ANALYTICAL CHEMISTRY

(CLD 10402)
Atomic Absorption Spectroscopy
Determination of Cooper (Cu) in AAS
PREPARED BY:
NAME: MUHAMMAD FADHIL BIN ABU BAKAR
ID NUMBER: 55103208065

TITLE: Determination of Cooper (CU) by using of the Atomic

Absorption Spectroscopy.
ABSTRACT:The elemental analysis Atomic Absorption Spectroscopy which is
widely used in analyzing environment, metal, food, pharmaceutical and
chemical industries samples. In this experiment, the Atomic Absorption
Spectroscopy performance (sensitivity) is checked. The amount of
copper in sample standard solution is determined. Firstly, standard
solution of copper is prepared, with acid nitric. Next the instrument is
operated, by optimizing the Burner System and then the Performance
is checked and lastly Calibration curve is created and samples are
analyzed. Then graph of absorbance against concentration was plotted
to show the Beers Lambert Law.

OBJECTIVE:To optimize the burner system by flame atomic

absorption spectroscopy using standard solution.
To check the performance (sensitivity) of the atomic
absorption spectroscopy using standard solution.
To prepare a serial dilution and generate a standard
calibration Curve.
To determine amount of cooper in the sample.
INTRODUCTION:Atomic absorption methods measure the amount of
energy (in the form of photons of light, and thus a
change in the wavelength) absorbed by the sample.
Specifically, a detector measures the wavelengths of
light transmitted by the sample (the "after"
wavelengths),
and
compares
them
to
the
wavelengths, which originally passed through the
sample
(the
"before"
wavelengths).
A
signal
2

processor then integrates the changes in wavelength,

which appear in the readout as peaks of energy
absorption at discrete wavelengths.
The process of atomic absorption spectroscopy (AAS)
involves two steps:
1.
Atomization of the sample
2.
The absorption of radiation from a light source by the free
atoms

Figure below is the schematic diagram of atomic absorption

spectrometer. Hollow cathode lamp will emit the line
spectrum of the element to be analyzed. Samples are then
atomized in the flame. Selection of wavelength of interest
done by the monochromator.

In order to tell how much of a known element is present in a

sample, one must first establish a basis for comparison using
known quantities. It can be done producing a calibration
curve. For this process, a known wavelength is selected, and
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the detector will measure only the energy emitted at that

wavelength. However, as the concentration of the target
atom in the sample increases, absorption will also increase
proportionally. Thus, one runs a series of known
concentrations of some compound, and records the
corresponding degree of absorbance, which is an inverse
percentage of light transmitted. A straight line can then be
drawn between all of the known points. From this line, one
can then extrapolate the concentration of the substance
under investigation from its absorbance. The use of special
light sources and specific wavelength selection allows the
quantitative determination of individual components of a
multi element mixture.
In this experiment, the ideal setup element used is
coopers which have a wavelength at 324.8 nm and
aspiration of solution of 4.0mg/L should produce of 0.200
absorbance.
Characteristic concentration is the concentration of
analyte that gives 1% absorption or 0.0044 absorbance (as
shown in checking the Performance part). Characteristic
concentration is very useful in assessing instrument
performance by showing a low characteristic concentration
value which indicates a higher sensitivity.

AAS EQUIPMENT
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APPARATUS: Perkin Elmer Atomic Absorption Spectrometer model

100 AAnalyst.
Copper hollow cathode lamp.
Eight 100 ml volumetric flask.
Beakers
Pipette (2 ml and 5 ml)
CHEMICAL SUPPLIED: 100 ppm Cooper (Cu) standard solution.
Concentrated nitric acid.

Distilled water.
Caution: Dispose all the chemicals in the proper waste
container.

EXPERIMENTAL PROCEDURES:A. Preparation of cooper standard solution.

