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Adsorption behavior of ytterbium (III) on gel-type weak acid resin

ZHENG Zhanwang ( ), XIONG Chunhua ( )
(Department of Applied Chemistry, Zhejiang Gongshang University, Hangzhou 310012, China) Received 11 January 2011; revised 22 February 2011

Abstract: The adsorption and desorption behaviors of Yb(III) on gel-type weak acid resin (110) were investigated. The influence of operational conditions such as contact time, initial concentration of Yb(III), initial pH of solution and temperature on the adsorption of Yb(III) were also examined. The results showed that the optimal adsorption condition of 110 resin for Yb(III) was achieved at pH=5.5 in HAc-NaAc medium. The maximum uptake capacity of Yb(III) was 265.8 mg/g at 298 K. Yb(III) could be eluted by using 3.0 mol/L HCl solution and the 110 resin could be regenerated and reused. The adsorption of Yb(III) followed the Langmuir isotherm, and the correlation coefficients were evaluated. Various thermodynamic parameters such as standard enthalpy change ( H), standard entropy change ( S) and standard free energy change ( G) were evaluated. The adsorption of Yb(III) on the 110 resin was found to be endothermic in nature. Thomas model was successfully applied to experimental data to predict the breakthrough curves and to determine the characteristics parameters of the column useful for process design. And the resin sample both before and after adsorption was described by IR spectroscopy. Keywords: gel-type weak acid resin (110 resin); ytterbium(III); adsorption; parameter; Thomas model; rare earths

Rare earth elements (REEs) have been regarded as the vitamin of metals, which means that a minute amount of REEs may greatly enhance the properties of metals. Ytterbium(Yb) is one of the most significant rare earth elements, which has attracted special attention due to its unique properties and wide range of applications. Yb can be used in optical materials, dentistry as well as stainless steel to help improve the properties of those materials; the 169Yb isotope has been used as a radiation source substitute for a portable X-ray machine[14]. However, as industry expands, ytterbium which is also one of the harmful elements persists in the environment and often creates long-term contamination problems. Therefore, extraction and preconcentration of these valuable ions from wastes are extremely important not only from the view of their limited resource availability, but also for the reduction of their quantum for disposal as wastes. Different methods have been proposed for separation and preconcentration of REEs, such as co-precipitation, solvent extraction, ion-exchange and solid phase extraction[59]. Solvent extraction and ion-exchange are the two most common methodologies for the preconcentration and separation of trace elements from various matrices[10]. Solvent extraction is inefficient due to the requirement of large volume of solvent, which may create health problem. In addition, solvent extraction procedures are usually time-consuming and labor-intensive [1113]. Ion exchange resins have been used in the chemical analysis for over 50 years[11]. They are solid and suitably insolubi-

lized high molecular weight polyelectrolytes which can exchange their mobile ions for ions of equal charge from the surrounding medium. The resulting ion exchange is reversible and stoichiometric with the displacement of one ionic species by another on the exchanger. 110 resin is a polymeric material containing a functional group (COOH). It has oxygen atom that can coordinate directly with metal ions[14,15]. 110 resin which can be used repeatedly has the advantages of high stability and adsorption capacity. The high adsorption rate of 110 resin due to its unique properties opens the door to the application in industry. In this work, the adsorption and desorption of Yb(III) ion on 110 resin using batch and column methods were investigated. Some factors affecting adsorption, such as contact time, initial pH of solution, initial concentration of Yb(III) ion and temperature were examined. Furthermore, kinetics and isotherm adsorption experiments were carried out. Thomas model was applied to experimental data obtained from column experiments. With the mentioned above, 110 resin can be widely used in the recovery of Yb(III) from aqueous solution.

