Factorial experimental design for recovering heavy metals from sludge with ion-exchange resin

Wastewaters containing heavy metals are usually treated by chemical precipitation method in Taiwan. This method can remove heavy metals form wastewaters efficiently, but the resultant heavy metal sludge is classified as hazardous solid waste and becomes another environmental problem. If we can remove heavy metals from sludge, it becomes non-hazardous waste and the treatment cost can be greatly reduced. This study aims at using ion-exchange resin to remove heavy metals such as copper, zinc, cadmium, and chromium from sludge generated by a PCB manufacturing plant. Factorial experimental design methodology was used to study the heavy metal removal efficiency. The total metal concentrations in the sludge, resin, and solution phases were measured respectively after 30 min reaction with varying leaching agents (citric acid and nitric acid); ion-exchange resins (Amberlite IRC-718 and IR-120), and temperatures (50 and 70 degrees C). The experimental results and statistical analysis show that a stronger leaching acid and a higher temperature both favor lower heavy metal residues in the sludge. Two-factors and even three-factor interaction effects on the heavy metal sorption in the resin phase are not negligible. The ion-exchange resin plays an important role in the sludge extraction or metal recovery. Empirical regression models were also obtained and used to predict the heavy metal profiles with satisfactory results.     

Study of Cu(II) biosorption by dried activated sludge: effect of physico-chemical environment and kinetics study

Biosorption is a recent technology used to remove heavy metal ions from aqueous solutions. The biosorption of copper ions from aqueous solution by dried activated sludge was investigated in batch systems. Effect of solution pH, initial metal concentration and particle size range were determined. The suitable pH and temperature for studied conditions were determined as 4.0 and 20 °C, respectively. The theoretical max biosorption capacity of activated sludge was 294 mg g⁻¹ at 20 °C for <0.063 mm particle size. The equilibrium data fitted very well to both Langmuir and Freundlich isotherm models. The pseudo first and second-order kinetic models were used to describe the kinetic data. The experimental data fitted to second-order kinetic model. The particle size and initial metal concentration were effected the biosorption capacity of dried activated sludge. An increase in the initial metal concentration increases of biosorption capacity, which also increases with decreasing particle size. Dried activated sludge has different functional groups according to the FT-IR results.     

Microwave enhanced stabilization of heavy metal sludge

A microwave process can be utilized to stabilize the copper ions in heavy metal sludge. The effects of microwave processing on stabilization of heavy metal sludge were studied as a function of additive, power, process time, reaction atmosphere, cooling gas, organic substance, and temperature. Copper leach resistance increased with addition of aluminum metal powder, with increased microwave power, increased processing time, and using a gaseous environment of nitrogen for processing and air for cooling [N2/air]. The organic in the sludge affected stabilization, whether or not the organic smoldered. During heating in conventional ovens, exothermic oxidation of the organic resulted in sludge temperatures of about 500 degrees C for oven control temperatures of 200-500 degrees C. After microwave heating dried the sludge, the sludge temperature rose to 500 degrees C. The reaction between copper ions and metal aluminum in the dried sludge should be regarded as a solid phase reaction. Adding aluminum metal powder and reaction temperature were the key parameters in stabilizing copper in the heavy metal sludge, whether heated by microwave radiation or conventional oven. The mass balance indicates insignificant volatization of the copper during heating.     

Adsorption of heavy metals from wastewater with waste activated sludge

Abstract

The purpose of this study is the investigation of the adsorption of heavy metals from wastewater with waste activated sludge (WAS) so as to increase the operational flexibility of activated sludge processes for the shock loading problems of heavy metals. By contacting the raw wastewater with WAS, before it entered the activated sludge process unit, some heavy metals in the wastewater were removed, and the pH value of the acidic wastewater rose. Five metals, Cu, Zn, Ni, Cd and Pb, were studied, some factors which affected this biosorption phenomena were investigated, and expressions of the adsorption isotherms were discussed. A semi‐empirical mass transfer‐adsorption model was developed to describe the kinetic experimental data.     

