, temperature and effluent pH on the adsorptive uptake of SDP from the BRE. Also, the research investigated the ability of three isotherm models: namely the Langmuir, the Freundlich and the Temkin adsorption isotherms to model the equilibrium adsorption data. Another major focus of the work was the kinetic study, conducted to determine the rate of SDP adsorption and evaluation of which of the four kinetic models (pseudo-first order, pseudo-second order, Elovich and Bhattacharya-Venkobachar) that best describes the adsorption process. Finally, material characterization and thermodynamic analyses were conducted to present the characteristic properties and energy changes associated with the adsorption study.
Materials and methods
Brewery effluent was obtained from a beer brewery at 9th Mile Corner Udi, Enugu Sate Nigeria and stored in black plastic container to preserve and further prevent changes in the characteristics of the effluent (Clesceri et al.1999).
C. Albidium seed shells
The precursor for the preparation of the bioadsorbents, C. albidium seed shells was obtained as a waste material from Nsugbe, Anambra State of Nigeria. Pretreatment of the shells by thorough washing with distilled water to remove the impurities was done and the washed sample dried in an air circulating oven at 40°C for 14 hours. The shell samples were blended, sieved and particles that ranged between 2 and 3 mm were obtained and stored in a desiccator for use in the experiments.
Two portions of the shell samples, of known weights, were immersed in 60% solutions of ammonium chloride and phosphoric acid, respectively, for 24 hours. The carbonization of the shell samples were carried out in a muffle furnace at 600°C for 4 hours, washed with distilled water to pH 7, dried at 110°C for 8 hours and subsequently sieved to desired diameter using standard sieves.
Standard APHA methods, as reported by Clesceri et al. (1999), were applied to determine the physiochemical and biological characteristics of the effluent.
Characteristics of ASAA and ASAS
BET Surface area (m2/g)
Total pore volume (cm3)
Bulk density (g/cm3)
% Ash content
Oil content (%)
Moisture content (%)
Tapped bulk density
where: w is weight of the dry material and v is volume of the dry material.
Percentage ash content
where: Wash is weight of ash and Wsample is weight of bioadsorbent sample.
Percentage moisture content
where: Wsample is the weight of bioadsorbent sample before drying, Wdry is weight of sample after drying.
where: Vpore is pore volume of the bioadsorbent and W inc is weight increase of the bioadsorbent and ρ water is the density of water.
Surface area was determined according to the modified methods of Kang et al. 2013. It was calculated from nitrogen gas adsorption isotherms based on Brunauer, Emmet and Teller (BET) method of surface area analysis (at 77.305 K) using Quantachrome 2.0 analyzer.
Physiochemical and instrumental characterization of bioadsorbent samples
Fourier transfer infrared analysis was carried out using Shimadzu FTIR 8400S spectrophotometer for the determination of functional groups present in ASAA and ASAS. The thermal behavior of the activated carbon was evaluated by thermogravimetric and differential scanning calorimetric analyses using TGA-Q 50 and DSC-Q 200 models, respectively. The surface morphology of the activated carbon was visualized via scanning electron microscopy (SEM) using a scanning electroscope model FEI-QUANTA 200. Physiochemical and instrumental characterization of the bioadsorbents were conducted using standard methods (Feng et al. 2010).
Batch adsorption experiments were performed in Erlenmeyer flask according to the methods reported by Sivakumar and Palanisamy (2009) and Yeddou and Bensmaili (2005). In a typical experiment, 20 ml of effluent sample was mixed with the appropriate amount of adsorbents (types ASAA and ASAS) in the range of 10-50 g/l and then shaken for a period of time ranging from 5 to 60 min at 20 rev/s. The temperatures of adsorption measurements ranged between 20 and 30°C and the appropriate value was applied accordingly as required. The sample was then filtered using Whatman no 42 filter paper having fine porosity and particle retention of 2.5 micrometer at slow flow rate in a glass funnel. The filtered liquid was analyzed with respect to particle (SDP) content.
where: C 0 , C t and D A are initial constant effluent concentration (mg/l), effluent concentration at any time, t and adsorbent dose (g/l), respectively.
Results and discussion
Characterization of results
Physiochemical and biological characteristics
Characterization result of Brewery Effluent and FEPA standard
Total hardness (mg/l)
The FTIR spectra of ASAA and ASAS are depicted in Figure 1b and c, respectively. For both figures, discernable peaks of note were recorded at 3991.82-3162.40 cm−1(O-H stretch/phenols), 3456.55 cm−1(O-H broad stretch/N-H medium stretch), 3060.17-2830.63 cm−1(O-H broad stretch), 1596.15-1595.16 cm−1(NO2 asymmetrical stretch), 1412.90 cm−1(C-H scissoring/bending), 1225.80 cm−1(C – N stretch/C-O stretch), 1220.98 cm−1(C-H/C-O stretches), 1100.43 cm−1(C-N/C-O stretches) and 814.95-819.77 cm−1 (C-H stretch bend).
