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Introduction

Flame atomic absorption spectroscopy is categorized as the simplest type of analysis.


It is most widely used technique for detect metals present in samples. Generally, the technique
is based on the principle of absorption light at a specific wavelength by the ground state metals
or non-excited atoms in the vapor state. Metal ions in a solution are converted to atomic state
by means of a flame. Hence, the amount of light absorbed is measured and reading can be
obtained when light of the correct wavelength is supplied. It is very accurate quantitative
technique and also a good qualitative technique.

During AAS analysation, aqueous sample is sprayed into a flame in order to dissociate
the sample into ground state atoms. This process is called as sample atomization where the
aqueous solvent is evaporated. Light with a characteristic wavelength of the analyte is then
radiated at the flame to ensure the analyte atoms absorb electromagnetic energy. The
absorbance is directly proportional to the concentration of analyte atoms in the sample.
Qualitative analysis can be done by determining the presence of analytes in a sample.
Quantitative analysis can be proceed by determining the actual amount of analytes present in a
sample. This analysation can be accomplished via calibration of the AAS using standard
solutions containing known amounts of analytes required. AAS used hollow-cathode lamp
which is very effective as source of radiation.

In this experiment, we used flame atomic absorption spectrophotometer to examine the


trace amount of Fe and Zn in dry cat food. Zn is needed for pet’s body’s immune system to
functioning well and acquired for their senses of smell and taste. While for Fe, pets also
need iron to make haemoglobin which involves in a transportation of oxygen to the body. In
order to decompose the organic constituents and solubilize the metal ions, the smple of pet food
were ‘wet ashed”. The objectives of this experiment are
DATA AND RESULTS

Calibration Curve for Zn


0.25

0.2

y = 0.2367x
Absorbance

0.15 R² = 1

0.1

0.05

0
0 0.2 0.4 0.6 0.8 1 1.2
Concentration (mg/L)

Graph 1.0: Calibration Curve of Zn Standard Solutions.

Calibration Curve for Fe


0.18

0.16 y = 0.0311x
R² = 1
0.14

0.12
Absorbance

0.1

0.08

0.06

0.04

0.02

0
0 1 2 3 4 5 6
Concentration (mg/L)

Graph 2.0: Calibration Curve of Fe Standard Solutions


Table 2.0 : Table shows the reading of concentration and absorbance for standard solution of Zinc

Standard Solution Concentration of Concentration of Zn Absorbance


Standard Solution (mg/L)

0.00 0.000 0.0000

0.25 0.258 0.0611


Zinc 0.50 0.494 0.1169

1.00 1.001 0.2369

Table 3.0: Table shows the reading of concentration and absorbance for standard solution of Ferum.

Standard Solution Concentration of Concentration of Fe Absorbance


Standard Solution (mg/L)

0.00 0.000 0.0000

0.25 1.308 0.0407


Ferum 0.50 2.561 0.0796

1.00 4.953 0.1540

Table 4.0: Table shows the concentration of Zn and Fe in sample

Analyte Mean Concentration (mg/L)


Zn 0.231
Fe 0.184

Table 5.0 : Table shows the data for Zinc in sample, food packaging and percentage error.

Data Value
Concentration of Zinc in pet food sample (mg/L) 0.231
Labeled Value of Zinc stated at the food packaging 150
(mg/kg)
Percentage Error (%)
DISCUSSION

In this experiment, we used Flame Atomic Absorption Spectroscopy (FAAS) in order


to determine the concentration of Fe and Zn ions in a dry cat food. In order to decompose the
organic constituents and solubilize the metal ions in the pet food samples, ‘wet ashed’ method
were applied on the 2g of dried pet food sample with HNO3 solution. Before analyzing the
sample, standard solution must be prepared first for Fe and Zn where the concentration of
standard solution are 0, 0.25, 0.50 and 1.00 ppm respectively. Standard solutions were prepared
by diluting references solutions into 100 ml volumetric flask and 10 ml of HNO3 was added
before diluting to the mark with DI water. Standard solution are solutions that consists of
known and precise concentration of substance or analyte. Hence, in order to determine the
unknown concentration of Zn and Fe in sample, standard solution is a compulsory as it used to
assist in identifying and determining their concentration.

In addition, blank solution also was prepared by the same method as sample preparation
by mixing DI water and 10% of HNO3. The usage of blank solution is essential in FAAS as it
calibrate the FAAS. FAAS need to be calibrated against a blank solution which the blank
solution’s absorbance will construct zero reference for next measurement after
it.(……………). In the other hand, the purpose of using HNO3 as solvent during the sample
preparation and standard solution to reduce the pH2. This can be accomplished as acidic
environment in the solution which is below ph2 lessen the occurrence of precipitation and
adsorption to container wall. Hno3 is highly preferable to be use as solvent compared to other
acid due to its oxidizing characteristic. Metal ions in the solutions become particularly more
soluble as they are in the state of their nitrate salts which converted by HNO3. Next, before
analyzation process in FAAS, sample digestion method is vital to prevent matrix affect which
will interfere during atomization. Matrix can be defined as components of a sample other than
the analyte. This interference which known as matrix effect may lead ionization suppression
which will negatively affect the measurement of analyte concentration. ( ……………..)

Based on the Diagram 1.0, FAAS’s main components of the system are ………………..
Hollow cathode lamp function as spectrum emitter towards specific element of which it is
made. Therefore, hollow cathode lamp must contain the element being determined. The
spectrum is focused through the sample cell into the monochromator. Then, the nebulizer
converts the sample solution into a mist or aerosol by absorbing the liquid sample and mixed
thoroughly with fuel and oxidant. The nebulized sample is then carried into the flame. In the
flame, sample atomization is occurred where the sample is being evaporated at a very high
temperature. The light source is passes through the flam into the monochromator.
Monochromator acts as an isolator where it isolates the analytical lines photons passing through
the flame. Scattered light of other wavelengths are removed from the flame by monochromator.
The light is then measured by a photomultiplier tube which is detector. Lastly, the signal is
then processed and the output is printed on the screen.(…………)

Based on Graph 1.0 and Graph 2.0, both are calibration curve constructed from running
Zn and Fe standard solution under the same condition as the sample. Generally, calibration
curve was used to determine the unknown concentration of Zn and Fe in dried pet food sample.
From the calibration curve, it was observed that the slope for the Zn and Fe Standard solutions
are 0.2367 and 0.0311 respectively. Both graph depicts line with R2=1. However, we directly
obtained the concentration of Zn and Fe as a result from the FAAS analysis. Based on the Table
4.0, the mean concentration of Zn and Fe in the sample are 0.231 and 0.184 mg/L respectively.
The concentration is calculated based on the Beer-Lambert Law. Therefore, we can conclude
that the absorbance is directly proportional to the concentration of the analyte absorbed.

The mean concentration of Zn in sample which is 0.231 mg/L was compared with the
standard labeled value of zinc stated at the food packaging which is 150 mg/kg. The mean
concentration of Zn in sample should be converted first into mg/kg which is 11.55 mg/kg.
Therefore, the comparison of both values can be proceed by calculating the percentage error.
The percentage error obtained is 92.3% which is very high. The reason of huge differences in
concentration of both values due to the ……………………..

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