REMOVAL OF TOXIC METAL LEAD BY ADSORPTION ON SILCA GEL AND STUDY ITS ADSORPTION PROPERTY

A Report on laboratory Project Submitted for Partial Fulfillment of the DEGREE OF MASTER OF SCIENCE In CHEMISTRY By SOUMITA TALUKDAR

DEPARTMENT OF CHEMISTRY INDIAN INSTITUTE OF TECHNOLOGY ROORKEE ROORKEE-247667(INDIA),APRIL 2011

CANDIDATES DECLARATION
I hereby certify that the work presented in dissertation entitled REMOVAL OF TOXIC METAL LEAD BY ADSORPTION ON SILICA GEL AND STUDY ITS ADSORPTION PROPERTY has been carried out by me during the period from January 2011 to April 2011 under the supervision of Dr.K.C.Gupta,department of chemistry,Indian Institute of Technology Roorkee,Roorkee.

Signature of the candidate

Date..

Signature of the supervisor

Date

ACKNOWLEDGEMENT

I am grateful to my guide Dr.K.C.Gupta, Department of Chemistry, IIT Roorkee, for his valuable guidance, constant encouragement throughout this project work. His critical evaluation and valuable suggestions at every stage of the project work deserve to be specially acknowledged. I take this opportunity to acknowledge my sincere thanks to Prof.V.K.Gupta, Head of the Department and Dr. Bina Gupta, Suprevisor of instrumentation, Department of chemistry and all faculty members for providing the necessary facilities to carry out the project. I am grateful to Mr.Saxena and Mr. Madan pal for their spontaneous helping hand in the instrumentation room and other areas. I am extremely thankful to my classmates and other research lab, for their enthusiastic cooperation without whom I could not have completed my project work.

SOUMITA TALUKDAR

CONTENTS

CANDIDATE DECLARATION ACKNOWLEDGEMENT ABSTRACT 1. INTRODUCTION AND LITERATURE REVIEW 1.1 INTODUCTION 1.2 LITERATURE REVIEW 2. PROJECT REPORT 2.1.1 CHEMICAL USED 2.1.2 INSTRUMENTS USED 2.1.3 EXPERIMENTAL PROCEDURE 2.1.4. EXPERIMENTAL DATA 3. RESULTS AND DISCUSSION 4. CONCLUSION 5.GRAPHIC PLOTS REFERENCES

ABSTRACT
The application of adsorption of toxic metals through adsorbent like silica gel is established method for removal of toxic metals like lead. Aqueous solutions of lead nitrate were taken and were kept with silica gel for adsorption and their removal from the aqueous solution. The amount of adsorption was detected by atomic adsorption spectroscopy. Different concentration of lead solutions was also prepared to study the adsorption properties at different concentration of lead nitrate solution and it was found to obey Langmuirs isotherm. Then adsorption properties were also studied by changing the adsorption conditions, like changing the amount of the adsorbent that is amount of silica gel, keeping the remaining conditions same. The plots were also constructed to show the variations of adsorption and from the plot of various concentrations we have also calculated the specific surface area of the adsorbent, silica gel.

INTRODUCTION AND LITERATURE REVIEW

1.1 INTRODUCTION
1.1.1 Adsorption is the adhesion of atoms, ions, biomolecules or molecules of gas, liquid, or dissolved solids to a surface. This process creates a film of the adsorbate (the molecules or atoms being accumulated) on the surface of the adsorbent. It differs from absorption, in which a fluidpermeates or is dissolved by a liquid or solid. The term sorption encompasses both processes, while desorption is the reverse of adsorption. It is a surface phenomenon. Like zeolites, silica gel functions on the basis of physisorption. Adsorption occurs due to van der Waals interactions and capillary condensation at high humidity. The adsorption force is less than for zeolites, resulting in a lower adsorption capacity at low concentrations of adsorbents.. On the other hand, at higher concentrations of adsorbents, the adsorption capacity is higher than for zeolites due to the higher internal pore volume. Certain grades of silica can adsorb up to 1.2 times their own weight of water. Due to the lower adsorption forces, silica gel is also easier to regenerate.

Due to this behavior, silica gel is the material of choice when only moderately low dew points need to be achieved and the high adsorption capacity and / or good regeneration behavior of silica gel can fully be exploited. The suitability of silica gels for the adsorption of liquids or gases and vapors varies based on the pore size distribution.

