CHM 260

BASIC INSTRUMENTAL ANALYSIS

LABORATORY SUMMARY WRITTEN

REPORT

EXPERIMENT 4
Flame Atomic Absorption Spectroscopy
(AAS)

Name: WAN ARINA SYAKIRAH BINTI WAN RUSLI

ID No.: 2019260774
Programme: CHM 260
Instructor: MADAM SITI NOR HAYATI BT MOHD TARMIZI
 EXPERIMENT 4
Flame Atomic Absorption Spectroscopy (AAS)

A. Pre-laboratory questions

a) Explain how you will dilute a 100ppm stock solution to the following concentration in a
50 mL flask. Show complete working calculation.
1 ppm, 3 ppm, 5 ppm, 7 ppm and 9 ppm

M 1 V 1= M 2 V 2
1 ppm

(100 ppm) ( V 1) =( 1 ppm ) (50 mL )

V 1=0.5mL

3 ppm
( 100 ppm ) ( V 1 )=( 3 ppm )( 50 mL )
V 1=1.5 mL

5 ppm

( 100 ppm ) ( V 1 )=( 5 ppm )( 50 mL )

V 1=2.5 mL

7 ppm
(100 ppm)(V ¿¿ 1)=(7 ppm)(50 mL) ¿
V 1=3.5 mL

9 ppm

(100 ppm)(V ¿¿ 1)=( 9 ppm)(50 mL) ¿

V 1=4.5 mL

Each of 0.5mL, 1.5mL, 2.5mL, 3.5mL, 4.5mL of 100 ppm stock solutions need to pipette and
dilute with distilled water into a 50 mL volumetric flask then close the volumetric flask with
a stopper and shake the flask upside down to make the solution homogenous.

b) Sketch and label the following graph. Indicate and explain how you can determine the
concentration of an unknown from the graph.
i. The standard calibration curve absorbance vs. concentration of the standard
 Determine the unknown concentration by reading the corresponding absorbance from the
graph.

ii. The standard addition method of absorbance against the concentration of the standard
solution.

Where the x value is at the x-intercept, a linear regression line is produced. The unknown
sample's concentration can be determined. The absolute value will be taken.

From these two graphs, we can use this formula to find unknown concentration,

bC std
CX=
mV x
b = y-intercept
m = gradient
V x =Volume of unknown solution
C std =concentration of standard
C x =concentrationunknwon

B. Post laboratory questions

Solutions Concentration (ppm) Absorbance

Standard 1 1.5 x 10-3 0.215
Standard 2 3.2 x 10 -3
0.445
Standard 3 4.4 x 10-3 0.599
Standard 4 6.3 x 10-3 0.856
Standard 5 8.2 x 10 -3
1.252
a) Using any available software, plot a standard calibration curve of absorbance versus
concentration of Ca standard solution.
 Graph Absorbance Versus Concentration of Ca
(ppm)
1.4 1.252
1.2
f(x) = 151.49189426026 x − 0.041641740908427
1 R² = 0.988357254589605 0.856
Absorbance 0.8
0.599
0.6 0.445
0.4 0.215
0.2
0
1.00E-03 2.00E-03 3.00E-03 4.00E-03 5.00E-03 6.00E-03 7.00E-03 8.00E-03 9.00E-03
Concentration (ppm)

b) In a standard addition method, you will prepare a series of solutions to add different
increments of standard solutions to fixed aliquots of unknown sample X (10.0 mL). All
solutions were prepared using a 50 mL volumetric flask. Suppose that the analysis of the
standard solution of X gave the following results:

Graph of Absorbance Versus Concentration (ppm)

0.6 0.554
f(x) = 0.0361065573770492 x + 0.2022 0.467
0.5
R² = 0.999934296300495 0.378
0.4
Absorbance

0.292
0.3
0.201
0.2
0.1
0
-8 -6 -4 -2 0 2 4 6 8 10 12
Concentration (ppm)

Solutions Concentration (ppm) Absorbance

Standard 1 0.00 0.201
Standard 2 2.44 0.292
Standard 3 4.88 0.378
Standard 4 7.32 0.467
Standard 5 9.76 0.554

Based on the slope above, we can determine concentration of the X. Based on the equation
above: (m = slope of the graph, c = intersect on y-axis at x = 0.000.)
y=mx+c
y=0.0361 x +0.2022
Hence, the slope is the concentration of X and from the data the slope is 0.0361. So, the
concentration of X is 0.0361 ppm.
 C. Complete the table of added volume and concentration of the diluted standard
Solution The volume of added standard, The concentration of added standard,
mL ppm
1 0.024 1.0
2 0.042 2.0
3 0.064 3.0
4 0.082 4.0
5 0.098 5.0