The FTIR spectra of used adsorbents showed (Figures are not shown) discernable peaks (in cm−1) for used ASAA at 461(S-stretching), 803(C-H stretch/NH2 wagging and twisting), 1084.03 (second overtone N-H and O-H stretching), 1419.66 (first overtone N-H and O-H stretching), 1608.69(pyridine C-N),3443.05 (primary NH2 asymmetric stretching), and for used ASAA at 389 (aliphatic P compound), 469 (S-stretching), 880.53/1101.39(aromatic P-O stretching), 1450.52/1573.97(C = C stretching), 3458.48(primary NH2),3633.05(O-H stretching).
The FTIR results of bioadsorbent precursor (Figure 1a), ASAA (Figure 1b), ASAS (Figure 1c) and used adsorbents indicated that some peaks were shifted or disappeared, and that new peaks were also detected. These changes observed in the spectra represent interactive effects due to involvement of those functional groups during production and use of the adsorbents. The changes observed in the peaks of the adsorbents after usage could be concluded to be the direct result of adsorptive uptake of SDP from the BRE by the adsorbents. The varying number of absorption peaks displayed by the samples reflected the complex nature of these materials (Hameed and El-Khaiary 2008; Chemistry Department at Colorado University CDCU 2002; Graham et al.2008).
DSC and TGA
As indicated in Figures 2a and 3a, DSC was used to characterize the phase transition that occurred in ASAA and ASAS over the temperature range of 25-277°C. Figure 2a revealed a sharp thermal transition in the temperature range of 125-150°C with transition enthalpy of 250 kJ/kg. Figure 3a indicated sharp transition in the temperature range of 112.5-138°C with transition enthalpy of 819.9 kJ/kg. This behavior by both ASAA and ASAS could be attributed to the de-stringing and coiling of carbon chain leading to spontaneous densification (Ramani et al.2012). The densification of the aggregated mass occurred at 175-180°C and 150-175°C for ASAA (Figure 2a) and ASAS (Figure 3a), respectively without absorption of thermal energy. In other words, the heat flow discs indicated exothermicity.
The thermal decomposition behaviors of the bioadsorbents are illustrated in Figures 2b and 3b for ASAA and ASAS, respectively. Figure 2b shows that ASAA lost weight by 11.17% and 15.18% at 120.63°C and 562.65°C, respectively. For Figure 3b, the weight loss of 10.75, 15.63 and 19.65% were recorded for 135.04, 517.16 and 649.84°C, respectively. For both Figures 2b and 3b, the initial weight loss could be attributed to the internal moisture and gaseous loss from the matrix molecules of the adsorbents (Ramani et al.2012). The second phase weight loss may be attributed to the decomposition of the labile component in the adsorbent. The results presented in Figures 2 and 3 conclusively suggested operational stability of the adsorbents.
Influence of contact time and adsorbent dosage on adsorptive removal of SDP from BRE
The observed adsorption dynamic profiles depicted by Figures 5 and 6 can be divided into three regimes (Ncibi et al.2008): (i) a linear increase in adsorption with time, (ii) a transition regime where the rate of adsorption levels off, and (iii) a plateau regime. First regime (initial steep slope) indicated instantaneous adsorption (overshoot phenomena) ability of effluent particles onto the surface of the adsorbents. The second regime indicated a phase of gradual attainment of equilibrium where the apparent fall in SDP adsorption rate might be due to utilization of active sites on adsorbents surface. Plateau regime indicated phase where equilibrium had been achieved (Mohan et al.2007).
One general phenomenon was the perceived increase in SDP uptake with increase in adsorbent dose. It should also be observed that the % Rem for doses considered in Figures 5 and 6 ranged closely; with only apparent difference noticed for 50 g/l (Figure 5). This could be attributed to the greater availability of close number of exchangeable sites or surfaces in the adsorbents (Meena et al.2008). Following optimal results obtained at 50 g/l and 30 min, the rest of the work was carried out at the stated results, unless otherwise indicated.
