Chemical Analysis & Evaluation

Flame Atomic Spectroscopy

(Experiment 4)
Dr Jorge Chacon
Azeem Khan; B00230817
Group 2: Donya Jafari & Maroobah Abbas

Aim
The aim of this experiment is to demonstrate the application of atomic
spectroscopy. In addition to this, to show that atomic emission spectroscopy can
be used for analytical determination for certain elements. Furthermore, to
illustrate and identify the problems of a sample matrix and effective solution to
the problems identified.

Introduction
Atomic spectroscopy is a widely used and sensitive technique to determine
metallic elements that may exist in a particular sample. Atomic spectroscopy is
originated upon measuring the absorption of electromagnetic radiation by atoms
in their elementary state (e.g. K+).
In this particular experiment, the analytical technique used is flame atomic
spectroscopy. This consists of a lamp made of sodium (cathode) with a supply of
8 milliamps. In addition to this, a burner supplying acetylene and oxygen (air)
burns at 2300oC, above the atomisation of the element (sodium). It is vital the
temperature is above the atomisation of the respective element, otherwise the
element will not atomise. Furthermore, a beam of light is fired across, which is in
line with the burner. The sample gets drawn up and sprayed into the burner. Any
water that exists boils away, and the resultant element, in this case sodium is
left. Finally, the light then hits the sodium and the absorption is determined by
the detector.

Equipment

Various sizes
of volumetric
flasks and
pipettes
Flame atomic

spectrophotometer

Method
Part 1

250cm3 of 10ppm sodium solution is prepared from a 1000ppm solution of

sodium. The resulting solution is diluted to 250 cm 3 in a volumetric flask.
Using the 10ppm sodium solution made above, 100 cm 3 of the following
solutions are made: (in ppm) 0.2, 0.4, 0.6, 0.8, 1.0, 1.2, 1.6, 2.0 and 3.0.
These solutions made are analysed by an atomic absorption
spectrophotometer. To set the instrument up, in order to zero the
instrument, it is to be sprayed with demineralised water.
Once the instrument is set up, the absorbance of tap water is determined.
Then the absorbance of each solution made up in the second bullet point is
analysed 3 times whilst spraying demineralised water between each
solution.
The absorbance of tap water is determined a further two times.
The appropriate data i.e. the absorbance readings, is written on the lab
proforma.

Part 2

The instrument used is adjusted so that it is able to read the solutions in

the atomic emission mode.
The ppm standards made up in in part 1 are to be used again for part 2.

Similarly from part 1, the emissions of tap water is determined. Then the
emissions of each solution made up in part 1 are to be analysed 3 times
whilst spraying demineralised water between each solution.
The appropriate data i.e. the absorbance readings, is written on the lab
proforma.

Part 3

100 cm3 of 50ppm iron solution is made by dilution from 500ppm iron
solution.
Two solutions of iron of 2 and 4ppm are prepared by dilution with
deionised water of the 50ppm iron stock solution into a 25 cm 3
volumetric flask.
Three 25 cm3 volumetric flasks, labelled A, B and C, are to contain 10
cm3 of the given irn bru solution.
Into flask A, 1 cm 3 of the 50ppm of the iron stock solution is added. Into
flask B, 2 cm3 of the 50ppm of the iron stock solution is added. Nothing
is added in flask C. All three flasks are made up to the 25cm 3 mark with
deionised water.
The instrument is set up to read the iron absorption line. The
instrument is zeroed using deionised water, as previously.
The absorbance for all five standards are analysed. Flask A, B and C are
repeated 3 times.
The appropriate data i.e. the absorbance readings, is written on the lab
proforma.

Calculations
For part 1, when preparing the 250cm3 of 10ppm sodium solution from a
1000ppm solution of sodium, the equation M 1V1=M2V2 was used.
V2 =

(250 x 10)
1000

= 2.5cm3; of 1000ppm sodium is required to make a 10 ppm

sodium solution up to 250cm3. (The rest of which is made up with deionised

water)
The same approach is used when preparing 100cm 3 solutions of 0.2, 0.4, 0.6, 0.8,
1.0, 1.2, 1.6, 2.0 and 3.0 (in ppm). As previously, the equation M 1V1=M2V2 is used.
For part 3, a similar method as described above is used to prepare 100 cm 3 of
50ppm iron solution from 500ppm iron solution. Again, the equation M 1V1=M2V2 is
used.
V2 =

(50 x 10)
500

= 10cm3; of 500ppm iron solution is required to make a 50ppm

iron solution up to 100cm3. (The rest of which is made up with deionised water)

For the atomic absorbance unknown. To determine the concentration, the

absorbance is analysed from the spectrophotometer. The reading is the
absorbance. Once a plot of the absorbance against concentration (ppm) is
obtained, the equation of a line y = mx + c can be used.
This gives a value for m and c, the absorbance reading is y. Rearranging this
equation to x gives;

x=

yc
m

where x = concentration. The dilution factor is 10

so the whole equation is to be multiplied by 10.

