OBJECTIVE

1. To determine the concentration of Iron and Cadmium in Water spinach plant tissue by
using AAS
2. To determine the weight and weight percent of Iron and Cadmium that present in the Water
plant tissue.

ABSTRACT
The experiment conducted is to find if there is a present of Iron and Cadmium in plant tissue.
The sample was undergoes acid digestion to convert it to solution for the instrument use. The
AAS was used in order to determine the concentration of Iron and Cadmium in the water
spinach. At the end, the result will be compared between both of the instruments.
INTRODUCTION
Atomic Absorption spectroscopy (AAS) is the technique for determine the composition
elemental of an analyte by its electromagnetic or mass spectrum. This technique can be used to
analyze concentration of over 62 different metals in a solution. Atomic Absorption happens when
a ground state atom absorbed light radiation at a specific wavelength and is transferred to an
excited state. The amount of light energy absorbed at specific wavelength increase as the number
of atoms of the selected element in the light path increases. There are 5 important basic
components in AAS which are the light sources, the atomizer, the monochromator, the detector
and readout. The light source use in AAS is Hollow Cathode Lamp (HCL), which have specific
light. It provided light energy for excitation. The atomizer is the flame itself. In this component,
the liquid sample is converted into a mist by a process called nebulization. The samples will be
sent to flame for atomization to occur. The process of atomization cause the metal in sample to
atomized and undergoes a transition from ground state to excited state by absorbing the light
from HCL. The emitted light from will pass to monochromator. The monochromator will select
the desired wavelength, so that the desired light passes through the monochromator and eliminate

all insignificant light. The detector, Photomultiplier Tube (PMT) will detect the light and the
readout will read and convert the signal into readable result.
Acid digestion method is a procedure to convert the sample into solution so that it can be
introduced to the AAS. Acid digestion method is carried out by using Nitric acid (HNO 3) and
also hydrogen peroxide (H2O2). The sample will be dissolve in nitric acid with the help of high
temperature. Then, the hydrogen peroxide is added to aid the oxidation properties of nitric acid.
Iron (Fe) and Cadmium (Cd) is a transition metal. These two metals is considered as a trace
metal because it is expected to have a low amount of concentration in the samples. Iron (Fe), is
good to human as it help the formation of haemoglobin in our blood, maintaining body
temperature, and increase the brain function. The deficits of Iron in body cause anaemia,
insomnia and problem with enzyme system. On the other hand, Cadmium serves a bad reputation
to human health. Cadmium poisoning is one of the bad effects of cadmium introduction to
human body. Moreover, Cadmium also causes kidney damage, fragile bones, vomiting and even
the worst, death to the person who consumed it.
EXPERIMENTAL PROCEDURE
A) SAMPLE PREPARATION

The vegetable was cut and put dried in and oven of 110C for 4 hours. The dried vegetables were
cut into pieces. About 3 grams of vegetable was weighed and placed in 250 ml beaker. 20-30 ml
of nitric acid (HNO3) was added into the beaker and was allowed to stand Overnight. The sample
was heated until red fume came out. Then it was cooled.1 ml of peroxide (H2O2) was added into
the cooled sample. The sample was reheated till concentrate. It was then filtered into 250ml
volumetric flask. The sample was diluted with distilled water and transferred into bottles

B) PREPARATION OF STANDARD
1. PREPARATION OF 10 PPM OF STANDARD SOLUTION FOR AAS AND
5 mL of 100 ppm stock solution of Iron / Cadmium was pipette into 50 mL volumetric flask by
using pipette. The volumetric flask was filled with distilled water until the calibration mark. The
volumetric flask contained solutions were labeled as 10 ppm Fe3+/ Cd2+.

2. PREPARATION SERIES OF STANDARD SOLUTION FOR AAS

2.1

CADMIUM SERIES STANDARD

Standard series of Cadmium range from 0 ppm, 0.2 ppm, 0.4 ppm, 0.6 ppm, 0.8
ppm and 1.0 ppm were made by using standard addition method. 0 mL, 1.0 mL,
2.0 mL, 3.0 mL, 4.0 mL and 5.0 mL of 10 ppm Cadmium standard were pipetted
and transfer into 50 mL of each volumetric flask. 10 mL of Water samples were
added into each volumetric flask contained standard series. All of the volumetric
flasks were then diluted with distilled water until the calibration mark.