Removal of copper from industrial sludge by traditional and microwave acid extraction

This work elucidates the removal of copper from industrial sludge by traditional and microwave acid extraction. The effects of acid concentration, extraction time, sludge particle size and solid/liquid (S/L) ratio on copper removal efficiency were evaluated. Leaching with more concentrated acid yielded greater copper content from the industrial sludge. The experimental findings reveal that the most economical traditional extraction conditions were the use of 1N sulfuric or nitric acid for 60 min at an S/L ratio of 1/20; however, at an S/L ratio of 1/6, the extraction time needed to achieve the same copper removal efficiency was increased to 36 h. Increasing the microwave power and reducing the S/L ratio increased the copper extraction efficiency and the effect in the larger S/L ratio system was more significant. A comparison of the results of microwave-assisted (microwave only) and microwave-enhanced (microwave with addition of active carbon) acid extraction demonstrated that under both conditions, S/L ratio = 1/6 and 1/20; adding active carbon shortened the extraction time required to achieve 80% copper extraction efficiency from 20 to 10 min. These experimental results indicate that the most important factors that most strongly affected microwave acid extraction were the addition of a microwave absorber, the microwave power input and the S/L ratio. The sludge particle size did not significantly affect the copper extraction. The results reveal that sulfuric acid was an effective extractant and that the copper fraction in the extracted sludge shifted from being mostly bound to the Fe–Mn oxides and organic matter, to being mostly bound to organic matter and remaining as a residue during acid extraction.     

Solid-liquid-solid extraction of heavy metals (Cr, Cu, Cd, Ni and Pb) in aqueous systems of zeolite-sewage sludge

This paper presents results of kinetic and equilibrium studies of the removal of heavy metals (Cr, Cu, Cd, Ni and Pb) from the sewage sludge using a new technique of solid-liquid-solid extraction with the adsorption-diffusion column filled by the zeolite. The metal extraction onto the zeolite from aqueous solution of the clinoptilolite and the sludge composition is characterized by three stages: intensive extraction, inversion and stabilization with the moderate extraction increase. Addition of 25% of the zeolite provides extraction efficiency of cadmium and lead of about 84%, chromium, copper and nickel of 66%, 61% and 50%, respectively. The estimated values of Gibbs free energy change DeltaG show that the metals extraction by the clinoptilolite may be considered as a physical adsorption. The negative values of DeltaG testify to an exothermic nature of the process. The difference between energetic potentials of the components is a driving force of the metal redistribution in the system "clinoptilolite-water-sludge".     

Preparation of porous nano-calcium titanate microspheres and its adsorption behavior for heavy metal ion in water

Using D311 resin as a template, porous nano-calcium titanate microspheres (PCTOM) were prepared by a citric acid complex sol-gel method and characterized by X-ray diffraction (XRD), SEM and FTIR. The method's adsorption capabilities for heavy metal ions such as lead, cadmium and zinc were studied and adsorption and elution conditions were investigated. Moreover, taking the cadmium ion as an example, the thermodynamics and kinetics of the adsorption were studied. The results show that the microspheres were porous and were made of perovskite nano-calcium titanate. The lead, cadmium and zinc ions studied could be quantitatively retained at a pH value range of 5-8. The adsorption capacities of PCTOM for lead, cadmium and zinc were found to be 141.8 mg g(-1), 18.0 mg g(-1) and 24.4 mg g(-1) respectively. The adsorption behavior followed a Langmuir adsorption isotherm and a pseudo-second-order kinetic model, where adsorption was an endothermic and spontaneous physical process. The adsorbed metal ions could be completely eluted using 2 mol L(-1) HNO(3) with preconcentration factors over 100 for all studied heavy metal ions. The method has also been applied to the preconcentration and FAAS determination of trace lead, cadmium and zinc ion in water samples with satisfactory results.     

