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Experiment 9-Ion Exchange Chromatography

Experiment 9-Ion Exchange Chromatography

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Published by Alma Pabilane

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Published by: Alma Pabilane on Jun 16, 2012
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05/02/2013

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Experiment 9: Ion-Exchange Chromatography
dela Cruz, Marie Giecel V.Pabilane, Alma L.Group 6, Chem 27.1, SEJ1, Ms. Noime WalicanMarch 19, 2011
I. Abstract
Ion-exchange chromatography is an important method of analysis for alkali metal cations and anions and for determining the distribution of complex species. In this experiment, the equivalent weight of the salt sodium chloride withmolecular weight 58.44 g/mol is determined by ion-exchange chromatography, particularly anion exchange, using sodiumhydroxide as eluting agent. The NaCl solution being the mobile phase was passed through a column of tightly packed anion-exchanger resin, which is the stationary phase. The anion of the resin, which is HO
-
is exchanged with the anion of the saltwhich is Cl
-
. The liberated HO
-
was titrated to methyl red end point using 3.1 mL of standard 0.1162 M hydrochloric acid. Theexperimentally determined equivalent weight of the salt was 56.015 g/eq, having a negative percent error of 4.15%.
II. Keywords:
ion-exchange chromatography, equivalent weight, resin, eluting agent
III. Introduction and Principles
 A lot of common chemical species such as alkalimetal cations and halide anions are difficult to measure inlarge amounts because they do not readily form insolubleprecipitates or colored complexes which would help in theanalysis of these species. Moreover, some metal ions maybe present in a solution as stable complex species such asthe case of Fe(CN)
63-
and CoCl
42-
or in different oxidationstates such as U
4+
or UO
22
. Ion exchange may be used toconcentrate and separate solution species based on their charges. It may also be used to determine quantitativelythe concentration of a solution species based on thestoichiometry of the charged species displaced from thesolid phase when the analyte binds to the ion exchanger.Ion-exchange chromatography involves theinteraction of a solid, insoluble phase that containspositively or negatively charged sites (the resin) with amobile phase (eluent solution) that contains the counter ion. The ion-exchange equilibrium can be written as,Cation exchange: B
+(aq) 
+ A
+
Res
-(s) 

A
+(aq)
+ B
+
Res
-(s)
 Anion exchange: X
-(aq)
+ Res
+
Y
-(s)

Y
-(aq)
+ Res
+
X
-(s)
One of the most common ion-exchange resin usedis copolymer of styrene and 4-12%divinylbenzene whichhas been sulfonated (acidified) to produce a strong-acidcation exchanger or aminated (basified) to give a strong-base anion exchanger.This experiment aims to determine the equivalentweight of the salt. In the experiment, the resin would bebasified with a strong base, 4 M sodium hydroxide. Theresin would become a strong anion exchanger. Once thesalt solution, which is the mobile phase, is passed throughthe column, it would exchange anion with resin, which isthe stationary phase. The salt is converted to a base. Theliberated OH
-
present in the eluent can now be titrated witha strong acid.
V. Methodology and Materials
In a beaker, 0.50-0.51 g of the salt was dissolvedwith enough distilled water. It was transferred in a 250-mLvolumetric flask and diluted to mark. A buret was used as glass column. The bottom of the buret was plugged with cotton. The column waspacked with enough resin to fill 10 in of the column. Theresin was regenerated using 50 mL of 4 M sodiumhydroxide at a flow rate of 3 mL/min. Afterwards, all thetraces of OH
-
was washed off the resin with distilled water added in 10 mL portions at a flow rate of 6 mL/min. To testthe completeness of washing, the last 10 mL of washingwas added with 1 drop of standard HCl and 3 dropsphenolphthalein. The color of the resulting mixture must beidentical with the color of 10 mL distilled water with 1 dropstandard HCl and 3 drops phenolphthalein. The standardHCl was prepared by diluting 8.62 mL of concentrated HClto 1 L. It was titrated against primary standard gradesodium carbonate.Ten milliliters (10 mL) of the salt solution waspipetted and passed through the column. Immediately, thiswas followed bwith 100 mL distilled water. The last 10 mLof washing was tested as described above.The eluent and washing was titrated with standardHCl using methyl red indicator. This was done thrice. Fromthe data gathered, the equivalent weight of the salt wascalculated.
VI. ResultsVII. Discussion
Chem 27.1. Spectrophotometric Determination of Stoichiometry of a ComplexPage
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