1) 10ml of 100ppm Cooper standard solution was

poured into a small beaker and 10ppm Cooper

standard solution been prepared in 100ml
volumetric flask using the following equation;

M V
1

M V

Where;
M

= Initial concentration in ppm

1

= Initial volume in ml (volume of solution required)

1

= Final concentration in ppm

2

= Final volume in ml (volume of volumetric flask

2

used)
2) I% (v/v) of concentration nitric acid (1% = 1ml)

was added into the 100ml volumetric flask and

deionized water was marked up to the volume.
WARNING!!!! Concentrated nitric acid is highly corrosive!!
Please use glove for protection when you are dealing with
the corrosive chemicals!!
3) 2.0 And 4.0 ppm of cooper standard solution is

prepared from freshly prepared 100ppm

standard solution using 100ml volumetric flask.
4) 0.5ppm, 1.0ppm, 1,5ppm, 2.0ppm and 2.5ppm
cooper standard solution was prepared using
100ppm Zinc standard solution. 1% v/v of
concentration nitric acid been added to each of
the standard solution and the volume was
marked up.
5) The standard solution prepared and ready to be
analyzed.

OPERATING THE INSTRUMENT:Please refer to the Appendix Step 1 until 5 and then do the
following order as below;

1. Optimizing the Burner System.

a) A blank solution was prepared.
b) The known standard was aspirated using 8ppm.
c) The burner position been adjusted using the
Horizontal adjustment knob and the
nebulizer adjustment nut until a maximum
absorbance is displayed on the screen.
d) The absorbance of blank was checked and it
should be zero.

2.Checking the Performance.

a) Characteristic Concentration was clicked in

the Analysis menu.

b) The sample concentration and instrument
reading (the maximum absorbance) were
entered.
c) The Tab key been pressed.
d) The Measured Characteristic Concentration
should be within 20% of the Comparison
Characteristic Concentration value.
e) Characteristic Concentration window was
closed. The characteristic concentration
value can also be calculated using the following
equation;
0.0044 X known
conc. Used
Characteristic Conc. Value = Absorbance for known
conc. used

3. Creating a Calibration Curve and Analyzing

Samples.
a. Creating a calibration curve.
i. The nebulizer tube was immersing into
blank solution.
ii. The calibration standard was selected to
analyze from the dropdown list. The
software completes the concentration entry
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according to the value entered in the

method.
iii. Analyze Standard was clicked. This step
been repeated for every calibration
solution; 0.5ppm, 1.0ppm, 1.5ppm, 2.0ppm
and 2.5ppm.
iv. The calibration curve been checked. If any
of the standards appear to be off the
calibration curve, then you may wish to edit
the calibration curve.
a. Analyzing the samples.
i. The nebulizer tube was immersed into
sample solution.
ii. Analyze Samples been clicked.

1.

Shut down the instrument by following step 7 in

the Appendix.

REPORT SHEET:-

The calculation is using this formula:-

M 1V1 = M 2V2

Stock
Concentration
of Cooper
(ppm)

Volume of Cooper
(ml)

M1

V1

Diluted
Concent
ration of
Cooper Volumetric
(ppm)
flask (ml)
M2

V2

100

V1 =

0.5(100)
= 0.5
100

0.5

100

100

V1 =

1.0(100)
= 1.0
100

1.0

100

100

V1 =

1.5(100)
= 1.5
100

1.5

100

100

V1 =

2.0(100)
= 2.0
100

2.0

100

100

V1 =

2.5(100)
= 2.5
100

2.5

100

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INSTRUMENT PARAMETERS:Blank solution

Standard solution concentration (ppm)
0.5
1.0
1.5
2.0
2.5
Unknown 1
Unknown 2

0.000
Absorbance (mean)
0.006
0.010
0.016
0.021
0.025
0.040
0.006

Comparison characteristic concentration value (2ppm) =

0.077 mg/L.
Measured characteristic concentration value (2ppm) = 0.303
mg/L
Comparison characteristic concentration value (4ppm) =
0.077 mg/l
Measured characteristic concentration value (4ppm) = 0.352
mg/l
% RSD (mean)
= 0.4472
Correlation coefficient (final) = 0.99786

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DISCUSSION:The amount of sample to be take for serial dilution was

calculated as in the table below

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The experiments were using 5 different concentrations which

are 0.5ppm, 1.0ppm, 1.5 ppm, 2.0 ppm, 2.5 ppm. And the
result is following 0.5 ml/ 0.5 ppm, 1.0 ml/ 1.0ppm, 1.5
ml/1.5 ppm, 2.0 ml/ 2.0 ppm, and 2.5 ml/2.5ppm. The
Atomic Absorption Spectrometer was using the flame
technique which is the sample towards the small tube and
burn with flame to get the absorption of the sample that
tested.

