University of Bahrain

College of Science
Department of Chemistry

Experiment 5
Determination of Selected
Metals

Name : Mua'az Ahmed Taha

Academic Number : 20073459
Course Number : CHEMY 310
Submission Date : 2010-4-1

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 Index

Page
o Objective……………..………………….3
o Abstract…………………………………..3
o Theory………………………………….3
o Requirements……………………………3
o Results……………………….…………..5
o Conclusions and Recommendations.....6
o References……………………………….6

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Objective:
-

Abstract:

Theory:
A class of spectroscopic methods in which the species examined in the spectrometer are in the
form of ATOMS (not molecules or ions as in solution spectrophotometry &
spectrofluorimetry). It is used widely for quantitative determined of trace metals, in different
sample: alloys, rocks, soils, foodstuffs, drinks, etc.

Three important methods based on spectroscopy of atomic species are:

1. Flame Emission Photometry (FEP)
2. Atomic Absorption Spectrophotometry (AAS)
3. Inductively Coupled Plasma Atomic Emission Spectrometry (ICPAES).

Only 2 will be considered in this subject. The atoms measured are most commonly
those of mineral elements such as Na, K, Mg, Cu, Fe, Ni, etc.

Atomic Absorption Spectrophotometry (AAS) Principle:

FEP limited (for most purposes) to Na & K. With non-alkali metals most atoms remain in the
ground state at normal flame temperature ---> no emission. AAS measurement is based on the
ground state atoms; has much wider applicability than FEP. Flame can be used as in FEP to
reduce & decompose ions/molecules in solution to atoms in flame. Then measure conc. of
GROUND STATE atoms by spectrophotometric principle - absorption of light from a beam
passing through flame. Use elongated burner - flame light path ~10cm - to enhance absorption.

Fig.1 - Atomic Absorption Spectrophotometer

Hollow Cathode Lamp:

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Absorption in the flame is by vapor phase atoms, giving line spectra (see 7.2), in this case
absorption lines. A continuous spectrum light source, even with high quality monochromatic
cannot achieve sufficiently narrow band pass width for absorption line spectra. Use special
lamps, each emitting line spectrum matched to the line spectrum of the analyte atoms in the
flame. The type of lamp is a hollow cathode lamp.

Fig.2 - Hollow Cathode Lamp

Different lamp for each analyte element, but some multi-element lamps available:

- At high voltage, ions of He or Ar gas form at anode and bombard cathode.

SPUTTERING occurs - atoms dislodged from the surface and produce an atomic cloud.
Some sputtered atoms are in excited state and emit their characteristic line spectrum as
they revert to the ground state. 

- Cylindrical shape of the cathode gives direction to emerging beam, and helps re-
deposit sputtered atoms back on cathode. 

- Monochromatic isolates particular spectral line & eliminates stray radiation e.g.
emissions from inert gas in lamp.

- Modulation of light beam upstream of flame (by rotating chopper) allows detector to
reject emission generated within flame.

Requirements:
- Volumetric Flasks.
- Pipettes.
- Measuring Cylinders.
- Funnels.

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Data Collected:
Sample No. Concentration (ppm) Volume ( ml) Absorbance
1 1 5 0.008
2 2 10 0.0255
3 3 15 0.0452
4 4 20 0.0397
Unknown No.2 Is to be calculated - 0.0241

Sample No. Concentration (ppm) Volume ( ml) Absorbance

1 50 25 100
2 40 20 96
3 30 15 91
4 20 10 83
5 10 5 70
Unknown No.2 Is to be calculated - 67

Sample Theoretical Reading Experimental

mg/L Reading
High Land 6 67
Al Qaseem 22.4 90
Al-Aein 8 69

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Results:

Concentration Vs Absorbance
0.05
0.05 f(x) = 0.01 x + 0
0.04 R² = 0.8
0.04
Concentration Vs
Absorbance

0.03
Absorbance
0.03
Linear (Concentration Vs
0.02 Absorbance)
0.02
0.01
0.01
0
0.5 1 1.5 2 2.5 3 3.5 4 4.5
Concentration ppm

Figure 1. Absorbance vs. Concentration (ppm)

Concentration Vs Absorbance
120

100
f(x) = − 0 x³ + 0.04 x² − 0.61 x + 82
80 R² = 1
Absorbance

Concentration Vs Absorbance
60 Polynomial (Concentration Vs
Absorbance)
40

20

0
5 10 15 20 25 30 35 40 45 50 55
Concentration Na+ ppm

Figure 2.Absorbance vs.Na Concentration (ppm)

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From fig.1 ;

y = 0.018x - 0.011

Unknown No.2 absorbance is equal to 0.0241 , then by substituting in the above

equation , the concentration will be " solving for x " :

x = 1.95 ppm .

From fig.2 ;

y = -0.0005x3 + 0.0443x2-0.6071x+82

Unknown No.2 absorbance reading is equal to 67 , then by substituting in the above

equation , the concentration will be " solving for x " :

x= 77.96 ppm "using calculator solver"

For Aspirin :

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Summary :
Aspirin Caffeine
Wave 273 nm 300 nm 273 nm 300 nm
Length
Slope 2450 135 613 1030

Analysis for unknown mixture :

For λ = 273 nm ,
A1 = ε1c1(aspirin) + ε2c2(caffeine)
1.156 =2450C1 + 135C2 -(1)
For λ = 300 nm ,
A2 = ε’1c1(aspirin) + ε’2c2(caffeine)
0.573 =613C1 + 1030C2 –(2)

Then by solving equations (1) and (2) , simultaneously ;

C1 = 4.56 x 10-4 M aspirin (mol/L)---(MM = 180 g/mol)

----C1=0.08208 M(g/mol)
C2 = 2.85 x 10-4 M .

Conclusion and Recommendation:

References:
1- http://en.wikipedia.org/wiki/titration

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 2- SKOOG/WEST/HOLLER, Fundamentals Of Analytical Chemistry,
Saunders HBJ , 6th Edition, 1992.