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Analytical Chemistry Laboratory 2

Determination of Magnesium by Ion-Exchange Chromatography

Mr. *****

Department of Chemical Engineering and Chemistry, Mapua Institute of Technology


November 22, 2005

A charged substance, Magnesium, was separated via column materials (resins and glass
wool) that carry a negative charge. The ionic groups of exchanger columns are covalently bound
to the gel matrix and are compensated by small concentrations of counter ions, which are present
in the buffer. When the unknown sample was added to the column, an ion exchange with the
weakly bound counter ions takes place. The percentage of Magnesium oxide in the sample was
computed to be 66.27% for sample #4.

Objective
ions such as Cl- or OH- accompany the
The purpose of this experiment is to positive sites. If the polymer structure is not
understand the principles of given in detail the anion exchange bead can
chromatographic separations particularly on be shown diagrammatically below:
ion exchange. The main objective is to
determine the concentration of Magnesium
in the sample.

Discussion

Overview

In ion-exchange column
chromatography the stationary phase is
composed of beads of a high molecular In either cation or anion-exchange
weight organic polymer which are closely chromatography, the attraction for the
related to the polystyrene from which coffee stationary phase is simple electrostatic
cups are made. In the beads the long attraction of positive charges for negative
polymer chains have a small percentage of charges, but each different type of cation or
crosslinking via divinyl benzene, and anion has its own affinity for the
contain a large number of either anionic or corresponding resin.
cationic groups which are covalently bound Cations in an aqueous solution are
to the polymer structure. Each of these never monoatomic species but are bonded to
charged sites in the polymer must be water molecules to form Lewis acid-base
accompanied by a small ion of the opposite adducts called "complex ions". In many
charge in order to insure total electrical instances it is possible to replace these water
neutrality. An anion exchange must contain molecules with other electron donating
positive charges. These are usually species, e.g. Cl- or NH3. Collectively these
quaternary ammonium groups where counter electron donating species are referred to as
ligands. If negatively charged ligands are system, causing muscle weakness, fatigue,
used, the positive ions can become neutral or sleepiness, or even hyperexcitability. In
even negative species. extreme states, magnesium overload can
In the experiment, the titrant 0.05 M cause death.
NaOH was standardized with primary-
standard potassium hydrogen phthalate Methodology
(KHP). Magnesium is the element to be
analyzed in the sample. Preparation of ion-exchange columns
Magnesium is a very important A plug of glass wool was inserted to
essential macromineral, even though there retain the resin particles. A sufficient strong-
are only several ounces in the body (0.05 base anion-exchange resin was then
percent of body weight). It is involved in introduced to give a 10- to 15-cm column.
several hundred enzymatic reactions, many The column was washed with about 50 mL
of which contribute to production of energy of 6 M NH3, followed by 100 mL of water
and cardiovascular function. As time goes and 100 mL of 2 M HCl. At the end of this
on, magnesium is recommended and used in cycle, the flow was stopped so that the
more and more treatments. Prevention or liquid level remains about 1 cm above the
treatment of myocardial infarctions (MIs), resin column.
prevention of kidney stones, and in
treatment of premenstrual syndrome are Chromatographic Analysis
some important recent uses. Magnesium has The number of tablets in the sample
been used with some success in relieving was recorded. The tablet was then
certain kinds of angina and reducing the transferred to a clean 500 mL volumetric
risks of coronary artery spasms, which can flask. They were dissolved in a minimum
lead to angina or, more severely, heart volume of 3 M HCl. Then it was diluted to
attack. Deficient magnesium levels have the mark with distilled water. The free acid
been found in the blood and hearts of was titrated in several 15-mL aliquots of the
cardiac victims. Besides preventing heart dissolved sample; phenolphthalein was used
attacks, magnesium has a mild effect on as an indicator. The column was conditioned
lowering blood pressure and so is used to with about 15 mL of 3 M HCl, followed by
treat and prevent hypertension and its three 15-mL portions of distilled water.
effects. Magnesium supplementation can Each column was charged with a 15-mL
reduce many of the symptoms of mitral aliquot of the sample. It was eluted of about
valve prolapse, such as palpitations or 2 to 3 mL/min. The column was washed
arrhythmias, and it may help in other cardiac with three 15-mL portions of water. The
arrythmias such as atrial tachycardia or elute and washings were collected in a
fibrillation, or those caused by taking excess conical flask. The eluted samples (and
digitalis, a cardiac drug. It may also reduce washings) were titrated with standard base.
the bronchoconstriction in asthma by The total volume that needed to titrate the
relaxing the muscle around the bronchial free acid was corrected.
tubes. Intravenous solutions containing
magnesium and other nutrients have been Instrumentation
used successfully to break acute asthma
attacks.
Toxicity due to magnesium overload
is almost unknown in a nutritional context,
as excesses are usually eliminated in the
urine and feces. However, symptoms of
magnesium toxicity can occur more likely if
calcium intake is low. These symptoms may
include depression of the central nervous
2. Skoog, D. A., and Leary, J. J., Principles
of Instrumental Analysis, 4th edition,
Saunders, New York 1992.

3. Harris, D.C., Quantitative Chemical


Analysis, 3rd edition, Freeman, New York,
1991.

The column contains resins which is 4. © 1993-2003 Microsoft Corporation. All


a quaternary ammonium ion. Beneath the rights reserved.
resins contains a glass wool to retain the
resin particles.

Interpretation

This experiment requires the weight


of a certain mass of the unknown salt, which
is 1.0019 g dissolved in a solvent, and
passed over a column of ion-exchange resin.
As mentioned previously, this process
serves the purpose of converting the salt into
its corresponding acid, MgCl., would all be
transformed to HCl. Once the salt has been
converted, the acid solution which is a result
of this procedure is titrated using a
standardized solution (KHP) of sodium
hydroxide. With the information obtained
from the titration, you can MgOH in the
unknown sample
mmol H+ = 2x mmol Mg2+
The percentage of concentration computed
was approximately 66.72%.

Conclusion

Ion exchange chromatography uses


an ion exchange resin as the stationary phase
and the sample as the mobile phase. The
mechanism of separation is based on ion
exchange equilibria. The Magnesium cation
in the sample was exchanged with the anion
resin. Due to this process MgO content in
the unknown can be computed.

References

1. Christian, G.D., Analytical Chemistry, 6th


edition, New Jersey, John Wiley, 2004.