Instrumental Analytical Methods

Lab Report 2013

Anastazija Ristovska
Experiment 1
Flame Photometric Analysis

The purpose of this experiment was to determine the concentrations of sodium and potassium
ions in solution through flame-photometric analysis. When excited in flame i.e. at the high temperature of
the flame, potassium and sodium elements emit light at a few characteristic and specific wavelengths
unique for these two elements. The intensity of the light emitted, i.e. the number of photons emitted by
each element at the particular wavelength is the basis for determining the concentration of potassium and
sodium in solution. As the name of the technique suggests, flame photometric analysis counts the number
of photons emitted per unit time and at one particular wavelength from the flame in which a solution
containing potassium and sodium ions is dispersed in aerosol spray form. The instrument does this by
utilizing photon-sensors and photomultipliers. This simple concept is the basis for designing complex
instruments that function on the same photometric idea such as atomic emission spectroscopy.

sodium

potassium

Flame
photometer
reading (FLM)

Sodium
concentration
(g/ml)

Flame photometer
reading (FLM)

Potassium
concentration
(g/ml)

76,9

20

78,8

20

61,7

16

81,7

16

45

12

69,2

12

35

43,2

21,8

25,5

We were given 6 solutions of unknown concentration, and, using the linear fit for the FLM
readings of the solutions of known concentration, we were supposed to find, or calculate to best
approximation, the concentration of sodium and potassium of these 6 solutions.
The first solution contained sodium only. It had a reading of 23.9 FLM. Using the equation of
the first plot y=0,2901x-1,9504, where y is the solution concentration and x is the FLM reading, [Na+] in
this solution was calculated to be 4,983 g/ml, or almost 5 g/ml.
The fifth solution contained potassium only. The flame-photometer reading of it was 25.1 FLM.
Using the equation of the second plot, y = 0,2438x - 2,5481, where y is the solution concentration and x
is the FLM reading, [K+] in this solution was found to be 3,571 g/ml, or almost 3,6 g/ml.

The composition and reading of all solutions, and their calculated concentrations are given in this table:
# Composition
1 Na+
2 Na+ + K+
3
4
5
6

Na+

K+

+
+
Na + K+
K+
K+

Na+ FML Reading

23.9
31.4

K+ FLM Reading
n/a
27.8

[Na+] (g/ml)
4,983
7.159

[K+] (g/ml)
n/a

4.230

Approx. (g/ml)
[Na+]=5
[Na+]=7, [K+]=4

24.8
27.1
n/a
n/a

47.1
38.2
25.1
33.0

5.244
5.911
n/a
n/a

8.935
6.765
3,571
5.497

[Na+]=5, [K+]=9
[Na+]=6, [K+]=7
[K+]=3.5
[K+]=5.5

We were able to determine the concentration of sodium and potassium in a mixture with a high
enough precision and accuracy as if they were not in a mixture but in two separate solutions by
themselves.
We did not use a blind sample in this experiment. Blind samples are often used to control for the
quality of emission analysis. In our experiment we only wanted to determine the concentration of samples
with known composition and identity. The purpose of a blind sample is to determine the identity of the
solutes through emission analysis. Even though it is possible to do this for alkaline metals as they give of
characteristic emission colors in the flame-photometer, yellow for sodium and purple for potassium, it
would had been hard to determine with accuracy what the elements are in a mixture of sodium and
potassium where the colors were blurred. Although originally an old technique for qualitative
identification of select metallic elements, we did not use blind samples with flame-photometry in our
experiment.
The instrument displayed greater sensitivity in measuring the concentration of sodium than that
of potassium. In the case of potassium the model we obtained explained for 88.4% of the variance in the
system, whereas the model for determining sodium concentration through linear fit explained for 99.3%
of the variance in system. Because it was able to more accurately detect and describe the concentration of
sodium than that of potassium, we say that the instrument was more sensitive in measuring the
concentration of sodium.

sodium concentration (micrograms per ml)

25
y = 0,2901x - 1,9504
R = 0,993
20

15
Series1
10

Linear Fit

0
0

20

40

60

80

100

FLM reading

potassium concentration (micrograms per ml)

25
y = 0,2438x - 2,5481
R = 0,8843

20

15
Series1
10

Linear (Series1)

20

40

60

80

100

Axis Title