EXPERIMENT 4

Flame Atomic Absorption Spectroscopy (AAS)

A. Pre-laboratory questions

a) Explain how you'll dilute a 100ppm stock solution in a 50 mL flask to the following concentration.
Display the entire working calculation.
1ppm, 5ppm, and 9ppm
Using formula: M1V1 = M2V2

1 ppm → (100 ppm)(V1) = (1 ppm)(50 mL)

V1 = 0.5 mL

5 ppm → (100 ppm)(V1) = (5 ppm)(50 mL)

V1 = 2.5 mL

10 ppm → (100 ppm)(V1) = (10 ppm)(50 mL)

V1 = 5 mL

0.5 mL, 2.5 mL, and 5 mL of the standard solution, 100 ppm, were pipetted into a
50 mL volumetric flask. The solution was then diluted with deionized water until
it reached the calibration point. The solution was then poured into a beaker and the
process was repeated until 1ppm, 5ppm, and 10ppm of solution remained.
b) The following graph should be sketched and labelled. Explain how you can use the graph to
determine the concentration of an unknown.
i) The standard calibration curve absorbance vs. standard concentration

Absorbance vs Concentration
3

2.5

2
Absorbance

1.5
Absorbance
1

0.5

0
0 0.5 1 1.5 2 2.5 3
Concentration of the standard

ii) \ Absorbance versus the concentration of the standard solution using the standard addition
method.

Absorbance vs Concentration
3
2.5 y = mx+c
R² = 1
2
1.5
Absorbance

1
0.5 Absorbance
0 Linear (Absorbance)
-2 -1 -0.5 0 1 2 3

-1
-1.5
-2
Concentration of the standard solution (ppm)
B. Post-laboratory questions

a) Plot a standard calibration curve of absorbance vs concentration of Ca standard solution using any
accessible software.

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

Absorbance vs Concentration
1.4
1.2
y = 151.49x - 0.0416
1
Absorbance

0.8
0.6
0.4
0.2
0
0.00E+001.00E-032.00E-033.00E-034.00E-035.00E-036.00E-037.00E-038.00E-039.00E-03
Concentration of Ca standard solution (ppm)

Absorbance Linear (Absorbance)

b) You'll build a series of solutions to add varying increments of standard solutions to fixed aliquots
of unknown sample X in a standard addition procedure (10.0 mL). A 50 mL volumetric flask was
used to make all of the solutions. Assume the following outcomes from the study of X's standard
solution:

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

Absorbance
0.6
y = 0.0361x + 0.2022
0.5
R² = 0.9999
0.4
Absorbance

0.3

0.2

0.1

0
-8 -6 -4 -2 0 2 4 6 8 10 12
-0.1
Concentration (ppm)

Absorbance Linear (Absorbance)

Finding the x-intercept, y=0:

0=0.0361x+0.2022
− 𝑖𝑛𝑛 =-5.60

Concentration of unknown
=| - inn |
0.0361x + 0.2022 = 0
X = -5.60
= | −5.60 | = 5.60 ppm
C. Objective

The objective of the experiment is to learn how to operate the flame AAS instrument
and plot a standard calibration curve to determine of Ca in a sample. The amount of
Fe in a sample also determine using the standard calibration curve.

D. Introduction

Atomic absorption spectroscopy (AAS) is a qualitative and quantitative instrument

analytical method for determining distinct elements present in a sample. It may
identify components in liquid or solid phases by using a light source with a specific
wavelength characteristic of the electromagnetic spectrum. Atomic absorption
spectroscopy is a simple and low-cost method for determining the composition of a
solution. Flame AAS has the disadvantage of having a small path length across the
flame and occasionally clogging on the tip. Furthermore, this spectroscopy has a poor
sensitivity and can only be used to analyse solutions. The atoms of an analyte absorb
light, which is the concept behind this approach. A metal-containing solution will be
inhaled as an aerosol and then injected into a hot flame. The solvent will evaporate
later, and the metal will be vaporised as atoms. A liquid sample will be used in this
experiment to determine the presence of ferum in the sample. AAS allows us to
determine the presence of calcium in a sample by measuring the radiation energy
absorbed during the passage of an electron to a higher electronic energy state.

E. Procedure

i. Preparation of Standard Solutions

5.00 mL of 1000 ppm stock solution was pipet and transferred into a 50.00 mL
volumetric flask to dilute it with deionized water until the mark. The solution
was marked as ‘100 ppm’. A series of standard solutions with concentration of
1 ppm, 3 ppm, 5 ppm, 7 ppm, and 9 ppm were prepared together with an
unknown solution using the 100 ppm solution and a 50 mL volumetric flask.

F. Result and Data

Solution The volume of The concentration of added Absorbance

added standard, mL
1 0
2 5
3 10
4 15
5 20
Unknown unknown
standard, ppm
1 0.0006
3 0.0077
5 0.0118
7 0.0225
9 0.0232
3.6 0.0103
 A Graph of Absorbance vs Concentration
0.03

0.025 y = 0.003x - 0.0018

Absorbance R² = 0.9538
0.02

0.015

0.01

0.005

0
0 2 4 6 8 10
Concentration

Absorbance Linear (Absorbance)

Based on the graph, the molar absorptivity is 0.003. The mean absorbance for unknown is
0.023. The sample path length is 1cm. A=εbc
C= A/εb
C= 0.0103/0.003(0.9538)
C= 3.6 ppm

G. Discussion

In this experiment, we will learn how to operate the Flame Absorption Atomic
Spectroscopy apparatus and plot a standard calibration curve using the data collected.
The concentration of the unknown must be determined using the standard calibration
curve graph.

First, we make a few standard solutions and name them 1 ppm, 3 ppm, 5 ppm, 7 ppm,
and 9 ppm using a 50 mL volumetric flask and a 100 ppm standard solution. We plot
a standard calibration and standard addition technique graph after the experiment is
completed to determine the unknown concentration of the drinking water based on the
absorbance and concentration of the standard solution that was used. The goal is to
use Flame Absorption Spectrophotometry to produce a standard addition method for
determining the unknown content of drinking water. We use the standard calibration
curve to determine the concentration using the formula A=εbc. For this method of
determining the concentration, the concentration is 3.6 ppm. As a result, we anticipate
some sort of inaccuracy affecting our final concentration from two different methods.
H. Conclusion

In conclusion, we were able to learn on how to operate the flame AAS instrument and
plot a standard calibration curve to determine of Ca in a sample both before and after
the experiment. The amount of Fe in a sample also determine using the standard
calibration curve.