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ANALYTICAL CHEMISTRY

(CLD 10402)

Atomic Absorption Spectroscopy

Determination of Cooper (Cu) in AAS

PREPARED BY:

NAME: MUHAMMAD FADHIL BIN ABU BAKAR

ID NUMBER: 55103208065

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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 Beer’s 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
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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;

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M V = M V
1 1 2 2

Where;

M = Initial concentration in ppm


1

V = Initial volume in ml (volume of solution required)


1

M = Final concentration in ppm


2

V = Final volume in ml (volume of volumetric flask


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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.

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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

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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:-

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The calculation is using this formula:-
M 1V1 = M 2V2

Stock Diluted
Concent
Concentration Volume of Cooper ration of
of Cooper (ml) Cooper Volumetric
(ppm) (ppm) flask (ml)
M1 V1 M2 V2

0.5(100)
1 100 V1 = = 0.5 0.5 100
100
1.0(100)
2 100 V1 = = 1.0 1.0 100
100
1.5(100)
3 100 V1 = = 1.5 1.5 100
100
2.0(100)
4 100 V1 = = 2.0 2.0 100
100
2.5(100)
5 100 V1 = = 2.5 2.5 100
100

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INSTRUMENT PARAMETERS:-

Blank solution 0.000


Standard solution concentration (ppm) Absorbance (mean)
0.5 0.006
1.0 0.010
1.5 0.016
2.0 0.021
2.5 0.025
Unknown 1 0.040
Unknown 2 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 Diluted
Concentr Volume
Concentration Volume of Cooper ation of of
of Cooper (ml) Cooper Cooper
(ppm) (ppm) (ml)
M1 V1 M2 V2

0.5(100)
100 V1 = = 0.5 0.5 100
100
1.0(100)
100 V1 = = 1.0 1.0 100
100
1.5(100)
100 V1 = = 1.5 1.5 100
100
2.0(100)
100 V1 = = 2.0 2.0 100
100
2.5(100)
100 V1 = = 2.5 2.5 100
100

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The
standard Concentration (ppm) Absorbance
calibration
was shown 0.5 0.006
in the table
below 1.0 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
0.025 2
R = 0.9967
Absorbance

0.02 Series1
0.015
Linear
0.01 (Series1)

0.005

0
0 1 2 3
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


Beer’s-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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