The reuse of dried activated sludge for adsorption of reactive dye

Adsorption processes are alternative effective methods for removal of textile dyes from aqueous solutions. The adsorption ability of adsorbent affects by physico-chemical environment for this reason in this paper effect of initial pH, dye concentrations, temperature and dye hydrolyzation were determined in a batch system for removal of reactive dye by dried activated sludge. The Langmuir isotherm model was well described of adsorption reactive dye and maximum monolayer adsorption capacity (at pH 2) of activated sludge was determined as 116, 93 and 71mgg(-1) for 20 degrees , 35 degrees and 50 degrees C, respectively. Initial pH 2, 20 degrees C and 30min contact time are suitable for removal of reactive dyes from aqueous solutions. Activated sludge was characterized by FT-IR analysis and results showed that active sludge has different functional groups and functional groups of activated sludge are able to react with dye molecules in aqueous solution. The pseudo first-order, second-order and intraparticle diffusion kinetics were used to describe the kinetic data. The pseudo second-order kinetic model was fit well over the range of contact times and also an intra particle diffusion kinetic model was fit well but in the first 30min. The dye hydrolyzation was affected adsorption capacity of biomass and adsorption capacity of biomass decreased with dye hydrolyzation from 74 to 38mgg(-1).     

Heavy metal speciation and leaching behaviors in cement based solidified/stabilized waste materials

A circuit board printing factory sludge containing high concentrations of copper, zinc and lead was stabilized and solidified (S/S) with different portions of ordinary Portland cement (OPC) and pulverized fly ash (PFA). The chemical speciation and leaching behavior of heavy metals in these cement-based waste materials were studied by different sequential extraction procedures, standard toxicity characteristic leaching procedure (TCLP) and progressive TCLP tests. The sequential extraction results showed that more than 80% of Cu, Pb and Zn were associated with Fraction 2 (weak acid soluble, extracted with 1M NaOAc at pH 5.0 with a solid to liquid ratio of 1:60). This indicated that the heavy metals could exist in the S/S matrix as metal hydrated phases or metal hydroxides precipitating on the surface of calcium silicate hydrates (C-S-H), PFA and sludge particles. The progressive TCLP test results and MINTEQA2 calculation also showed the importance of Cu and Zn oxides during the leaching process. The leaching behaviors of these metals in the S/S waste materials were mainly controlled by the alkaline nature and acid buffering capacity of the S/S matrix. During the progressive TCLP tests, the alkaline conditions and acid buffering capacity of the matrix decreased with the dissolution of calcium hydroxide and C-S-H, therefore, the leaching of heavy metals in the S/S waste materials increased. The leaching of heavy metals in the S/S materials can be considered as a pH dependent and corresponding metal hydroxide solubility controlled process.     

Total concentrations and speciation of heavy metals in municipal sludge from Changsha, Zhuzhou and Xiangtan in middle-south region of China

The presence of heavy metals in municipal sludge restricts its use for agricultural purposes. In this paper, the bioavailability and eco-toxicity of heavy metals in municipal sludge was evaluated, taking into consideration both the speciation of metals and the local environmental characteristics. The dewatered municipal sludge samples were collected from five sewage plants in Changsha, Zhuzhou and Xiangtan respectively, which are representative cities with characteristics of the middle-south region of China. Some agricultural significant parameters and total metal concentrations in the sludge were determined and the metal speciation was studied by using BCR sequential extraction procedure. It was found experimentally that in general the municipal sludge collected from the five sewage plants was rich in organics, N and P. Except that the sludge from Xia Wan Sewage Treatment Plant showed higher concentrations of heavy metals, the sludge from other plants all showed a low total content of heavy metals with only Cd slightly exceeding the permitted values of the national application standard of acid soil in China (GB18918-2002). The sequential extraction results showed that Cu and Zn were principally distributed in the oxidizable fraction, which meant a high potential toxicity, but the bioavailability of Zn might be overestimated to the soil of Hunan. Pb was mainly in the residual fraction. The distribution of Cd showed no obvious characteristics.     

