Separation of Heavy Metal ions by using

Modified Amberlite IR-400 (cl) Resin

SANJAY YADAV

EXAM NO. 4200

GUIDED BYDr. Ran Bahadur

ACKNOWLEDGEMENT

I 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.
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1.INTRODUCTION

Heavy 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

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Techniques used for separation of heavy metal ions;

Ion exchange

Adsorption

Precipitation.

Technique of current interest is Ion exchange.

Cadmium and lead metal ions of current toxicology concern.

Ion exchange :

It is a mechanism by which ions are exchanged particularly of same charge

Ion exchangers

It can be easily modified , depends upon application

various application like :

Water softening

Water purification, decontamination

Food and beverages

Current resin is AMBERLITE IR-400

TYPE: chelating resin

Strongly basic, clear gel, weak anion exchanger

Matrix : styrene DVB copolymer

Total exchange capacity : 3.1

Modification : tri-methyl ammonium

Polymeric Resin physical form

AIM

The 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.

MODIFICATION

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 celsius

MODIFICATION

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CHARACTERIZATION : IR SPECTRA
RESIN AMBERLITE

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IR SPECTRA OF MODIFIED RESIN

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METAL REMOVAL

0.1 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.
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METAL REMOVAL

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IR SPECTRA : Metal loaded resin

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DISTRIBUTION BEHAVIOUR

10ml 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.

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DISTRIBUTION BEHAVIOUR

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pH Effect

Sorption 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.

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In 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.

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ELUTION

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.

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% Elution of metal ions

Metal ion

NH4NO3

NH4NO3

HClO4-

HClO4-

CH3COOH

CH3COOH

(0.02M)

(0.2M)

(0.02M)

(0.2M)

(0.02M)

(0.2M)

Cd+2

75

79

76

80

84

90

Pb+2

75

83

68

70

68

78

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BINARY 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.

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% Elution of metal ions (Binary)

Metal ion

CH3COOH (0.2M)

Metal ion

HClO4- (0.2M)

Cd+2

88

Pb+2

78

Metal ion

CH3COOH(0.2M)

Metalion

NH4NO3

Cd+2

92

Pb+2

84

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CURVES
60

50

water

40

%Elution

30
20

10
0
0

10

20

30

40

50

60

70

80

90

100

Volumeofeluent(ml)

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REGENERATION

This 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 .

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RETENTION GRAPH

100
90
80
70
60

%Retention

50
40
30
20
10
0
1

Number of cycles
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CONCLUSIONS

In 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 promising

Binary separations gave an idea of selection of particular ion in

presence of other.

Good reusability, but after 4 cycles its efficiency is decreased.

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REFERENCE

1) Ion Exchange Letters 2 (2009) 1-14

2) The second book of Moses, Exodus, Chapt.15, verse 25

3) B.A. Aristotle, works, 7 (about 330, B.C.), 933 b

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7) A. Rumpler, Inttern. Kongr. f. angrew Chem., Berlin (1903) 59

8) J. Lamberg, Z. Dent. Geal. Gos. 22 (1870) 355

9) G. Wiegner, J. Land Wirisch 60 (1912) 111

10) O. Folin, R. Bell, J. Biol. Chem. 29 (1917) 329erdam, (1964)

29

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13) K.A. Kraus, H.O. Phillips, J. Amer. Chem. Soc. 78 (1956) 644

14) K.A. Kraus, H.O. Phillips, T.A. Carlson, J.S. Johnson, Proceeding of
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Elementary Instrumental Analysis by Arthur I. Vogel, D.Sc. (Lond.),
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p.443,444
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