FACULTY OF APPLIED SCIENCE

BACHELOR OF SCIENCE (HONS) ENVIRONMENTAL

TECHNOLOGY

COURSE CODE: CHM571

EXPERIMENT 5: ATOMIC ABSORPTION SPECTROMETRY.

SEMESTER: 2

STUDENT NAME: NIK NURNIESHA ARDDINA BT NIK ISMAIL.

MATRIC ID: 2022663878

GROUP: AS2292A1

SUBMISSION TO: DR. NORAINI KASIM

TITLES MARKS
INTRODUCTION
OBJECTIVE
METHOD
RESULT
DATA/CALCULATION
DISCUSSION
CONCLUSION
REFERENCES
Total:

EXPERIMENT DATE: 5 APRIL 2023 SUBMISSION DATE: 2 JULY 2023

INTRODUCTION
An analysis technique called atomic absorption spectrometry (AAS) uses light
absorption to estimate the content of trace metals in various samples. Nowadays, the method
is employed all over the world and is a crucial analytical tool in numerous industries. AAS is
employed in the medical field for the analysis of blood and soft tissues as well as in the
development and manufacturing of medications. AAS is also very important for the analysis
of metal traces in water.

AAS serves as an atomization process. AAS measures the concentration of gas-phase

atoms by measuring the amount of light that is absorbed. Since samples tend to be solids or
liquids, it is necessary to vaporise the analyte atoms or ions in a flame or graphite furnace.
For these energy transitions, the amount of radiation energy absorbed by a ground-state atom
in a flame is measured using an instrument called an AAS. The atomic absorption apparatus
uses a hollow cathode lamp as its light source, and in this case, calcium serves as the metal
being analysed for the cathode. This experiment uses Electrodeless Discharge Lamp (EDL) as
a source to measure element concentration. For this experiment, standard calibration curve
and standard addition method were used to evaluate the concentration of calcium in tap
water.

OBJECTIVE
1. To determine the concentration of calcium in a tap water using a standard calibration
curve and standard addition method.

METHOD

For Part I, which is the Calibration Curve Method, a series of standard solutions of the
following concentrations were prepared from standard 100 ppm stock solutions: 2, 4, 6, 8 and
10 ppm. Then, an empty water (deionized water) was run before solution measurements were
made. Next, absorption of standard solution series; 2, 4, 6, 8, 10 ppm were measured. The
absorption of an unknown calcium solution was measured. Then, tap water absorption was
measured. After that, absorption ratio of 1: 1 (tap water: distilled water) was measured.
Lastly, the calibration curve (Absorption versus standard calcium concentration) was plotted
and the calcium concentration in an unknown calcium solution, tap water, 1: 1 tap water to
distilled water ratio was determined.

For Part II, the Standard Addition Method. Firstly, 5 mL of an unknown calcium
solution was transferred into six 100 mL volumetric flasks. The flask for a series of solutions
were prepared and labelled for standard addition methods. Next, a standard calcium solution
(100 ppm) was added by 0, 2, 4, 6, 8, 10 mL in each of the six volumetric flasks at number 1,
respectively. Then, each of the six volumetric flasks was filled with distilled water to the
mark. After that, the absorption of the solution series for the standard addition method was
measured. Lastly, the concentration of calcium in an unknown calcium solution has been
determined.
RESULTS
DATA/CALCULATION

PRE LAB
Preparation of standard solution:

C1V1 = C2V2

Concentration, ppm Volume needed, mL

0 0

2 2

4 4

6 6

8 8

10 10

A. Standard calibration curve:

Calcium in standard solution (ppm) Absorbance

Blank 0.0000

2 0.2169

4 0.3350

6 0.4359

8 0.5390

10 0.6337

1:1 (tap water: deionized water) 0.3671

Tap water 0.6820

Table 1: Absorbance of Ca in standard solution
 Absorbance (A) VS standard concentration
(ppm)
0.7 0.6337
tap =water
f(x) :
0.0683554545454545 x
0.6 0.6820 0.539
ABSORBANCE, A

0.5 0.4359
0.4 0.335
1:1 = 0.3671
0.3 0.2169
0.2
0.1 5.1174 ppm
10.1223 ppm
0
0
0 2 4 6 8 10 12

STANDARD CONCENTRATION (PPM)

Standard calibration curve graph

B Standard addition method:

Flask Concentration of standard Volume of standard Id Absorbance

(ppm) added (mL)