Adsorption characteristics of heavy metal ions onto a low cost biopolymeric sorbent from aqueous solutions

In this study, the adsorption conditions of Cu(II), Pb(II) and Cd(II) metal ions onto sporopollenin have been studied. The different variables effecting the sorption capacity such as pH of the solution, adsorption time, initial metal ion concentration and temperature have been investigated. Adsorption isotherms correlated well with the Freundlich type adsorption isotherm and adsorption capacities were found to be 0.0195, 0.0411 and 0.0146 mmol g(-1) for Cu(II), Pb(II) and Cd(II) metal ions, respectively. Experimental data were also evaluated to find out kinetic characteristics of the adsorption process. Adsorption processes for three target heavy metal ions were found to follow pseudo-second order type adsorption kinetics. Intraparticle diffusion was found to take part in adsorption processes but it could not be accepted as the primary rate-determining step. The mean free energies of adsorption (E) were found to be between 8 and 16 kJ mol(-1) for the metal ions studied and therefore adsorption mechanism for the adsorbent was explained as an ion-exchange process. But it was observed that chelating effect is also playing an important role in the adsorption of metal ions onto sporopollenin. Thermodynamic parameters, DeltaH degrees , DeltaS degrees and DeltaG degrees were also calculated from graphical interpretation of the experimental data. Standard heats of adsorption (DeltaH degrees ) were found to be endothermic and DeltaS degrees values were calculated to be positive for the adsorption of Cu(II), Pb(II) and Cd(II) ions onto the adsorbent. Negative DeltaG degrees values indicated that adsorption process for these three metal ions onto sporopollenin is spontaneous.     

Biosorption of cadmium by various types of dried sludge: an equilibrium study and investigation of mechanisms

Batch equilibrium sorption experiments were used for screening for cost-effective four types of sludge, which were DWS (drinking water treatment plant sludge), LLS (landfill leachate sludge), ADSS (anaerobically digested sewage sludge), and SS (sewage sludge). SS removed cadmium most efficiently from aqueous solution (0.38 mmol/g), and showed the highest desorption efficiency (26.3%). Only the SS can be fitted by Langmuir isotherm model (r2 = 0.996). The FT-IR spectra of SS and cadmium loaded SS indicated that carboxyl groups were major binding sites of cadmium binding sites. In kinetic experiment, it was found that the uptake of the metal by the SS was accompanied with proton release, indicating that the metal binding occurs via an ion exchange as well as by electrostatic interaction between carboxylate groups and cadmium ions. This sorbent may have a potential for use as high-value biosorbent of heavy metals and it deserves further investigations into the details of practical application, for example on the development of desorption methods and on sorption process optimization.     

Chelant extraction of heavy metals from contaminated soils.

