ANALYSIS OF Na and K IN WATER BY FLAME PHOTOMETRY

Analytical flame spectroscopy is a simple, rapid and versatile physical technique of

quantitative and qualitative chemical analysis. The method is now well established in
chemical analysis and has found a wide spread application, usually metallic elements in
solution. The solution is nebulized into a flame where the solvent and solute are vaporized
and decomposed. An atom is composed of a nucleus and orbiting electrons. The size and
shape of the orbital in which the electron travel is fixed, only certain permitted shapes and
sizes being possible. These are described mathematically by the quantum theory.
When solutions are aspirated into the flame, the solvent evaporates and the remaining
compounds are decomposed to atoms of very simple molecules by absorption of thermal
energy. The electronic transition may then absorb additional energy and undergo electronic
transition to various excited states. These excited states are unstable, so the atoms quickly
emit radiation energy and return to low energy state. The measurement of this emitted
radiation is the basis of flame photometry (alternatively) titled “Flame Emission
Spectroscopy” (FES).
The most useful application of flame photometry, for several reasons, is for the detection
and determination of elements in group I and II of the periodic table (Na+, K+, Rb+, Cs+,
Ca2+, Ba2+). These atoms have low excitation energies and are thus determined with this
method. Furthermore, analysis of these elements in trace amounts by non-flame methods
are among the most difficult and tedious of all the elements. The observation of radiation of
the characteristic wavelength is indicative of the presence of the metal in the sample.
The concentration of metal in the sample can be calculated either from a calibration plot of
emission intensity against concentration or by standard addition method. The former, being
simpler is the most commonly used.
Flame emission spectrometry complements Atomic Absorption Spectroscopy (AAS) because
it operates most effectively for elements, which are easily ionized whilst AAS method
demand a minimum of ionization. Detection limits for Flame Emission techniques are
comparable to those for AAS i.e., <0.001 – 10ppm.
Oral rehydration salts are oral powders containing either anhydrous glucose or glucose,
sodium chloride, potassium chloride and sodium citrate or sodium bicarbonate. After being
dissolved in the requisite volume of water, they are intended for the prevention and
treatment of dehydration due to diarrhoea, including maintenance therapy.

Requirements
Flame photometer, analytical balance, water samples, filter paper (whatman no. 42) and
volumetric flasks
PROCEDURE
a. Preparation of standard stock solution of sodium and potassium
Prepare 40ppm sodium and 100ppm potassium solution:
- Dissolve 0.02542g of NaCl (dry) and 0.04775g of KCl in 250cm3 volumetric flask using
distilled water.
– use the dilution equation to prepare 10ppm KCl in 100mls volumetric flask.

b. Working solutions
a. By suitable dilutions of the stock solution (40ppm), prepare a series of working standards
containing 5, 10, 20 and 40ppm of sodium. The minimum volume of each solution required
is 50 cm3.
b. By suitable dilutions of the stock solution (10ppm), prepare a series of working standards
containing 2, 4, 6, 8 and 10ppm of Potassium. The minimum volume of each solution
required is 50 cm3.

Preparation of calibration curve

Determine the calibration curve for sodium using the direct intensity method. Use deionised
(or distilled water) and the strongest standard solution to adjust the scale reading to zero
and 100 divisions respectively. Without changing the instrument controls determine the
emission readings for the standard solutions.

Q1. Draw a graph of emission readings vs concentration (ppm) of sodium and Potassium.
Q2. Using the calibration curve prepared, determine the concentration in ppm for the water
samples provided. Be sure to aspirate deionised or distilled water into the instrument at the
termination of the measurements. This prevents blockage of the aspirator when the
instrument is not in use.