Chromatography

the process of separating and analyzing mixtures involves a mobile phase and a stationary phase

Types include:

Gas chromatography High performance liquid chromatography

Gas chromatography

Separation and analysis of a gas

High performance liquid chromatography

separation and analysis of a liquid Types include: High performance partition- immiscible stationary phase High performance adsorption- finely divided silica and alumina is the stationary phase Ion exchange

Ion Exchange

makes use of ion exchange resins for the stationary phase. Resins: may be cation or anion, essentially trades ions with those in a solution (mobile phase)

Discussion Questions
2. The significance of the steps in the ionexchange procedure (from preparation to analysis) a) Soaking the resin in water for an hour before introducing to the I/E column. Why cant a dry resin be used? - Increase the moisture content of the resin - Increase strength of cross linakages

b) Keeping the water level above the top of the resin air pockets bar the solution from reacting with the resin causing errors in the reaction Make sure all resin can and will react with the solution

c) Addition of H2SO4 to the column - Regeneration-> ions are eliminated -The resin is returned to its protonated form: (RSO3)nM + H2SO4 2(RSO3-)H+ + (Mn+) (SO4-2)

d) Rate flow of 15 drops per minute - makes sure a complete reaction occurs through this rate hydrogen ions can completely exchange with the copper(II) ions If rate is faster, copper may not bind well with the resin -> copper may be flush down as eluate

e) Washing the column until the eluate has the pH equal to the pH of distilled water Copper <-> Hydrogen ions Hydrogen ions flush down as eluate pH decreases because of this When pH equals 5 (dH2O), hydrogen ions are no longer flushing down as eluate Hydrogen ions are displaced completely by copper

3. Complete balanced equation of the I/E column 2RSO3-H+ + Cu2+ (RSO3)2Cu + 2H+

4. Factors that affect ion-exchange Resin (size, type, etc.) Rate of drops Retention- how long it takes for the mobile phase to pass through the stationary phase

5. M Cu2+ in the unknown sample

Trial 1 2 3 Average M Cu2+ 0.0446 0.0446 0.06695 0.05205 when 3 is rejected, 0.0446

Calculations
Aliquot Factor: 10mL 2500 ppm Cu 50mL100mL

10mL

10mL

100 50 x = 50 10 10

M NaOH (Standardization)
1KHP:1NaOH
1molKHP 1NaOH 1 (0.4126gKHP)x x x = 0.0898 M 204.2g 1KHP (0.0225L)

Average M NaOH= 0.0892

Ppm Cu2+
1H + 1Cu 2+ 63.546g 1000mg 1 0.0892 MNaOHx(0.0002L)x x x x x x50 + 2+ 1NaOH 2H 1Cu 1g 0.010L

Average ppm Cu2+= 2834.1516 ppm Cu2+

SW

An aliquot solution of 20.00mL Cu2+ was taken from a solution of 100.0mL 3000.ppm Cu2+. That solution was then pass through a column with resin. Eluate was then titrated with NaOH (0.8620M). It was found out that 0.5000mL of NaOH was used until the endpoint was achieved. A. How much ppm (experimental) of Cu2+? B. What is the percent error?

Cause and Effect

1. Effect of air spaces on the ppm. (Liquid level fell below resin) 2. Effect of pH water not being equal to pH of eluate to the ppm. (pH of eluate is higher than pH water) 3. Effect of using the wrong resin on a solution on ppm. 4. Effect of rate flow being more than 15 drops per minute on the ppm. 5. Effect of not washing the resin with sulfuric acid on the ppm.