The current state of the art regarding the use of chelating agents to extract heavy metal contaminants has been addressed. Results are presented for treatability studies conducted as worst-case and representative soils from Aberdeen Proving Ground's J-Field for extraction of copper (Cu), lead (Pb), and zinc (Zn). The particle size distribution characteristics of the soils determined from hydrometer tests are approximately 60% sand, 30% silt, and 10% clay. Sequential extractions were performed on the 'as-received' soils (worst case and representative) to determine the speciation of the metal forms. The technique speciates the heavy metal distribution into an easily extractable (exchangeable) form, carbonates, reducible oxides, organically-bound, and residual forms. The results indicated that most of the metals are in forms that are amenable to soil washing (i.e. exchangeable+carbonate+reducible oxides). The metals Cu, Pb, Zn, and Cr have greater than 70% of their distribution in forms amenable to soil washing techniques, while Cd, Mn, and Fe are somewhat less amenable to soil washing using chelant extraction. However, the concentrations of Cd and Mn are low in the contaminated soil. From the batch chelant extraction studies, ethylenediaminetetraacetic acid (EDTA), citric acid, and nitrilotriacetic acid (NTA) were all effective in removing copper, lead, and zinc from the J-Field soils. Due to NTA being a Class II carcinogen, it is not recommended for use in remediating contaminated soils. EDTA and citric acid appear to offer the greatest potential as chelating agents to use in soil washing the Aberdeen Proving Ground soils. The other chelating agents studied (gluconate, oxalate, Citranox, ammonium acetate, and phosphoric acid, along with pH-adjusted water) were generally ineffective in mobilizing the heavy metals from the soils. The chelant solution removes the heavy metals (Cd, Cu, Pb, Zn, Fe, Cr, As, and Hg) simultaneously. Using a multiple-stage batch extraction, the soil was successfully treated passing both the Toxicity Characteristics Leaching Procedure (TCLP) and EPA Total Extractable Metal Limit. The final residual Pb concentration was about 300 mg/kg, with a corresponding TCLP of 1.5 mg/l. Removal of the exchangeable and carbonate fractions for Cu and Zn was achieved during the first extraction stage, whereas it required two extraction stages for the same fractions for Pb. Removal of Pb, Cu, and Zn present as exchangeable, carbonates, and reducible oxides occurred between the fourth- and fifth-stage extractions. The overall removal of copper, lead, and zinc from the multiple-stage washing were 98.9%, 98.9%, and 97.2%, respectively. The concentration and operating conditions for the soil washing extractions were not necessarily optimized. If the conditions had been optimized and using a more representative Pb concentration (approximately 12000 mg/kg), it is likely that the TCLP and residual heavy metal soil concentrations could be achieved within two to three extractions. The results indicate that the J-Field contaminated soils can be successfully treated using a soil washing technique.     

Evaluation of the effectiveness of various amendments on trace metals stabilization by chemical and biological methods

We evaluated the effects of five different kinds of amendments on heavy metals stabilization. The five amendments were: zero valent iron, limestone, acid mine drainage treatment sludge, bone mill, and bottom ash. To determine bioavailability of the heavy metals, different chemical extraction procedures were used such as, extraction with (Ca(NO(3))(2), DTPA; toxic characteristic leaching procedure (TCLP), physiologically based extraction test (PBET) that simulates gastric juice, and sequential extraction test. Bioavailability was also determined by measuring uptake of the heavy metals by lettuce (Lactuca sativa L.) and earthworms (Eisenia fetida). In addition, dehydrogenase activity was measured to determine microbial activity in the soil with the different amendments. The addition of amendments, especially limestone and bottom ash, resulted in a significant reduction in extractable metal contents. Biological assays using lettuce, earthworm, and enzyme activity were found as appropriate indicators of available metal fraction after in situ stabilization of heavy metals. In conclusion, TCLP and sequential extraction test appear to be promising surrogate measure of metal bioavailability in soils for several environment endpoints.     

Effect of metal spiking on different chemical pools and chemically extractable fractions of heavy metals in sewage sludge

A laboratory experiment was conducted to study the effect of metal spiking and incubation on some properties and sequentially extractable chemical pools of some heavy metals (F1, two extractions with 0.1 M Sr(NO3)2; F2, one extraction with 1 M NaOAc (pH 5.0); F3, three extractions with 5% NaOCl (pH 8.5) at 90-95 degrees C; F4, three extractions with 0.2 M oxalic acid + 0.2 M ammonium oxalate + 0.1 M ascorbic acid (pH 3.0); and F5, dissolution of sample residue in HF-HClO4 (residual fraction,) and also 1 M CaCl2 and 0.005 M DTPA extractable heavy metals in sewage sludge. Metal spiking and incubation decreased pH and easily oxidizable organic C content of sludge but increased electrical conductivity. Metal spiking and incubation increased F1 fraction of all heavy metals, F2 fraction of Ni, Pb, Cu, and Cd, F3 fraction of Pb, Cu, and Cd, F4 or reducible fraction of Ni, Cu, and Cd and residual fraction of Zn and Pb, but decreased F2 fraction of Zn, F3 of Zn and Ni, F4 fraction of Zn and F5 fraction of Ni, Cu, and Cd. Metal spiking and incubation increased 1 M CaCl2 and 0.005 M DTPA extractable amounts of all heavy metals in sludge except for 0.005 M DTPA extractable Zn, which registered only very marginal decrease.     