In addition, narrow pore and wide pore silica gels exhibit different degrees of stability against liquid water. Liquid water can lead to a destruction of the silica gel pores in case of a narrow pore silica gel, while wide pore silica gel is not affected by the presence of liquids.

1.1.2 ATOMIC ADSORPTION SPECTROSCOPY(AAS)

AAS is a spectroanalytical procedure for the qualitative and quantitative determination of chemical elements employing the absorption of optical radiation (light) by free atoms in the gaseous state. In analytical chemistry the technique is used for determining the concentration of a particular element (the analyte) in a sample to be analyzed. AAS can be used to determine over 70 different elements in solution or directly in solid samples. Atomic absorption spectrometry was first used as an analytical technique, and the underlying principles were established in the second half of the 19th century.
The technique makes use of absorption spectrometry to assess the concentration of an analyte in a sample. It requires standards with known analyte content to establish the relation between the measured absorbance and the analyte concentration and relies therefore on Beer-Lambert Law. In short, the electrons of the atoms in the atomizer can be promoted to higher orbitals (excited state) for a short period of time (nanoseconds) by absorbing a defined quantity of energy (radiation of a given wavelength). This amount of energy, i.e., wavelength, is specific to a particular electron transition in a particular element. In general, each wavelength corresponds to only one element, and the width of an absorption line is only of the order of a few picometers (pm), which gives the technique its

elemental selectivity. The radiation flux without a sample and with a sample in the atomizer is measured using a detector, and the ratio between the two values (the absorbance) is converted to analyte concentration or mass using Beer-Lambert Law.

1.2.

LITERATURE REVIEW

According to T.Mill in his symposia paper produced before the divisional environmental chemistry, American chemical society Chicago in August 2001,talked about using known chelating agents supported on silica gel for removal of heavy metals like lead ,silver,copper,etc. The results indicate fair removal of lead ions. Md.Salim and Yukihiro Munekage in their paper, published by International Journal of Chemistry ,in February 2009,worked on lead removal from aqueous solution using silica ceramic. The results of their experiment indicate that it has extensive surface area and can be used as potential adsorbent. It was also observed that lead adsorption efficiency was high below 4.5 pH. Their results also show similar trend of lead removal by Zeolite and Sapiolite and by natural phosphate. A series of experiments were also undertaken by varying initial Pb concentration on removal of Pb from solutions.

This figure shows that adsorption of lead(II) by silica ceramic as the initial Pb concentration increased. Effect of adsorbent dose were also studied at fixed initial concentration of lead and it was observed that removal efficiency increases with increase in adsorbent,that means increase of the total available surface area of the adsorbent particles. H.H. Tran, F.A. Roddick and J.A. ODonnell in their journal in ELSVIER SCIENCE LTD. 1999 , compared the adsorption property of desiccant silica gel and chromatography silica gel for its ability to remove metal ions. Adsorption of metal ions obeyed Langmuir isotherm. Adsoprtion from lead(II)-uranium(VI) showed adsorption of lead(II) being more influenced by Uranium(VI) than vice versa due to higher affinity of silica gel for the latter. The data on effect due to pH showed that the adsorption of metals was markedly influenced by the solution pH. The pH region in which there is a rapid lead ion adsorption was found out to be 3.5-5.5. Above this the pH the adsorption curves increased very slightly or tended to level out.

The results show that the adsorption due to DSG silica gel took longer time than CSG due to difference in mean pore diameters of the two silica gel types. The isotherms for the heavy metal ions fit the Langmuir model. The adsorption was best described by ion-exchange mechanism. In a mixture of ions the affinity sequence was found to be U(VI)>Pb(II)>Cu(II)>Ni(II)>Zn(II)>Cd(II), indicating high selectivity of silica gel towards uranium. It is therefore suggested that silica gel can be used in the concentration, purification, separation of uranium from other elements over a wide concentration range. It could also be applicable to the removal of heavy metals from highly dilute solutions,where other methods may not be effective.