Stock
Concentration
of Cooper
(ppm)

Volume of Cooper
(ml)

M1

V1

Diluted
Concentr Volume
ation of
of
Cooper
Cooper
(ppm)
(ml)
M2

V2

100

V1 =

0.5(100)
= 0.5
100

0.5

100

100

V1 =

1.0(100)
= 1.0
100

1.0

100

100

V1 =

1.5(100)
= 1.5
100

1.5

100

100

V1 =

2.0(100)
= 2.0
100

2.0

100

100

V1 =

2.5(100)
= 2.5
100

2.5

100

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The
standard
Concentration (ppm)
calibration
was shown
0.5
in the table
below
1.0

Absorbance
0.006
0.010

1.5

0.016

2.0

0.021

2.5

0.025

Standard Calibration Graph for the Cooper

0.03
y = 0.0101x + 0.0004
2
R = 0.9967

Absorbance

0.025
0.02

Series1

0.015

Linear
(Series1)

0.01
0.005
0
0

Concentration

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Concentration of Unknown1:
Y=mx+c
0.040 = 0.0101(x) + 0.0004
X= 3.9207ppm
Concentration of Unknown 2:
Y=mx+c
0.006= 0.0101(x) + 0.0004
X= 0.5545ppm

CONCLUSION:As the final result the absorption measurement follow the

Beers-Lambert Law. The absorbance is directly proportional
to the path length and the concentration of atomic vapor in
the flame. From the experiment that had done the result for
volume for the serial dilution are using the formula. The
volumes are calculated from the concentration which is
0.5ml/ 0.5ppm, 1.0ml/ 1.0ppm, 1.5ml/ 1.5ppm,
2.0ml/2.0ppm and 2.5/ 2.5ppm cooper stock.
Wavelength scan are used to determine at what the
wavelength the cooper able to absorb. The result for the
wavelength is 324.8nm. The standard calibration graph was
determining the absorbance towards the concentration
given. From the experiment the R is 0.4472 . Besides, the %
2

RSD (mean) is 0.676 and correlation coefficient (final) is

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0.9978. The concentration of unknown 1 is 3.9207 ppm and

concentration of unknown 2 is 0.5545ppm and it absorbance
is 0.006.

REFERENCE: www.weather.nmsu.edu
www.answer.com
www.wikipidea.com

Raymond Chang., General Chemistry, McGraw-Hill International

Edition, p142 & p507.

APPENDIX:Pre Laboratory Question:

1. What is the function of monochromator?
- Function of monochromator is to isolate analytical lines'
photons passing through the flame. Remove scattered
light of other wavelengths from the flame. In doing this,
only a narrow spectral line impinges on the PMT.

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2. You are given a 100 ppm mercury stock solution. What

is the volume needed in ml to prepare a 15 ppm standard
stock solution in 50 ml volumetric flask?
M1V1 = M2V2
100(V1) = 15(50)
100 V1 = 750
V1 = 7.5 ml.

Volume needed to prepare 15 ppm :

15ml-7.5ml
= 7.5 ml need to add to 100 ppm solution to make
15 ppm solution in 50ml volumetric flask.

3. How would you determine the performance of atomic

absorption spectrometer?
. The measured characteristic concentration should
be within 20% of the
comparison characteristic concentration value or
calculated using the
following equation;

Characteristic = 0.0044 x known conc. used

Conc. Value
Absorbance for known
Conc. used
4. Calculate the characteristic concentration value for
2ppm cooper standard that has absorbance value of 0.194
absorbance.
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Characteristic Con. Value = (0.0044) X (known conc. used)

Absorbance for known
conc.
Used
= (0.0044) X (2 ppm)
0.194
= 0.0454

Post Laboratory Questions

1. Ignator
2. Burner head
3. Nebulizer adjusting nut
4. Vertical adjustment knob
5. Horizontal adjustment knob

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