Figures 7 and 8, present results similar to Figures 5 and 6 in respect of the variation of adsorption capacity q t (mg/g) with contact time and adsorbent dose. It was evident that q t increases with decreasing adsorbent dose and increasing contact time before leveling-off. The highest and lowest q t were recorded at 10 and 50 g/l, respectively for both ASAA (Figure 7) and ASAS (Figure 8). In specific terms, q t at 10 g/l increased from 9.812 to11.308 mg/g for 5 and (30–60) min, respectively as shown in Figure 7. Also, the q t at 50 g/l ASAA increased from 2.0504 to 2.4002 mg/g for 5 and (30–60) min, respectively. Figure 8 indicated that qt at 10 mg/l recorded increment from 8.4920 to 10.703 mg/g for 5 and (30–60) min, respectively while that of 50 g/l increased from 1.7842 to 2.1868 mg/g for 5 and (30–60) min, respectively. The results indicated also that the ASAA performed better than ASAS.
The apparent decrease in adsorption density (amount adsorbed per unit mass of the adsorbent) with increase in adsorbent dose was due to progressive unsaturation of adsorption sites through the adsorption reaction. Another reason might be due to the particle interaction, such as aggregation, usually resulting from high adsorbent concentration. Such aggregation would lead to decrease in total surface area of the adsorbent and on increase in the diffusional path length (Shukla et al.2002). Particle interaction might also desorb some of the adsorbate that was only loosely and reversibly bound to the adsorbent surface.
Influence of temperature on the adsorptive removal of SDP from BRE
Both Figures 9 and 10 indicated that the retention of SDP by the adsorbents increased while the temperature and time increased. The perceived increase of SDP uptake with temperature might be due to the acceleration of some originally slow adsorption steps or the creation of some active sites on the adsorbent surface (Hashem 2007; Nasssar and Magdy 1999). The enhanced mobility of SDP from the bulk solutions towards the adsorbent surface should also be taken into account (Hashem 2007; Yubin et al.1998). Increased temperature encouraged the process of agglomeration and widening adsorbent pore resulting in certain activation of the surface of the solid support (Larous et al.2005). Obtained results indicated clearly that the adsorption process under study was an endothermic process. This fact was illustrated in Section 3.6. Results similar to the one of this study had been reported by Khalid and Ahmad (1998).
Influence of pH on the adsorptive removal of SDP from BRE
In quantitative terms, the percentage SDP removal increased with pH from 2 to about 6.95 and remained unchanged thereafter. In respect of ASAA and ASAS, the SDP removal increased from 69.5768% at pH 2 to 73.0839% at pH 6.95 and 66.3161% at pH 2 to 70.4231% at pH 6.95, respectively. At pH greater than 6.95, the SDP removal remained constant till pH 8. The gentle decrease at about pH 3–6 of the initial rapid adsorption of SDP was presumed to be due to competitive adsorption between hydrogen ion and particles of the BRE. The adsorption at near neutral pH values could be attributed to the cellulose component of adsorbents where site binding adsorption might be occurring. This could be due to surface complex phenomena of functional groups present in the adsorbent (Hashem 2007; Menkiti et al. 2011a).
Graphical results of Figure 11 could be linked strongly to the influence of pH, in addition to the functional groups on the adsorbent and their ionic state at a particular pH (Mohan et al.2007; Genc et al. 2003). Equally, the apparent increment in adsorption with pH was believed to result from corresponding increase in the number of negatively charged sites. Consequently, the electrostatic attraction between the negative surface and the cationic BRE molecules increased with pH and reached saturation at about pH 6.95. Sivakumar and Palanisamy (2009) and Noroozi et al. (2007)) had reported similar results for the adsorption of basic red 29 onto Euphorbia antiquorum L and BR 41 onto silkworm pupa, respectively.
Equilibrium isothermic analysis
The study of the adsorption isotherm is fundamental (Gräf et al. 2012), and played an important role in determination of the maximal capacity of adsorption, in addition to development of an equation which accurately represented the results that could be used for design purposes. Three equilibrium isotherms were analyzed: Langmuir, Freundlich and Temkin.
The Langmuir isotherm is arguably the best known of all isotherms describing adsorption. It applies to the cases of adsorption on completely homogenous surfaces where interactions between adsorbed molecules are negligible. The Freundlich isotherm is the earliest known relationship describing the adsorption isotherm. This empirical isotherm applies fairly well when describing the adsorption in dilute aqueous solution systems. Temkin isotherm applies on the bases that a fall in heat of sorption is linear rather than logarithmic as obtained in Freundlich equation. Heat of sorption of all molecules in the layer would decrease linearly with coverage due to sorbate- sorbent interactions (Larous et al.2005; Sujatha et al.2008).