1 0 0 X+0 0.4297

2 1 1 X+2 0.6038

3 2 2 X+4 0.6898

4 3 3 X+6 0.7849

5 4 4 X+8 0.8595

6 5 5 X + 10 0.9407
Table 2: Absorbance of Ca in addition of unknown
 Absorbance (A) VS standard concentration (ppm)
1 0.9407
0.8595
0.9 f(x) = 0.0488171428571429 x + 0.473980952380952
0.7849
0.8 R² = 0.975276062140085
0.6898 (5, 0.9407)
ABSORBANCE, A

0.7 0.6038
0.6
0.4297
0.5
0.4
0.3
(0, 0.4)
0.2
0.1
0
0 2 4 6 8 10 12
1 2 3 4 x 5 6
STANDARD CONCENTRATION (PPM)

Standard addition method graph

B. Standard addition method derives from Beer’s Law:

y = mx+c
y = 0.0488x+0.474 Cx = b C standard
m Vx
= (0.474)(100ppm)
(0.0488) (5ml)
Cx = 194.2623ppm
Cx = concentration unknown
b = pathlength (y-intercept)
m = gradient
Vx = volume unknown (5 ml)
C standard = 100ppm
Find Cx

1 mL standard added: Cx = (0.474) (1) / (0.0488) (5)

= 1.9426 ppm

2 mL standard added: Cx = (0.474) (2) / (0.0488) (5)

= 3.8852 ppm

3 mL standard added: Cx = (0.474) (3) / (0.0488) (5)

= 5.8279 ppm

4 mL standard added: Cx = (0.474) (4) / (0.0488) (5)

= 7.7705 ppm

5 mL standard added: Cx = (0.474) (5) / (0.0488) (5)

=9.7131 ppm
DISCUSSION

In this experiment, a straight line without a cross y-axis is displayed on the graph
using the standard calibration curve method. Deionized water (1:1 v/v) has a calcium content
of 5.1174 ppm, whereas tap water has a calcium concentration of 10.1223 ppm. The
calibration curve approach was used to extract the data from the graph. Compared to other
types of water, tap water has the highest quantity of calcium. It is due to the fact that tap
water is not pure, meaning it contains a lot of minerals. Calcium and magnesium are the two
minerals that are most frequently found in "hard" water. The level of hardness rises together
with the calcium concentration in water. This is the main reason why tap water has the
highest concentration of calcium compared to others when determined by using the
calibration curve method.

The graph pattern for the standard addition method is also a straight line, but it crosses
the y-axis at 0.40. It's because the solution contains elements of the unknowable. It is possible
to compute the concentration of unknown added, which is 194.2623ppm. In the standard
addition method, the concentration of the unknown rises as the volume of standard added
rises; hence, absorbance rises as well. It is as a result of Beer's Law, which states that the
absorbance is directly proportionate to the concentration. The amount of light that interacts
with molecules determines how much of it is absorbed.

A few mistakes could be made during the carrying out of this experiment, producing
an unreliable outcome. Take into account the mistake of misreading the pipette mark when
creating standard solutions. To ensure an accurate transfer of solution volume, the eye should
be perpendicular to the pipette mark. The following error was dropping the solution while it
was being diluted. An excessive drop of solution could skew the reading. Another potential
source of mistake in this experiment is leaching or absorption by the container material. To
reduce mistake, be sure to calibrate and clean the glasses properly beforehand. Last but not
least, before doing the experiment, make sure to cover the volumetric flask with the stopper
and swirl it thoroughly. In addition to obtaining accurate results, it is to prevent
contamination and leaking out of the solution.
CONCLUSION

In a nutshell the atomic absorption spectrometry experiment was successfully

completed and the experiment's objectives, which were to use standard addition methods and
standard calibration curves methods to determine the amount of calcium in an unknown
calcium solution, were also met. Using the calibration curve method, these tests have also
successfully estimated the calcium concentration in tap water and 1: 1 (tap water: distilled
water). It has been demonstrated that the calibration curve method produces results with a
higher concentration than the standard addition method. Additionally, it can be concluded
that as the concentration increased, the absorbance increased proportion to the Beer’s Law.
Therefore, this theory is accepted.

REFERENCES

Angino, E. (2019). Atomic Absorption Spectrometry in Geology. (2nd ed.).

ELSEVIER PUBLISHING COMPANY.

Raja, P. M. V., & Barron, A. R. (2022, August 29). Introduction to Atomic Absorption
Spectroscopy. Rice University. https://chem.libretexts.org/@go/page/55813

BASIC INSTRUMENTAL ANALYSIS CHM571 LABORATORY MANUAL. (JULY-OCTOBER 2007). SHAH

ALAM: UNIVERSITI TEKNOLOGI MARA FAKULTI SAINS GUNAAN SHAH ALAM.