Michael C.

Guinita

BS Chem-3

10-11-14

ANALYSIS OF A PLANT MATERIAL BY ATOMIC ABSORPTION

SPECTROSCOPY
Introduction
Atomic absorption spectroscopy (AAS) is one of the most widely used techniques in
instrumental analysis. It is used to determine the concentrations of analyte elements, usually
metals, which come at very low or trace amounts, such as Pb, Ni, among others. Flame atomic
absorption spectroscopy (FAAS) is a technique where the analyte solution is turned into gaseous
atoms by passing it to a flame and then analyzed by spectroscopy using radiation coming from a
lamp made out of the metal to be analyzed (i.e. when Pb is analyzed, a Pb lamp is used).
In this experiment, lead in Cyperus alterniforus L. (umbrella plant) from a known source
is analyzed via AAS to be able to determine the amount of lead present in every part of the plant
(i.e. leaves, stem, roots).
Methodology
A. Materials and instrumentation: Cyperus alterniforus L. taken from the back of the
basketball court in the University of San Carlos, Cebu City; concentrated nitric acid; dilute
nitric acid; standard lead solution (1000 ppm); Shimadzu atomic absorption spectrometer
B. Sample preparation. Samples were air dried for three weeks, heated in an oven at about
105C and then pulverized.
C. Digestion of samples. An accurately weighed plant sample was moistened with a few drops
of water, added with concentrated nitric acid and evaporated to moist salts. The residue
was diluted in 2 mL nitric acid and diluted quantitatively to 50 mL in a volumetric flask.
D. Determination of Pb by external calibration method. The following standards were
prepared for the calibration curve: 0.2 ppm, 0.4 ppm, 0.8 ppm, 1.0 ppm and 1.2 ppm. Each
standard was run to the instrument to obtain their individual absorbances. A plot of
absorbance versus concentration was generated. The plant sample was then analyzed. In a
separate 25-mL volumetric flask, a portion of the unknown was added with 0.8 ppm Pb
and then diluted to the mark. This solution was also analyzed.
E. Moisture. One gram of accurately weighed plant sample was placed in a pre-weighed
empty crucible. The mass of the crucible with the plant was recorded. The crucible was
heated at 105C for one hour. Once the crucible had cooled, it was weighed again.

Results and Discussion

A. Preparation of the calibration curve. The equation of the line from the calibration curve is
y = 0.026411x 0.00041310; R2 = 0.9993 where x is the concentration of lead while y is
the absorbance.
Concentration
0.0000
0.2000
0.4000
0.8000
1.0000
1.2000
Unknown

Absorbance
-0.0001
0.0043
0.0104
0.0204
0.0266
0.0310
0.0014

Calibration Curve
0.035
y = 0.0264x - 0.0004
R = 0.9987

0.03

Absorbance

0.025
0.02
0.015
0.01
0.005
0
-0.005

0.2

0.4

0.6

0.8

1.2

1.4

Concentration of Pb (ppm)

B. Determination of Pb. The following data were obtained in the determination of lead in the
(1) unknown, (2) unknown + 0.8 ppm Pb, and (3) 0.8 ppm Pb:
1. Unknown
Trial
1
2
3
Average

Absorbance
0.0012
0.0006
0.0014

Concentration
(ppm)
0.0611
0.0384
0.0686
0.0560

Mass of Pb
(g)
3.06x10-6
1.92x10-6
3.43x10-6
2.80x10-6

% Pb
2.53x10-4
1.70x10-4
3.25x10-4
2.49x10-4

2. Unknown + 0.8 ppm Pb

Trial
Absorbance
1
2
3
Average

Concentration (ppm)

Mass of Pb (g)

0.8751
0.8865
0.7956
0.8524

2.188x10-5
2.216x10-5
1.989x10-5
2.131x10-5

0.0227
0.0230
0.0206

3. 0.8 ppm Pb
Absorbance
0.0204

Concentration
0.8000

C. Percent recovery (calculated using % =

2 1
3

100)

Trial
1
2
3
Average

%R
94.1
101.2
82.3
92.5

D. Moisture data (calculated using % =

100)
Trial

Mass of
empty
crucible (g)

1
2

31.2417
37.2616

Mass of Pb (g)
2.000x10-5

Mass of
crucible +
sample
before
heating (g)
32.2425
38.2670

Mass of
crucible +
sample after
heating (g)

Mass of
sample (g)

% moisture

32.1255
38.1478

1.0008
1.0054

11.69
11.86

E. Corrected percent lead after taking % moisture into account (using the formula
%

%
100

100%

Original % Pb
2.49x10-4

Corrected % Pb
2.20x10-4

Conclusion
The lower detection limit of the instrument is 0.004 absorbance units, and the readings
from the unknown are less than the LDL, which makes the entire determination invalid. Since the
readings are below detection limit, it can be concluded that the amount of lead absorbed by the
plant sample from the soil was planted was minimal.