1 Materials and methods

1.1 Apparatus The Yb(III) ion was determined with Shimadzu UV-2550 UV-VIS spectrophotometer. Mettler toledo delta 320 pH

Foundation item: Project supported by the grants from the National Key Technologies Research and Development Program of China (2008BAD94B09), and the Key Grant of Education Department of Zhejiang Province, China (Z200907459) Corresponding author: XIONG Chunhua (E-mail: xiongch@163.com; Tel.: +86-571-88932083) DOI: 10.1016/S1002-0721(10)60469-3

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meter was used for measuring pH of solutions. The sample was shaken in a DSHZ-300A and a THZ-C-1 temperature constant shaking machine. The water used in the present work was purified using a Molresearch analysis-type ultrapure water machine. 1.2 Materials 110 resin was supplied by The Chemical Plant of Nankai University (Tianjin, China) and the properties are shown in Table 1. The stock solutions of Yb(III) ion were prepared from Yb2O3 (A.R.). HAc-NaAc buffer solution with pH= 3.506.50 and C6H15O3N-HNO3 buffer solutions with pH= 7.2 were prepared from the NaAc, HAc, C6H15O3N and HNO3 solutions. The chromophoric reagent of 0.1% arsenazo-I solution was obtained by dissolving 0.1000 g arsenazo-I powder into 100 ml deionized water. All other chemicals were of analytical grade and purified water was used.
Table 1 General description and properties of 110 resin
Item Resin Functional group Capacity/(mmol/ml) Containing moisture/% Wet superficial density/(g/ml) True wet density/(g/ml) Property Gel-type weak acid resin COOH 12 70.080.0 0.700.80 1.101.15

and inlet concentrations were equal. All the experiments were carried out at room temperature. 1.4 Analytical method A solution containing lower than 75 g of Yb (III) was added into a 25 ml colorimetric tube, and then 1.0 ml of 0.1% arsenazo-I solution and 10 ml pH 7.2 C6H15O3N-HNO3 buffer solution were added. After the addition of deionized water to the mark of colorimetric tube, the absorbency was determined in a 1 cm colorimetric vessel at wavelength of 570 nm and compared with blank test. The adsorption amount (Q) and distribution coefficient (D) were calculated with the following formulas[17,18]: Q=(C0Ce)V/m (1) D=Q/Ce (2) where C0 (mg/ml) and Ce (mg/ml) are the initial and equilibrium Yb(III) concentrations, respectively, V (ml) is the total volume of solution, and m (g) is the mass of 110 resin.

2 Results and discussion

2.1 Influence of pH on the distribution coefficient for Yb(III) The pH of aqueous solution has been identified as the most important variable governing the adsorption capacity of adsorbent. The influence of pH on the adsorption behavior of 110 resin for Yb (III) is illustrated in Fig. 1. The uptake of Yb(III) as a function of hydrogen ion concentration was in the range of pH 3.506.50 for an initial concentration of Yb(III) ion 5.0 mg/30.0 ml at 298 K, 100 r/min. The adsorption coefficient (D) for Yb(III) ion was the highest when pH value was 5.50 in the HAc-NaAc medium and decreased by either raising or lowering pH under the experimental conditions. At lower pH values, the Yb(III) ion uptake was inhibited in the acidic medium, which can be attributed to the presence of H+ ion competing with the Yb(III) ion for the adsorption sites. In contrast, the Yb(III) ion is prone to precipitation at higher pH values. Therefore, all the following experiments were performed at pH 5.5 in the HAc-NaAc system.

1.3 Adsorption experiments Experiments were run in a certain range of pH, temperature, initial Yb(III) ion concentrations, and contact time as well as adsorption isotherms[16]. The operation for the adsorption and desorption of Yb(III) ion is usually carried out in batch vessels and glass columns. Batch experiments were performed under kinetic and equilibrium conditions. A desired amount of treated 110 resin was weighed and added into a conical flask, in which a desired volume of buffer solution with pH 5.5 was added. After 24 h, a required amount of standard solution of Yb(III) ion was put in. The flask was shaken in a shaker at constant temperature. The upper layer of clear solution was taken for analysis until adsorption equilibrium reached. The procedure of kinetic tests was identical to that of the equilibrium tests. The concentrations of Yb(III) ion of aqueous samples were measured at preset time intervals. Continuous flow adsorption experiments were conducted in a vertical glass column of 0.45 cm inner diameter and 23.5 cm height filled with Yb(III) ion solution. At the bottom of the column, a stainless sieve was attached followed by a layer of cotton wool. The particles were dropped in from the top of the column. Time taken by the particles to travel a distance of 7.4 cm in vertical direction was noted. The Yb(III) ion solution was fed from the top at a fixed flow rate. The Yb(III) ion solutions at the outlet of the column were collected periodically and analyzed for the Yb(III) ion concentration using a UV-visible spectrophotometer at 570 nm. The flow through the column was continued till the outlet

