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Ion Exchange Chromatography Separation of cadmium and zinc.


Resin used is a strongly basic anion exchange resin like Amberlite IR 400 (de acidite FF) or Duolite A (Dowax 1). Amberlite IR is a polystyrene tertiary amine resin. A cation exchanger consists of a polymeric anion and active cations while an anion exchanger is a polymeric cation with active anions. A widely used cation exchange resin is that obtained by the co polymerization of styrene and a small proportion of DVB, followed by sulphonation. An anion exchange resin is a polymer containing amine (or quaternary ammonium) groups as integral parts of the polymer lattice and an equivalent amount of anions such as chloride, hydroxyl or sulphate ions.

Preparation of anion exchange column:


Prepare an anion exchange column using 25 30g of Amberlite (Cl form). Mix the resin with about 100ml of water in a measuring cylinder and shake for a few minutes. Decant the liquid as soon as the large particles have settled. The volume of the resin should be about 25ml. stir the resin with distilled water, allow to settle and decant the supernatant liquid. Repeat the process until the supernatant liquid is clear. Transfer the resin slurry to a burette containing a plug of glass wool until a column of well packed resin about 22cm long is obtained. Do not allow the level of the liquid in the column to fall below the upper surface of the resin; the level should be preferably being about 1cm above it. Then allow the resin to settle in 0.5M HCl. Transfer the resin slurry to the column. After settling, the resin column should be about 20cm in length if a 50ml burette is used.

Separation of cadmium and zinc on an anion exchanger. Theory:


Cadmium and zinc form negatively charged chloro complexes which are absorbed by a strongly basic anion exchange resin, such as Amberlite. The maximum absorption of Cd and Zn is obtained in 0.12M hydrochloric acid containing 100g of sodium chloride per litre. The zinc is eluted quantitatively by a 2M NaOH solution containing 20g of sodium chloride per litre, while the cadmium is retained on the resin. Finally, the cadmium is eluted with 1M nitric acid. The zinc and cadmium in their respective effluents may be determined by titration with standard EDTA. Elements such as Fe(III) , Mn , Al , Bi , Ni , Co , Cr , Cu , Ti , the alkaline earth metals and the lanthanides are not absorbed on the resin in the HCl-NaCl medium.

Reagents:
Reagent 1: This solution consists of 0.12M hydrochloric acid containing 100g of analytical grade NaCl per litre. Prepare 1litre solution. Reagent 2: This consists of 2M sodium hydroxide containing 20g of sodium chloride per litre. Prepare 1litre solution. Zinc ion solution: Dissolve about 7.0g of analytical grade zinc sulphate heptahydrate in 25ml of Reagent 1. Prepare 50 ml of the solution in a standard measuring flask. Cadmium ion solution: Dissolve about 6g of analytical grade crystallized cadmium sulphate in 25ml of Reagent 1. Prepare 50ml of the solution in a standard measuring flask. EDTA solution: prepare 3 litres of 0.01M EDTA solution. Buffer Solution, pH=10: Dissolve 7.0g of analytical grade ammonium chloride and 57ml of concentrated ammonia solution in water and dilute to 100ml. Prepare 300ml of the buffer. Eriochromeblack T indicator Nitric acid: prepare 1 litre of 1M nitric acid.

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Procedure:
Wash the anion exchange column with two 20 ml portions of Reagent 1; drain the solution to about 0.5 cm above the top of the resin. Mix thoroughly equal volumes (2ml each) of the zinc and cadmium ion solutions and transfer by means of a pipette 2 ml of the mixed solution to the top of the resin column. Allow the solution to drain to within about 0.5 cm of the top of the resin and wash down the tube above the resin with a little of Reagent 1. Pass 150 ml of Reagent II through the column at a flow rate of about 4ml per min and collect the eluate (containing the zinc) in a 250ml graduated flask, dilute to volume with water. Wash the resin with about 50 ml of water to remove most of the sodium hydroxide solution. Now place a 250 ml graduated flask in position as receiver and pass 150 ml of 1M nitric acid through the column at a rate of about 4ml per min and cadmium will be eluted. Dilute the effluent to 250 ml with distilled water. The resin may be regenerated by passing Reagent 1 through the column, and can then be used again for analysis of another Zn-Cd sample. Analyses: Original zinc ion solution: Dilute 2 ml (pipette) to 100 ml in a graduated flask. Pipette 10.0ml of the diluted solution into a 250ml conical flask, add 90ml of water, 2ml of the buffer solution, and sufficient of the eriochrome black T indicator mixture to impart a pronounced red color to the solution. Titrate with standard 0.01M EDTA to a pure blue color. Zinc Iron Eluate: Pipette 50ml of the solution into a 250ml conical flask, neutralize with HCl and dilute to 100ml with water. Add 2ml of the buffer mixture then a little eriochrome black T indicator powder and titrate with standard 0.01M EDTA until the color changes from red to pure blue. Original Cadmium ion solution: Dilute 2ml (pipette) to 100ml in a graduated flask. Pipette 10.0ml of the diluted solution into a 250 ml conical flask, followed by a pinch of eriochrome black T indicator and 2ml of buffer. If the pH is correct (5-6) the solution will have a pronounced red color. Titrate with standard 0.01 M EDTA until the color changes from red to clear orange yellow. Cadmium ion eluate: Pipette 50.0ml of the solution into a conical flask, and partially neutralize (to pH 3-4) with aqueous sodium hydroxide. Add a pinch of eriochrome black T indicator and 2ml of buffer solution. Titrate with standard 0.01M EDTA to a color from red to clear orange-yellow.