From the plot, y = 0.163x + 0.015. For reading 1; x =

(0.0810.015)
0.163

x 10 =

4.049 ppm
The same equation is used for the rest of the 4 readings. In addition to this, the
same method is also used for the atomic emission unknown. Where the equation
of the line is; y = 0.558x + 0.004.
To calculate the iron content in irn bru, a plot of absorbance against
concentration is to be obtained.
The equation of the line is; y = 0.006x + 0.008.
The Iron content in Irn Bru can be determined in two ways:
By extrapolating the slope of the graph back to the x axis.
Or alternatively, the equation; y = mx + c, can be used. Where x is the iron
content in irn bru, and y= 0.
Y = 0.006x + 0.008
Y = 0, so x =

c
m

0.008
0.006

= 1.33 ppm.

However, the dilution factor is 2.5. So, the iron content in irn bru
= 1.33 x 2.5 `
= 3.325 ppm.

Discussion

When determining the absorbance of the various range of solutions, the

method was repeated three times and an average of the three results is
taken. The reason for this is to make sure the absorbance reading from the
instrument is accurate and precise.

The difference between accuracy and precision is; Accuracy means getting
a result that is close to the real result. Precision means getting the same
result every time you try.

For the limits of calibration, the main cause of the loss of linearity at a high
concentration is because, for sodium. The atom is hugely excited, so much
that it causes it to self-absorb, lowering the content of Na + atoms.

The lower limits of the techniques used are determined by the sensitivity
of the instruments.

Out of the two spectroscopic techniques used (Atomic Absorption and

Atomic Emission) In terms of precision; Atomic Emission is more precise
and is better suited for an easily exited atom such as sodium.

Conclusion
To conclude this experiment, the metallic content of a range of samples were
analytically determined successfully. This illustrates the application of atomic
spectroscopy and why one may use such a technique. In this particular
experiment, the iron content in irn bru was determined which may be of
significance to a health and safety consultant. In addition, to an environmentalist
or farmer, this technique can be used to detect the richness of soil by the
detection of metallic minerals. Furthermore, in the same way, a chemical
engineer may want to detect the metallic content of a solution that is fed into a
reactor. Finally, with support from the calculations, this experiment is successful
and fulfilling to the original aim.

Please
turn over
Figures & Graphs
FLAME ATOMIC ABSORPTION
PART 1
SODIUM IN POTABLE WATER
SODIUM CONCENTRATION (PPM)
0
0.2
0.4
0.6
0.8
1
1.2
1.6
2
3

ABSORBANCE
0
0.053
0.091
0.121
0.15
0.174
0.205
0.276
0.337
0.508

Sodium in Potable Water Calibration Plot

0.6
0.5

f(x) = 0.16x + 0.02

R = 1

0.4
Absorbance

0.3
0.2
0.1
0
0

0.5

1.5

2.5

Sodium Concentration (ppm)

PART 2
SODIUM - FLAME EMISSION
SODIUM CONCENTRATION (PPM)
0
0.2
0.4
0.6
0.8
1

EMISSION
0
0.107
0.216
0.325
0.438
0.562

3.5

Sodium Flame E
0.6

f(x) = 0
R = 1

0.5
0.4
Absorbance

0.3
0.2
0.1
0
0

PART 3
IRON IN IRN BRU
IRON CONCENTRATION (PPM)
2
4

ABSORBANCE
0.026
0.027

0.

Iron in Irn Br
0.03
0.03
0.03
0.03
0.03
Absorbance 0.03
0.03
0.03
0.03
0.03
1.5

ATOMIC ABSORPTION UNKNOWN

1
z2
3
4
5
MEAN ABSORBANCE
STD. DEV

ABSORBANCE
0.081
0.081
0.082
0.082
0.08
0.0812
0.00083666

ATOMIC EMISSION UNKNOWN

1

ABSORBANCE
0.316

2
3
4
5
MEAN ABSORBANCE
STD. DEV

IRN BRU
0
2
4

0.314
0.311
0.32
0.318
0.3158
0.00349285

ABSORBANCE
0.008
0.022
0.035

ABS
0.04
0.04
0.03
0.03
Absorbance

0.02
0.02
0.01
0.01
0
0

0.5