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Separation of Heavy Metal ions by using Modified Amberlite IR-400 (cl) ResinSANJAY YADAV GUIDED BY-EXAM NO. 4200 Dr. Ran Bahadur11ACKNOWLEDGEMENTI would like to convey my deep regards to my project supervisor DR. RAN BAHADUR, Assistant Professor, Applied Chemistry Department, Faculty of Technology & Engineering, Kalabhavan. I thank him for his patience, guidance, regular monitoring of the work and inputs, without which this work could have never come to fruition. Indeed, the experience of working under him is one of that I will cherish forever.I am extremely thankful to Prof. P.T.DEOTA, Head, Applied Chemistry Department, Faculty of Technology & Engineering, Kalabhavan, The M. S. University of Baroda for providing me the various laboratory and instrumental facilities during my project work. Also want to acknowledge my classmates and friends who direcltly or indirectly supported me.21.INTRODUCTIONHeavy metals as a non biodegradable materials

Highly toxic

Sources of heavy metal ions emission

Majority sources are industrial sources they directly release into ecosystem

Toxicity persists in both form chemical as well as elemental form

3Techniques used for separation of heavy metal ions;Ion exchangeAdsorptionPrecipitation.

Technique of current interest is Ion exchange.

Cadmium and lead metal ions of current toxicology concern.4Ion exchange :It is a mechanism by which ions are exchanged particularly of same charge Ion exchangersIt can be easily modified , depends upon application various application like :Water softeningWater purification, decontamination Food and beverages 5Current resin is AMBERLITE IR-400TYPE: chelating resinStrongly basic, clear gel, weak anion exchanger Matrix : styrene DVB copolymerTotal exchange capacity : 3.1Modification : tri-methyl ammonium6Polymeric Resin physical form

7AIMThe aim of the present work is to develop preconcentration system for the determination of trace level of Pb (II) and Cd (II) from the aqueous solution by employing batch method using Amberlite IRA-400 modified / functionalized with EDTA .

By using Complexometric EDTA titration for determination of lead and cadmium using xylenol orange as indicator.8MODIFICATION 5.0 g Amberlite IR-400 resin in Cl- form was treated with 250 ml of aqueous solution of 0.1M EDTA contents were left for 24 hours with intermittent shaking to ensure the optimum adsorption.

The resin was separated from the solution and washed several times with demineralized water until the supernatant liquid was found free from excess reagent.

Finally, the resin was dried in an oven at 60 degree celsius9MODIFICATION

10CHARACTERIZATION : IR SPECTRARESIN AMBERLITE

11IR SPECTRA OF MODIFIED RESIN

12METAL REMOVAL0.1 gm of the functionalized resin was taken in 10 ml of metal ion solution of different concentrations (0.001M 0.01M) for different hours of sets (1hr, 2hrs, 3hrs,, 24hrs). Then solution was decanted and washed with 5ml (3 portions) DM water

Metal ions were determined from decanted solutions by using Complexometric titration

To 10 ml metal solution, add 10ml of distilled water and 2-3 drops of xylenol orange as an indicator. Hexamine powder has been added with shaking and titrated against 0.002M EDTA solution until colour changes from red to lemon yellow.

13METAL REMOVAL

14IR SPECTRA : Metal loaded resin

15DISTRIBUTION BEHAVIOUR10ml metal ion solution (0.001-0.01M) was shaken with 0.1 gm of modified resin in stoppered conical flasks at room temperature for different time intervals (1hr, 2hrs, 3hrs, ., 24hrs).

The supernatant liquid was decanted after every prescribed time interval, and the metal ion concentration evaluated. 16DISTRIBUTION BEHAVIOUR

17pH EffectSorption of metal ions Cd2+ and Pb2+ using Functionalized Amberlite IR-400 with EDTA was carried out in the pH range 1-8 and 1-6 respectively. To 0.1 gm of exchanger, 10 ml of metal ion solution was added, pH adjusted in acidic range using dilute HNO3 and in alkaline range using dilute NaOH and resulting mixture shaken for 5hrs for Pb2+ metal ion solution and 4hrs for Cd2+ metal ion solution. The supernatant liquid was used to determine the metal ion concentration by EDTA titrations.18In both the cases around neutral pH, percentage uptake of the metals ions is more. When pH is lowered consequently percentage uptake of metal ions is also decreased.