2. PROJECT REPORT 2.1 EXPERIMENTAL SECTION 2.1. 1. CHEMICALS USED:

LEAD NITRATE SILICA GEL

MERCK LAB REAGENT 60-120 MESH

DOUBLE DISTILLED WATER

2.1.2 INSTRUMENT USED:

ATOMIC ABSORPTION SPECTROSCOPY (AAS) PERKIN ELMER AANALYST 800

2.1.3 EXPERIMENTAL PROCEDURE

STEP 1(Calibration and calculating the unknown): 3.31 g of lead nitrate0.1(M) of lead nitrate was prepared in a 100 ml volumetric flask and its concentration in ppm was calculated. Then it was diluted to different concentrations in the

range of ppm. Four standards were prepared for detection by AAS. Those are 5ppm,10 ppm,15 ppm and 20ppm. For the calibration plot five different concentrations were prepared 5ppm,8 ppm,10ppm,15ppm and 20ppm lead nitrate solution. The solutions were detected by AAS and a calibration plot was obtained. From the calibration plot we calculated the unknown lead nitrate solution.

STEP 2

Preparation of lead nitrate solutions:

3.31 g of lead nitrate was weighed to prepare 0.1(M) lead nitrate solution. Its corresponding concentration in ppm was found out and then its diluted to different concentrations of 5ppm,8ppm,10ppm,15ppm and 20ppm.

Experimental procedure:

500mg of silica gel was weighed and added to 50 ml lead nitrate solution of different concentrations each. It was then kept for 6 hours for adsorption to take place. Then all the five solutions were filtered. First 5ml filtrate was discarded and then the filtrate was taken for detection by AAS. The value of the solutions before mixing and after mixing with the adsorbent silica gel, gives the amount of lead adsorbed on silica gel for different concentration of lead.

STEP 3

3.31g of lead nitrate was weighed and 0.1(M) solution was prepared and its concentration in ppm was determined. Then it is diluted and five solution of 10ppm was prepared. Then different amount of adsorbent was added in different solutions of 50ml. The solutions were kept for 24 hours and then filtered. First 5ml of the filtrate was discarded and then filtrate was taken and then concentration was detected by AAS.

2.1.4 EXPERIMENTAL DATA STEP 1: CALIBRATION PLOT DATA : TABLE-1

NO. OF SOLUTIONS CONCENTRATION(PPM) READING(mg/L)

1 2 3 4 UNKNOWN

5 10 15 20 8

0.254 0.509 0.870 1.10 0.451

STEP 2:

TABLE-2
NO. OF CONC.(mg/L) CONC.(mg/L) SOLUTIONS BEFORE AFTER C X (mg/L)

X /m

C/(x/m)

1 2 3 4 5

4.458 8.631 9.436 15.683 19.850

0.006 1.191 0.8578 4.683 8.354

4.980 7.440 8.578 11.000 11.496

0.0089 0.014 0.017 0.022 0.023

450 580 550 712 863

STEP 3 TABLE-3
NO. OF SOLUTIONS AMOUNT OF CONCE.BEFORE CONCE. ADSORBENT(g) (mg/L) AFTER (mg/L) 0.1 0.965 0.858 0.2 0.3 0.4 0.5 0.971 0.969 0.973 0.970 0.858 0.829 0.821 0.812

X (mg/L)
0.107 0.122 0.140 0.152 0.158

1 2 3 4 5

3. RESULTS AND DISCUSSION

From the calibration plot we can conclude that the unknown concentration corresponds to 8ppm of lead solution.

Effect of initial concentration of the lead solution

From the experimental data we observe that the adsorption increases when we increase the initial concentration of the stock lead nitrate solution. As we increase the initial concentration from 5ppm to 20ppm we observe that the amount of adsorption increases with increase in concentration and then the increase is significantly lessen. The plot of the amount of adsorbate adsorbed with the initial concentration of adsorbent shows that it obeys Langmuirs type of isotherm.(TABLE-2)

Effect of amount of the adsorbent

The experimental data suggests that with increase in the amount of adsorbent to different stock lead solution of same initial concentration of 10ppm, we observe that the efficiency of adsorption increases, may be due to the increase in surface area.(TABLE-3).

3. CONCLUSION

The calibration plot which was carried out, gives a linear plot and thus the unknown solution was calculated to be 8ppm. Adsorption studies were made on various conditions and we can conclude from the experimental datas and from the literature studies that the adsorption of metal ions by silica gel obeys Langmuirs type of isotherm. The adsorption efficiency increases when initial concentration of the metal ion increased but increase in adsorption gradually slows down at higher concentration range. The efficiency of adsorption also increases when the amount of the adsorbent that is silica gel is increased keeping the initial concentration of the lead solutions same as due to the increase in surface area for adsorption.