Isotherm mathematical model equations used for adsorption data analysis
Isotherm parameters obtained from SDP adsorption on ASAA and ASAS at pH of 6.95, DA=50g/l, C 0 = 161.92 mg/l
R L indicates the shape of the isotherm. This is: (i) unfavorable when R L > 1, (ii) linear when R L = 1 (iii) favorable when 0 < R L < 1, and (iv) irreversible when R L = 0. The calculated R L values for the two adsorbents, shown in Table 4 were all in the range of 0–1, which confirmed that adsorption process was favorable within the studied experimental conditions.
In respect of Freundlich isotherm, favorability of the process is achieved if n lies in range of 1–10. Based on the values of Freundlich constant (n) displayed in Table 4, the present adsorption system could be considered favorable since n values lie between 1and 10 for all cases studied.
Thermodynamic analyses of adsorption isotherm data
Thermodynamic parameters for SDP on ASAA and ASAS
Table 5 shows that ΔG˚ values were increasingly negative with temperature, which indicated the increasing feasibility and spontaneity of the adsorption process. The adsorption of SDP onto ASAA was greater than that of SDP onto ASAS overall. Also, from Table 5, the values of ΔS˚ are increasingly positive with temperature, an indication of increasing randomness of solid–liquid interface with increasing temperature (Debnath and Ghosh 2008). From the table, the values of ΔH° recorded for ASAA and ASAS are 3.493 kJ/mole and 2.477 kJ/mole, respectively. The values are found to be less than 40 kJ/mole which indicated that physisorption dominated the adsorption of SDP onto ASAA and ASAS. The present results are found to follow similar trend with the results reported by Patel and Suresh (2008) on the biosorption of reactive black 5 dyes by Aspergillus foetidus.
Surface packing, surface charge and hopping number
where: C o and C e are initial and equilibrium concentrations in mg/cm3, Γ is the adsorption density in mg/m2, Z = 4 is the valency of organic carbon, which is a major constitutent (Driessen and Vereijken 2003; Kanagachandran and Jayaratne 2006; Janhom et al. 2009; Menkiti 2010) of SDP in the BRE, r = 0.70 ×10- 9 m is the effective radius of the organic carbon enriched-SDP reported elsewhere (Crystalmarker 2014; United States Environmental Protection Agency USEPA 1999), R is gas constant, and T is the absolute temperature (K).
Adsorption kinetic analysis
Kinetic and equilibrium data are pertinent in the evaluation of adsorption dynamics and by extension, the optimization of residence time for the uptake of SDP on ASAA and ASAS. Adsorption kinetics could be controlled by several independent processes (bulk diffusion, film diffusion, chemical reaction, intra-particle diffusion, temperature, pH, etc.) that could act in series or in parallel (Abia and Asuquo 2006). In order to investigate the kinetic of BRE adsorption on ASAA and ASAS, the data obtained at 30°C have been analyzed by pseudo first order(PFO) (Langergren 1898, Eq. Nineteen), pseudo second order(PSO) (Ho and Mckays 1999, Eq. Twenty); Elovich (Chien and Clayton 1980, Eq. Twenty-one) and Bhattacharya – Venkobachar (BVM) (Bhattacharya and Venkobachar 1984, Equation Twenty-two) kinetic model equations and subsequently subjected to accuracy tests via R2 and SSE (Eq. 6).
The kinetic equations used for analysis of kinetic data
ln(q e − q t ) = ln q e − K1t
ln(q e − q t ) vs. Time
q t vs. Time
ln[1 − (U)T] = K B t
ln[1 − (U)T] vs. Time
Kinetic parameters of the adsorption process at 30°C ,pH 6.95, D A = 50 g/l , C 0 = 161.92 mg/l
African star apple shell biomass (ASAA and ASAS) was able to adsorb SDP from brewery effluent (BRE). The removal of SDP from BRE using ASAA and ASAS was a function of contact time, bioadsorbent dosage, temperature and pH. Adsorption capacity increased with increasing temperature. The optimum SDP removals were achieved at pH 6.95, 50 g/l dose and 30°C. Among the isotherm models considered, equilibrium data fitted the Langmuir model best within the studied experimental conditions. The kinetic data agreed very well with the pseudo-second order equation. The calculated thermodynamics parameters showed that the related adsorption systems were favorable, endothermic and spontaneous for both ASAA and ASAS.
The authors acknowledge the underlisted organizations for their assistance towards the completion of this work:
1. Chemical Engineering Department, Nnamdi Azikiwe University, Awka, Nigeria.
2. Scientific Equipment Development Institute, Enugu, Nigeria.
3. National Research Institute for Chemical Technology, Zaria, Nigeria.
4. Central Leather Research Institute, Chennai, India.
5. Indian Institute of Chemical Technology, India.
6. India National Science Academy/Center for International Cooperation in Science, India.
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