Waste metal hydroxide sludge as adsorbent for a reactive dye

An industrial waste sludge mainly composed by metal hydroxides was used as a low-cost adsorbent for removing a reactive textile dye (Remazol Brilliant Blue) in solution. Characterization of this waste material included chemical composition, pH(ZPC) determination, particle size distribution, physical textural properties and metals mobility under different pH conditions. Dye adsorption equilibrium isotherms were determined at 25 and 35 degrees C and pH of 4, 7 and 10 revealing reasonably fits to Langmuir and Freundlich models. At 25 degrees C and pH 7, Langmuir fit indicates a maximum adsorption capacity of 91.0mg/g. An adsorptive ion-exchange mechanism was identified from desorption studies. Batch kinetic experiments were also conducted at different initial dye concentration, temperature, adsorbent dosage and pH. A pseudo-second-order model showed good agreement with experimental data. LDF approximation model was used to estimate homogeneous solid diffusion coefficients and the effective pore diffusivities. Additionally, a simulated real effluent containing the selected dye, salts and dyeing auxiliary chemicals, was also used in equilibrium and kinetic experiments and the adsorption performance was compared with aqueous dye solutions.     

Leaching behaviour of a galvanic sludge in sulphuric acid and ammoniacal media

Leaching studies of a sludge produced by the physico-chemical treatment of wastewaters generated by a Ni/Cr plating plant were carried out in both sulphuric acid and ammoniacal media aiming to decide which of them would be the best treatment for this kind of waste material. The dissolution behaviour of some metals (Cu, Ni, Cr and Zn) was studied in order to assure the best metal recovery conditions in subsequent processes by the use of some separation methods such as solvent extraction and precipitation techniques. Therefore, the study here presented deals with the first chemical stage of an integrated treatment process. For the sulphuric acid leaching, maximal conversions obtained were 88.6% Cu, 98.0% Ni and 99.2% Zn for the following experimental conditions: a 100 g L(-1) acid concentration, a 5:1 liquid-to-solid ratio (L/S), a particle size less than 1 mm, a digestion time of 1h, a stirring speed of 700 rpm (all at room temperature and under atmospheric pressure). As expected, no selectivity was achieved for the sulphuric acid leaching, despite this option yielding much higher metal ion dissolution when compared with that reached by ammoniacal leaching. The use of this latter medium allowed the extraction of Cu and Ni without Cr species, but rates of conversion were only about 70% for Cu and 50% for Ni, much lower than those obtained for sulphuric acid leaching.     

Total concentrations and fractions of Cd, Cr, Pb, Cu, Ni and Zn in sewage sludge from municipal and industrial wastewater treatment plants

Heavy metals are one of the important factors that affect the final disposal of sewage sludge. In this paper, the metal mobility and bioavailability of heavy metals in sewage sludge were studied by using Community Bureau of Reference (BCR) sequential extraction procedure to get more information for the reasonable disposal of sludge. Sewage sludge was collected from five municipal wastewater treatment plants and three industrial wastewater treatment plants. The sludge was examined for and the total concentrations and different chemical fractions of Cd, Cr, Pb, Cu, Ni and Zn. The total metal concentrations of heavy metals in sludge varied greatly. The contents of Zn and Cu were the highest, followed by then Cr, Ni and Pb and the content of Cd was the least. There was no significant difference in total metal concentration between municipal and industrial wastewater treatment plants. Fractions extracted by the BCR sequential procedure were acid soluble/exchangeable, reducible and oxidizable fraction. Sludge pH was found to have profound effect on the chemical fractions of heavy metals. Acidic sludges (Xiamen and Jinlin Petrochemical Group Co., wastewater treatment plant) had higher proportion of the acid soluble/exchangeable fractions than in neutral sludge. In neutral sludges, Pb and Cr were principally distributed in between the oxidizable fraction and the residual fraction; Cu was in the oxidizable fraction; Cd mainly in the residual fraction in municipal wastewater treatment plants and had high percentage of acid soluble/exchangeable and reducible fractions in industrial wastewater treatment plants; Ni and Zn had higher percentage in the acid soluble/exchangeable and the oxidizable fraction.     