Adsorption of metal ions also decreased with decreased the pH.

We can conclude that uptake of metal ion also a function of pH.19

20ELUTION For this type of study column is prepared and the metal ion solution is loaded on the resin, metal solution 0.003M, 10mL is loaded on the resin. Then the metal loaded is eluted with different types of eluting agents such as HCLO4, CH3COOH, and NH4NO3 at a concentration of 0.02 and 0.2 M. The metal recovered can be easily calculated in terms of percentage elution as E (%) =( Ce/C0)*100, where Ce is the concentration of metal ion in the eluted solution and C0 is the concentration of metal ion loaded onto the column.21% Elution of metal ionsMetal ionNH4NO3 (0.02M)NH4NO3 (0.2M)HClO4- (0.02M)HClO4- (0.2M)CH3COOH (0.02M)CH3COOH (0.2M)Cd+2757976808490Pb+275836870687822BINARY SEPARATION Binary separation of lead and cadmium has been performed using concept of separation factor in a particular medium , in case of binary separation maximum metal eluted is Cd+2 i.e 92% and Pb+2 is 83%.

This observation is in keeping with separation factor () and Kd values of metal ions, metal ion with high Kd value is less eluted and vice versa.

So it could be concluded that resin material is an effective chelate ion exchanger.23% Elution of metal ions (Binary)Metal ionCH3COOH (0.2M)Metal ionHClO4- (0.2M)Cd+288Pb+278Metal ionCH3COOH (0.2M)Metal ionNH4NO3Cd+292Pb+28424CURVES 25REGENERATIONThis experiment is performed for lead by batch method .0.003M concentration of pb is treated with 0.2M Ammonium nitrate and kept for 3 hours.

After 3 hours of shaking then it is decantated and titrated with same concentration of EDTA.

This process is repeated for several times upto 6 cycles. This process is repeated till wide variation in kd value is observed .26RETENTION GRAPH

27CONCLUSIONSIn present work, the Amberlite-IR 400 has been functionalized with Na2H2Y.The functionalized materials were characterized with FTIR, TGA and EDX.The adsorption capacity of functionalized resin was evaluated for removal of toxic metal ions like lead and cadmium. The most promising property of the functionalized resin is its high selectivity for Pb2+ and Cd2+.Extensive studies such as variation in concentration of metal ions, time variation and effect of pH on absorption have been studied.Elution studies observed for metal ions were also promisingBinary separations gave an idea of selection of particular ion in presence of other.Good reusability, but after 4 cycles its efficiency is decreased.

28REFERENCE1) Ion Exchange Letters 2 (2009) 1-142) The second book of Moses, Exodus, Chapt.15, verse 253) B.A. Aristotle, works, 7 (about 330, B.C.), 933 b4) H.S. Thompson, J. Roy, Agr. Soc. Eng. 11(1850) 685) J.T. Way, Agr. Soc. Eng. 11 (1850) 3136) E. Eichorn, Ann. Phys. Chem. 105 (1850) 1267) A. Rumpler, Inttern. Kongr. f. angrew Chem., Berlin (1903) 598) J. Lamberg, Z. Dent. Geal. Gos. 22 (1870) 3559) G. Wiegner, J. Land Wirisch 60 (1912) 11110) O. Folin, R. Bell, J. Biol. Chem. 29 (1917) 329erdam, (1964)

2911) R. Gans, Jahrb. preuss. geol. Landesanstalt 26 (1905) 17912) B.A. Adams, E.L. Holmes, J. Chem. Soc. Ind., 54T (1935) 113) K.A. Kraus, H.O. Phillips, J. Amer. Chem. Soc. 78 (1956) 64414) K.A. Kraus, H.O. Phillips, T.A. Carlson, J.S. Johnson, Proceeding of second international conference on peaceful uses of Atomic Energy, Geneva, 1958, Paper No.15/P/1832, United Nations, 28, 3 (1958)16) C.B. Amphlett, L.A. Mcdonald, Proc. Chem. Soc. (1962) 27617) A Text book of Quantitative Inorganic Analysis including Elementary Instrumental Analysis by Arthur I. Vogel, D.Sc. (Lond.), D.I.C., F.R.I.C., third addition, chapter 9, p.702-708, chapter 4, p.443,444

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