Fig. 1 Influence of pH on the distribution coefficient of Yb(III) (Resin 15.0 mg, C0=5.0 mg/30.0 ml, T=298 K, 100 r/min)

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2.2 Isotherm adsorption curve The Langmuir model perhaps is the best known isotherm to describe adsorption from a liquid solution. The Langmuir model assumes uniform energies of adsorption on the surface and no interaction between adsorbed molecules. The model also assumes that adsorption is limited to complete surface coverage by a monomolecular layer and can be represented by the following equation[19,20]: Ce C e 1 = (3) Qe Qm bQm

where Ce (mg/ml) is equilibrium concentration of Yb(III), Qe (mg/g) the adsorbing capacity in equilibrium state, Qm (mg/g) the saturated adsorption capacity and b the Langmuir constant which reflects quantitatively the affinity between the 110 resin and Yb(III) ions. It is used to analyze batch equilibrium data by plotting Ce/Qe versus Ce, which yields a linear plot if the data conform to the Langmuir isotherm. According to the experiment data, plotting of Ce/Qe versus Ce gave a straight line and the correlation coefficient R2 (R2288 2 2 K=0.9913, R 298 K=0.9869, R 308 K=0.9958) were high as shown in Fig. 2. This was indicative of applicability of the proposed model for the process undertaken. In other words, the Langmuir-type adsorption isotherm was suitable for equilibrium studies. This indicates that the adsorption of Yb (III) ion by 110 resin is of monolayer-type[21].
2.3 Determination of adsorption rate constant at different temperatures and apparent activation energy

Fig. 3 Adsorption capacity (Q) at different contact time and temperatures (Resin=15.0 mg, C0=18.0 mg/60.0 ml, pH=5.5, 100 r/min)

The influence of contact time on the adsorption of Yb(III) ion onto 110 resin (Fig. 3) was investigated at various temperatures, i.e., 288, 298 and 308 K. The amount of adsorption increased with increasing contact time. Further, the loading half time t1/2 was 7 h and the maximum adsorption was observed after 36 h, beyond which there was almost no further increase in the adsorption. Therefore, this interaction time could be well taken as equivalent to the equilibrium time. Meanwhile, the equilibrium adsorption capacity of Yb(III) ion onto 110 resin was found to increase with increasing temperature, indicating that the adsorption of Yb(III) ion onto the adsorbent was favored at higher temperatures.

This effect suggests that the adsorption mechanism associated with Yb(III) ion onto 110 resin involves a temperature dependent process. According to Brykina method, the adsorption rate constant k can be calculated from[22,23]: (4) ln(1F)=kBt where F=Qt/Qe, Qt (mg/g) and Qe (mg/g) are the adsorption amounts at certain time and at equilibrium, respectively. The experimental results accord with the equation and a straight line is obtained by plotting ln(1F) versus t (Fig. 4) and the adsorption rate constants of 110 resin for Yb(III) can be found from the slope of the straight line, which are shown in Table 2. According to Boyd equation, it can be deduced from the linear relationship of ln(1F) versus t that the liquid film spreading is the controlling step in the adsorption process. According to the formula of Arrhenius[24]: Ea lgk lgA (5) 2.30 RT where A is the Arrhenius factor. The relationship between

Fig. 4 Determination of adsorption rate constant (Resin=15.0 mg, C0=18.0 mg/60.0 ml, pH=5.5, 100 r/min) Table 2 Adsorption rate constants of 110 resin for Yb (III)
T/K 288 298 308 Linearity relation of ln(1 F) and t y=0.0833x0.0385 y=0.0882x0.0294 y=0.0912x+0.0223 k/(10 5 s 1) 2.31 2.45 2.53 R2 0.9924 0.9934 0.9959

Fig. 2 Langmuir isotherm curves (Resin 15.0 mg, C0=5.0 mg/30.0 ml9.0 mg/30.0 ml, pH=5.5, 100 r/min)