D. Report summary (1-2 pages)

a) INTRODUCTION
The technique of atomic absorption spectrometry (AAS) is used to quantify the number of
chemical elements present in environmental samples by measuring the absorbed radiation by
the chemical composition of interest. When a sample is stimulated by radiation, the spectra
produced are read. As a result of absorbing ultraviolet or visible light, the atoms migrate to
higher energy levels. The quantity of energy absorbed by the sample in the form of photons
of light is measured using atomic absorption methods. In the 18th century, John Dalton
proposed the notion of atoms, saying that all atoms of a given element are identical and that
atoms with various qualities might combine to form molecules. Niels Bohr revolutionised
atomic theory in 1913 when he proposed the Bohr model of the atom, which included
quantum numbers, a positively charged nucleus, and electrons orbiting around the nucleus.
Louis deBroglie postulated the quantized energy of electrons shortly after, which is crucial in
AAS. DeBroglie's hypothesis was then expanded upon by Wolfgang Pauli, who said that no
two electrons might have the same four quantum numbers. Understanding the process of
AAS necessitates these seminal atomic theory breakthroughs. Selectivity is important in AAS
since each element has its own set of energy levels. This results in relatively narrow
absorption lines. As a result, choosing the right monochromator is vital. To create a linear
calibration curve (Beers' Law), the absorbing species' bandwidth must be greater than the
light source's, which is difficult to do with typical monochromators. Because it is used to
separate the thousands of lines created by all elements in a sample, the monochromator is a
critical component of an AA spectrometer. Lastly, atomic absorption spectroscopy (AAS) has
a wide range of applications because of its specificity. Biological analysis, environmental and
marine analysis and geological analysis are the three broad categories.

b) METHODOLOGY
Part A is preparation of standard solutions. 5.00 mL of 1000 ppm stock solution was pipetted
and transferred to 50.0 mL volumetric flask then diluted with deionized water until the mark.
The solution was labelled as ‘100 ppm’. A series of standard solutions having 1 ppm, 3 ppm,
5 ppm, 7 ppm and 9 ppm was prepared by using the 100 ppm solution and a 50 mL
volumetric flask. The unknown solution was obtained. The absorbance of the standard
solution in step 2 was measured, followed by the unknown. Part B is operation of atomic
absorption spectroscopy (AAS). The Cu lamp was switched on. The burner was aligned. The
acetylene, air valve and oxidant were opened. The flame was ignited. Part C is measurement
of atomic absorbance. The blank was aspirated and run. The standard was aspirated and
analysed (the correlation value should be better than 0.999). The sample was aspirated and
analysed. Part D is shutting down procedures. The water was aspirated to clean the burner.
The flame and all the oxidant’s sources were switched off. last but not least, the AAS
instrument was switched off.
c) ANALYSIS

Graph Absorbance Versus Concentration of Ca

(ppm)
1.4 1.252
1.2
f(x) = 151.49189426026 x − 0.041641740908427
1 R² = 0.988357254589605 0.856
Absorbance

0.8
0.599
0.6 0.445
0.4 0.215
0.2
0
1.00E-03 2.00E-03 3.00E-03 4.00E-03 5.00E-03 6.00E-03 7.00E-03 8.00E-03 9.00E-03
Concentration (ppm)

Atomic absorption spectrometry, like other analytical techniques, necessitates precise

calibration. Beer's law states that the absorbance of an absorbing analyte is proportional to its
concentration, which is the idealised calibration or standard curve. Based on the graph
absorbance versus concentration above, we can say that when we increase the concentration
of solution, the amount of absorbance will be increased.
d) CONCLUSION
From this experiment, we were abled to know how to operate a flame AAS instrument. We
also abled to plot a standard calibration curve for determination of Ca in the sample. Atomic
Absorption Spectroscopy (AAS) has the advantages of being simple to use and less expensive
than other forms of high precision spectroscopy. AAS has the advantage of having lower
sensitivity than other spectroscopy, allowing for the study of smaller samples between 5-
60μL, whereas other spectroscopy requires samples in the range of 1-3 mL. The limitation of
AAS is it can only be used for quantitative element analysis, whereas atomic emission and
atomic fluorescence are both quantitative and qualitative instruments. The AAS method, on
the other hand, is a technique for determining the concentrations of metallic elements in
various materials. As an analytical tool, it employs electromagnetic wavelengths emitted by a
light source. These wavelengths will be absorbed by the elements in different ways. To
achieve the optimum atomic absorption results, the system's instrumental and chemical
parameters must be optimised for the formation of neutral ground state atoms of the element
of interest.
REFERENCES
 García, R., & Báez, A. P. (2012). Atomic absorption spectrometry (AAS). Atomic absorption
spectroscopy, 1, 1-13.
 K.G.K. (2016, April 19). Advantages and Disadvantages of Atomic Absorption
Spectrometry and Graphite Furnace. Chemistry Net. Retrieved January 2, 2022, from
http://chem-net.blogspot.com/2013/12/advantages-disadvantages-atomic-absorption-
graphite-furnace.html
 Libretexts. (2021, March 21). 1.4: Introduction to Atomic Absorption Spectroscopy.
Chemistry LibreTexts. Retrieved December 31, 2021, from
https://chem.libretexts.org/Bookshelves/Analytical_Chemistry/Physical_Methods_in_
Chemistry_and_Nano_Science_(Barron)/01%3A_Elemental_Analysis/
1.04%3A_Introduction_to_Atomic_Absorption_Spectroscopy