Kinetics and equilibrium studies on biosorption of cadmium, lead, and nickel ions from aqueous solutions by intact and chemically modified brown algae

The present study deals with the evaluation of biosorptive removal of Cd (II), Ni (II) and Pb (II) ions by both intact and pre-treated brown marine algae: Cystoseira indica, Sargassum glaucescens, Nizimuddinia zanardini and Padina australis treated with formaldehyde (FA), glutaraldehyde (GA), polyethylene imine (PEI), calcium chloride (CaCl(2)) and hydrochloric acid (HCl). Batch shaking adsorption experiments were performed in order to examine the effects of pH, contact time, biomass concentration, biomass treatment and initial metal concentration on the removal process. The optimum sorption conditions for each heavy metal are presented. One-way ANOVA and one sample t-tests were performed on experimental data to evaluate the statistical significance of biosorption capacities after five cycles of sorption and desorption. The equilibrium experimental data were tested using the most common isotherms. The results are best fitted by the Freundlich model among two-parameter models and the Toth, Khan and Radke-Prausnitz models among three-parameter isotherm models for Cd (II), Ni (II) and Pb (II), respectively. The kinetic data were fitted by models including pseudo-first-order and pseudo-second-order. From the results obtained, the pseudo-second-order kinetic model best describes the biosorption of cadmium, nickel and lead ions.     

Influence of physicochemical treatments on iron-based spent catalyst for catalytic oxidation of toluene

The catalytic oxidation of toluene was studied over an iron-based spent and regenerated catalysts. Air, hydrogen, or four different acid solutions (oxalic acid (C2H2O4), citric acid (C6H8O7), acetic acid (CH3COOH), and nitric acid (HNO3)) were employed to regenerate the spent catalyst. The properties of pretreated spent catalyst were characterized by the Brunauer Emmett Teller (BET), inductively coupled plasma (ICP), temperature programmed reduction (TPR), and X-ray diffraction (XRD) analyses. The air pretreatment significantly enhanced the catalytic activity of the spent catalyst in the pretreatment temperature range of 200-400 degrees C, but its catalytic activity diminished at the pretreatment temperature of 600 degrees C. The catalytic activity sequence with respect to the air pretreatment temperatures was 400 degrees C>200 degrees C>parent>600 degrees C. The TPR results indicated that the catalytic activity was correlated with both the oxygen mobility and the amount of available oxygen on the catalyst. In contrast, the hydrogen pretreatment had a negative effect on the catalytic activity, and toluene conversion decreased with increasing pretreatment temperatures (200-600 degrees C). The XRD and TPR results confirmed the formation of metallic iron which had a negative effect on the catalytic activity with increasing pretreatment temperature. The acid pretreatment improved the catalytic activity of the spent catalyst. The catalytic activity sequence with respect to different acids pretreatment was found to be oxalic acid>citric acid>acetic acid>or=nitric acid>parent. The TPR results of acid pretreated samples showed an increased amount of available oxygen which gave a positive effect on the catalytic activity. Accordingly, air or acid pretreatments were more promising methods of regenerating the iron-based spent catalyst. In particular, the oxalic acid pretreatment was found to be most effective in the formation of FeC2O4 species which contributed highly to the catalytic combustion of toluene.