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lgk and 1/T is shown in Fig. 5, and the slope of the straight line Kslope=174.97. So the apparent activation energy Ea= 3.35 kJ/mol can be calculated. It can be seen from the rate constant that the adsorption speed accelerates when the temperature increases within the scope.
2.4 Influence of adsorption temperature on distribution ratio and determination of thermodynamic parameters

free energy variation, G was calculated from: G= HT S (7) The thermodynamic parameters of the sorption of Yb(III) were calculated and given in Table 3. The positive values of H indicate the endothermic character of the solid phase extraction and sorption process, but the negative value of G indicates the spontaneous nature of Yb(III) sorption. The positive entropy change ( S) value corresponds to an increase in the degree of freedom of the adsorbed species.
2.5 Desorption and regeneration studies

The distribution coefficient (D) of the 110 resin for Yb (III) in the temperature range of 288308 K was measured, and the result is shown in Fig.6. A straight line was obtained by plotting lgD against 1/T with a correlation coefficient of 0.9908. The result obviously indicates that it is favorable for the adsorption with the temperature increasing. It implies that the adsorption process is endothermic. So the adsorption reaction is a chemical adsorption. The vant Hoff equation given below, can be used to calculate the enthalpy changes associated with the adsorption process of the metal ions. H S lg D (6) 2.30 RT 2.30 R where R is the universal gas constant, D the distribution coefficient and T (K) the absolute temperature. The plot of lgD versus 1/T gives a straight line, from which H (the enthalpy variation) and S (the entropy variation) were deduced from the slope and intercept of the line, respectively. And the

Whether an adsorbent is an appropriate material in removal of metal ions from aqueous solutions depends not only on its adsorptive capacity, but also on its regeneration ability. For repeated use of an adsorbent, adsorbed metal ions should be easily desorbed under suitable conditions. In this work, 15.0 mg 110 resin was added into a mixed solution composed of pH 5.5 buffer solution and desired amount of Yb(III) ion solution. After the equilibrium was achieved, the concentration of Yb(III) ion in the aqueous phase was determined, and the adsorption capacity of the 110 resin for Yb(III) ion was obtained. Then, the 110 resin separated from aqueous phase was washed three times with pH 5.5 buffer solution. The 110 resin adsorbed Yb(III) ion was shaken with 30.0 ml HCl eluant. After equilibrium was achieved, the concentration of Yb(III) ion in aqueous phase was determined and then the percentage of elution for Yb(III) ion was obtained. The results shown in Fig. 7 indicate that the percentage of elution for Yb(III) ion is different when the concentration of HCl is changed. It is evident that the 3.0 mol/L HCl solution is suitable to be the eluant.
Table 3 Thermodynamic data calculated for adsorption of Yb(III) on 110 resin
T/K 288 298 308 G/(kJ/mol) 22.80 24.45 26.10 H/(kJ/mol) 24.59 S/(J/(molK)) 164.56

Fig. 5 Relationship between lgk and 1/T (Resin=15.0 mg, C0=18.0 mg/60.0 ml, pH=5.5, 100 r/min)

Fig. 6 Influence of temperature on distribution ratio (D) (Resin= 15.0 mg, C0=5 mg/30 ml, pH=5.5, 100 r/min)

Fig. 7 Desorption of Yb(III) from 110 resin by HCl in varying concentrations (Resin=15.0 mg, pH=5.5, T=298 K, 100 r/min)

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2.6 Dynamic adsorption and desorption

2.6.1 Dynamic adsorption curve The performance of packed beds is described through the concept of the breakthrough curve. The breakthrough curve shows the loading behavior of Yb(III) to be removed from solution in a fixed bed and is usually expressed in terms of adsorbed Yb(III) concentration (Cad=inlet Yb(III) concentration (Co) outlet Yb(III) concentration (Ce)) or normalized concentration defined as the ratio of effluent Yb(III) concentration to inlet Yb(III) concentration (Ce/Co) as a function of time or volume of effluent for a given bed height[25]. The area under the breakthrough curve obtained by integrating the adsorbed concentration (Cad, mg/L) versus the throughput volume (V, ml) plot can be used to find the total adsorbed Yb(III) quantity (maximum column capacity). Total adsorbed Yb(III) quantity (Q, mg/g) in the column for a given feed concentration and flow rate is calculated from Eq. (8): V (C Ce ) 0 QC = dV (8) 0 m where m (g) is the mass of the adsorbent. The capacity value Qc (mg/g) was obtained by graphical integration as 305 mg/g. Successful design of a column adsorption process requires prediction of the concentration versus time profile or breakthrough curve for the effluent. The maximum sorption capacity of 110 resin is also in design. Traditionally, the Thomas model is used to fulfill the purpose. The model has the following form[26]:
Ce C0 = 1 1 + exp[K T (QTm C 0Ve )/ ]