2.2

IRON SERIES STANDARD

Standard series of Iron range from 0 ppm, 1.0 ppm, 1.5 ppm, 2.0 ppm, 2.5 ppm
and 3.0 ppm were made by using standard addition method. 0 mL, 5.0 mL, 7.5
mL, 10.0 mL, 12.5 mL and 15.0 mL of 10 ppm of Iron standard were pipetted and
transfer into 50 mL of each volumetric flask. 10 mL of Water spinach samples
were added into each volumetric flask contained standard series. All of the
volumetric flasks were then diluted with distilled water until the calibration mark.

RESULT

CONCENTRATION
IRON
CADMIUM
Blank
Blank
1
0.2
1.5
0.4
2
0.6
2.5
0.8
3
1

ABSORBANCE(y1 )
IRON
CADMIUM
0.092
0.070
0.137
0.107
0.161
0.143
0.182
0.182
0.201
0.218
0.223
0.249

VOLUME(x1 )
IRON
CADMIUM
0
0
5 ml
1 ml
7.5 ml
2 ml
10 ml
3 ml
12.5 ml
4 ml
15 ml
5 ml

Calculation:
Least square method:
CONCENTRATI
ON
Fe
Cd
Blank
Blank
1
0.2
1.5
0.4
2
0.6
2.5
0.8
3
1

IRON

ABSORBANCE
(y1)
Fe
Cd
0.092
0.070
0.137
0.107
0.161
0.143
0.182
0.182
0.201
0.218
0.223
0.249
y=
y=
0.996
0.969

VOLUME (x1)
Fe
0
5 ml
7.5 ml
10 ml
12.5 ml
15 ml

Cd
0
1 ml
2 ml
3 ml
4 ml
5 ml

= 50

= 15

X1X1
Fe
0
25
56.25
100
156.25
225
xx=
562.5

Cd
0
1
4
9
16
25
xx= 55

X1Y1
Fe
0
0.685
1.2075
1.82
2.5125
3.345
xy= 9.57

Cd
0
0.107
0.286
0.546
0.872
1.235
xy=
3.056

iron
0.25
f(x) = 0.02x + 0.12
R = 1

0.2
0.15

Linear ()

0.1
0.05
0
0.5

xy = ((xy) -

=9.57 -

1.5

( x)( y)
N

( 50 ) (0.996)
6

= 1.27
xx = (xx)

= 562.5
= 145.83

m=

xy
xx

2.5

( x )2
N
(50)2
6

3.5

4.5

5.5

1.27
55145.83

= 0.0087

c=

y 1 m( x 1)

N
N

0.996 0.0087 (50)

6
6

=0.0935
Concentration of Chromium in plant tissue:
C=

(V s)( b)
( Vt ) ( m)

(10 ) (0.0935)

= ( 10 ) (0.0087)
= 10.75 ppm

CADMIUM

cadmium
0.3
0.25

f(x) = 0.04x + 0.07

R = 1

0.2

Linear ()

0.15
0.1
0.05
0
0.5

1.5

2.5

xy = ((xy) -

( x)( y)
N

=3.056-

( 15 ) (0.969)
6

= 0.6335
xx = (xx)

= 55
= 17.5

( x ) 2
N
(15)2
6

3.5

4.5

5.5

 xy
xx

m=

0.6335
17.5

= 0.0362

c=

y 1 m( x 1)

N
N

0.969 0.0362(15)

6
6

= 0.071
Concentration of cadmium in plant tissue
(V s)( b)
( Vt ) ( m)

C=

( 10 ) (0.071)
(10)(0.0362)

=1.96 ppm

Percent weight of iron:

0.001 gram per litre = 1 ppm
=10.75 x 0.001
= 0.01075
Percent of iron =

mass of ironthe sample

x 100
mass of sample

0.01075
x 100
=
2.0
= 0.5375 %

Percent weight of cadmium:

0.001 gram per litre = 1 ppm
=1.969 x 0.001
= 0.00196
Percent of cadmium =

0.00196
x 100
2.0

= 0.098 %

mass of ironthe sample

x 100
mass of sample

DISCUSSION
In this experiment, we used wet digestion methods for sample preparation. It is for
elemental analysis that involves the chemical degradation of sample matrices in solution, usually
with a combination of acids to increase solubility as it has been done on day 2 and allow to stand
overnight. The various acid and ux treatments are carry out at high temperatures in specially
designed vessels that help to minimize contamination of the sample with substances in the air,
the local environment, and from the vessel walls. Sample may be loss due to adsorption onto the
vessel walls, volatilization, and coextraction, but these can be reduced by procedural
modications. The use of closed systems, where the digestion reaction is completely isolated
from the surroundings, may help to reduce both contamination and sample loss. For this
experiment, the sample was covered with aluminium foil.
Standard addition methods are particularly useful for analyzing complex samples in
which the likelihood of matrix effects is substantial. A standard addition method can take several
forms. One of the most common forms is spiking method as we had use it in preparing standard.
Each solution was diluted to marked point before measuring or analyzing it.
The least square method is a typical calibration graph where I have plotted in calculation
area for both sample chromium and cadmium respectively. The sample was injected into the
atomic absorption spectroscopy and the result was obtained. Absorbance versus volume graph
was plotted and the linear equation and R 2 was calculated in Microsoft excel and as well as
manually which had been shown.

For analysis using Flame AAS, the concentration of Iron (Fe) and Cadmium (Cd) can be
determined by measuring the absorbance. The samples was undergoes standard addition method.
10 mL of water sample is added into each standard. The purpose of standard addition method is
to eliminate matrix interference. Other than that, it is used widely for the trace element detection
as trace element is present in low concentration. From the experiment, the Iron and Cadmium
concentration are

ppm and

ppm respectively.

CONCLUSION
The amount of concentration of iron and cadmium can be determined by using AAS and ICPOES. From the experiment, the amount of Iron and Cadmium by using AAS is 10.75 ppm and
1.75 ppm respectively.
REFERENCE
Cadmium.org (n.d). Cadmium exposure and human health. Retrieved at 22nd December 2014
from http://www.cadmium.org/pg_n.php?id_menu=5
Ingle, J.D. Jr., Crouch, S.R., (1988). Spectrochemical analysis. Englewood Cliffs, New Jersey:
Prentice-Hall, Inc.
Krisha McCoy, MS. (2014). Cadmium Toxicity. Retrieved at 22nd December 2014 from
http://medicine.med.nyu.edu/conditions-we-treat/conditions/cadmium-toxicity#risk
Organicfacts.net (n.d). Health benefits of Iron. Retrieved at 22nd December 2014 from
https://www.organicfacts.net/health-benefits/minerals/health-benefits-of-iron.html

Skoog, D.A., West, D.M., Holler, F.J., & Crouch, S.R. (2004). Fundamental of analytical
chemistry. (8th ed.), Belmont, CA: Brooks/Cole Cengage Learning.

Skoog, D. A., Holler, F. J., & Nieman, T. A. (1998). Principles of instrumental analysis.
Philadelphia: Saunders College Pub.

QUESTION
1. Briefly explain other method of digestion that is available for sample treatment in atomic
absorption or atomic emission spectroscopy
- Sample preparation can be performed by simple dilution or heating for pre-concentration or
partial or total dissolution. However to achieve most sample preparation, it is necessary to add
reagent to the sample and to apply enough energy to break some bond and the structure of solids.

2. Explain what are standard addition method and the purpose of this method
- The standard addition method is the method to determine the concentration where by the
sample was added together with the standard.

3. Briefly discuss why different hollow cathode lamps (HCL) were used for different element
and how cathode lamp works.
- The cathode is a hollowed out cylinder constructed entirely or in part of metal whose spectrum
is to be produced. The anode and cathode are sealed in a glass cylinder filled with noon or argon.
The glass cylinder has a quartz or uv glass window for optimum transmittance of emitted
radiation.

TITLE OF EXPERIMENT: DETERMINATION OF IRON AND CADMIUM IN PLANT

TISSUE BY ACID DIGESTION METHOD USING ATOMIC
ABSORPTION SPECTROMETRY (AAS)
COURSE

: AS245

COURSE CODE

: CHM580

NO OF EXPERIMENT

: 4

NAME:

MAXVICKLYE RAYNER ABID (2014586975)

LECTURERS NAME

DATE REPORT SUBMISSION

: 31 MARCH 2016

GROUP

: AS2454D1