with the observed data as shown in Fig. 9. The Thomas model was found in a relatively good fitness with breakthrough curve for sorption of Yb(III) on 110 resin with a R2 value 0.9869. In addition, theoretical maximum adsorption capacity value QT was very close to the experimental one Qc. Therefore, it can be concluded that the experimental data fitted well to the Thomas model, which indicates that this model was successfully used for the prediction of the breakthrough curves and can be employed to determine the characteristics parameters of the column process design. 2.6.2 Dynamic desorption curve Efficient elution of adsorbed solute from 110 resin in column was essential to ensure the recovery of metal ions as well as the reuse of resin for repeated adsorption/desorption cycles. With respect to the stripping of Yb(III) from 110 resin, 3.0 mol/L HCl eluant was employed. Desorption curve was formed by plotting the effluent concentration (Ce) versus elution volume (ml) from the column at a certain flow rate. It can be seen from Fig. 10 that the desorption flow rate was less so that the volume of elution was less which helped in easy handling and high concentration for economical recovery of Yb(III). It was observed that the total volume of eluent was 175 ml, after which further desorption was negligible. Therefore, the 3.0 mol/L HCl eluant could help in easy handling and recovering of Yb(III).

(9)

where KT (ml/(minmg)) is the Thomas rate constant, (ml/min) the volumetric flow rate, and QT (mg/g) the theoretical maximum sorption capacity value. The linearized form of the Thomas model is as follows:
C ln ( 0 Ce 1) = K TQT m K TC 0 Ve

(10)

The kinetic coefficient KT and the adsorption capacity of the bed QT can be determined from a plot of ln [(Co/Ce)1] versus t at a certain flow rate as shown in Fig. 8. The Thomas equation coefficients for Yb(III) ion adsorption were KT=9.7102 ml/(minmg) and Qc=311 mg/g. The theoretical predictions based on the model parameters were compared

Fig. 9 Dynamic adsorption curves of 110 resin for Yb(III) (Resin=150.0 mg, C0=0.1 mg/ml, pH=5.5, flow rate=0.28 ml/min, T=298 K)

Fig. 8 Thomas model for the continuous adsorption of Yb(III) (Resin=150.0 mg, C0=0.1 mg/ml, pH=5.5, flow rate=0.28 ml/min)

Fig. 10 Dynamic desorption curve of 110 resin for Yb (III) (Resin=150.0 mg, CHCl=3.0 mol/L, flow rate=0.25 ml/min, T=298 K)

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Fig. 11 Infrared spectra of 110 resin (1) Before adsorption; (2) After adsorption

2.7 IR spectra

The IR spectra of resin samples both before and after Yb(III) was adsorbed, detected and identified by IR spectrometer. From the results above (Fig. 11), it can be deduced that the sorption of Yb(III) by 110 resin can be classified as chemical sorption by ion exchange ( H>0). And the functional group of 110 resin (C=O) and Yb(III) formed chemical bonds. It was found that the characteristic absorption peak of the bond C=O (1710.77 cm 1) was sharply weakened, and the new peak (1544.62 cm 1) formed. The result shows that there are coordination bonds between oxygen atoms and Yb(III).

3 Conclusions
Yb(III) could be optimally adsorbed on 110 resin in HAcNaAc medium at pH 5.50. The statically saturated adsorption capacity of Yb(III) was 265.8 mg/g 110 resin at 298 K. The adsorption behavior of 110 resin for Yb(III) obeyed the Langmuir isotherm. The adsorption rate constant was k298 K= 2.4510 5 s 1 and the apparent activation energy was Ea= 3.35 kJ/mol. Thermodynamic parameters, S, H and G, on the adsorption for Yb(III) indicated that the adsorption process was spontaneous and endothermic. The Yb(III) adsorbed on 110 resin could be eluted by using 3.0 mol/L HCl solution as an eluant. Infrared spectra of 110 resin adsorbed Yb(III) showed that the functional group of resin was coordinated with Yb(III) to form coordination compound.

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