GROUP THREE(3).

HEAVY METAL ANALYSIS.

Heavy metal analysis is a crucial method for the detection and quantification of
potentially harmful elements in various samples, such as soil, water, air, food, and biological
tissues. The presence of heavy metals in these samples can pose serious health risks to both
humans and the environment, making accurate analysis essential.

In order to perform heavy metal analysis, a range of sophisticated instrumentation is

required. These instruments are capable of detecting and quantifying even trace amounts of
heavy metals in samples, ensuring precise and reliable results. Some commonly used instruments
for heavy metal analysis include atomic absorption spectrometry (AAS), graphite furnace (GF-
AAS), and cold vapor (CV-AAS).

Each of these instruments offers unique advantages and capabilities for heavy metal
analysis, allowing researchers and analysts to tailor their methods to the specific needs of their
samples.

ATOMIC ABSORPTION SPECTROMETER.

Atomic Absorption Spectroscopy (AAS) is a powerful analytical technique used to

determine the concentration of elements in various samples. It is based on the principle that each
element absorbs light at a unique wavelength, allowing for the identification and quantification
of specific elements.

The basic components of an AAS instrument include a light source, a sample holder, a
monochromator, and a detector. The sample is atomized and exposed to a beam of light at a
specific wavelength corresponding to the element of interest. The amount of light absorbed by
the sample is proportional to the concentration of the element present.

There are different types of AAS techniques, such as Flame AAS, Graphite Furnace AAS,
and Cold Vapor AAS, each with its own advantages and limitations. Flame AAS is commonly
used for the analysis of metals in solution, while Graphite Furnace AAS offers improved
sensitivity and reduced interference for trace elements. Cold Vapor AAS is specifically useful for
the determination of volatile elements such as mercury and arsenic.
 GRAPHITE FURNACE (GF-AAS).

A graphite furnace is a common type of sample introduction system used in atomic

absorption spectrometry (AAS) and inductively coupled plasma atomic emission spectroscopy
(ICP-AES). It is designed to improve the sensitivity and detection limits of these analytical
techniques, particularly for trace and ultratrace analysis of metals and metalloids.

The graphite furnace works by vaporizing and atomizing the sample in a small graphite
tube that is heated to high temperatures using an electric current. The sample is introduced into
the furnace in small volumes, typically in the form of a liquid droplet or a solid sample placed
directly onto the graphite tube. The intense heat of the furnace causes the sample to undergo
thermal decomposition, leading to the formation of free atoms in the gaseous state.

OPERATION OF THE MACHINE

1. Sample Preparation: Before analysis, samples need to be appropriately prepared to

make them suitable for introduction into the graphite furnace. This may involve
digestion, dilution, or filtration steps, depending on the nature of the sample and the
metals of interest.

2. Calibration: A calibration curve is typically established using standard solutions of

known metal concentrations. These calibration standards are run through the graphite
furnace machine to create a linear relationship between the metal concentration and
the instrument response.

3. Sample Introduction: Samples are introduced into the graphite furnace either
manually or automatically using a sample introduction system. The sample is
 transferred into the graphite tube, which is heated to high temperatures to atomize the
analyte.

4. Atomization and Detection: In the graphite furnace, the sample is dried, ashed, and
then atomized at a specific temperature sequence to convert the analyte into free
atoms. These atoms absorb light at characteristic wavelengths when exposed to a
hollow-cathode lamp, and the absorption is measured by the detector.

5. Data Analysis: The absorbance values obtained from the graphite furnace machine
are used to determine the concentration of the analyte in the sample. This is done by
comparing the absorbance values to the calibration curve and applying mathematical
calculations to quantify the amount of metal present.

6. Quality Control: To ensure the accuracy and precision of the results, quality control
measures such as running blank samples, replicates, and control standards are
typically included in the analysis process.
INTERPRETATION:
The interpretation of outputs in GF-AAS is quite simple and follows Beer’s law,
namely that absorbance is directly proportional to concentration. This means that the
analyte’s concentration correlates with the electrical output received from the
detector. One of the ways to determine the unknown concentration of an analyte is to
use several solutions of known concentrations to calibrate the instrument. The curve
shows radiation (absorbance) versus concentration and once the sample is measured,
the concentration value could be obtained from the calibration curve.

COLD VAPOR (CV-AAS).

Cold vapor atomic absorption spectroscopy (CV-AAS) is a specialized technique used for
the detection and quantification of volatile mercury species in environmental and biological
samples. It is a highly sensitive and selective method that relies on the conversion of mercury
compounds into gaseous elemental mercury, which is subsequently measured using an atomic
absorption spectrometer.

In CV-AAS, the sample is first treated with a reducing agent such as stannous chloride
(SnCl2) or sodium borohydride (NaBH4) to convert any mercury present into elemental mercury.
The resulting vapor is then atomized and quantified in the atomic absorption spectrometer, which
measures the absorption of specific wavelengths of light by mercury atoms.

A cold vapor machine, also known as a cold vapor atomic absorption spectrometer
(CVAAS), is a specialized instrument used for the detection and quantification of mercury in
various samples. The operation of a cold vapor machine involves specific steps to ensure
accurate and sensitive measurement of mercury levels.

1. Sample Preparation: Samples containing mercury are typically digested or treated

with specific reagents to release mercury in its volatile form. The sample may be
heated or treated with reducing agents to convert mercury to its elemental form for
analysis.

2. Mercury Vapor Generation: In the cold vapor machine, the released mercury is
converted into vapor form through a process called cold vapor generation. This
usually involves mixing the sample with a reducing agent and a carrier gas to
facilitate the formation of mercury vapor.

3. Atomization and Detection: The generated mercury vapor is introduced into the
atomic absorption spectrometer, where it is atomized and exposed to a light source at
a specific wavelength. The detector measures the absorption of light by the mercury
atoms, allowing for the quantification of mercury levels in the sample.
4. Calibration: Prior to sample analysis, a calibration curve is prepared using standard
solutions with known concentrations of mercury. The calibration curve helps establish
a relationship between the absorbance of mercury vapor and its concentration in the
sample.

5. Sample Analysis: Samples containing mercury are introduced into the cold vapor
machine, and the absorbance of mercury vapor is measured. The instrument calculates
the concentration of mercury in the sample based on the calibration curve and the
absorbance readings.

6. Quality Control: To ensure the accuracy and precision of the analysis, quality control
measures such as running blank samples, replicates, and control standards are
included in the analysis process. This helps to monitor and correct for any potential
sources of error in the measurement.

INTERPRETATION.
The graphite furnace atomic spectroscopy method is based on the excitation of
mercury atoms using electromagnetic radiation. With this method, the free atoms of
mercury in the observation cell are initially in the ground state and are moved to an
excited state by mercury-specific radiation. The atoms then return to the ground state
and re-emit mercury-specific fluorescent radiation, which is converted to an electric
signal in a detector. The measured intensity makes it possible to calculate the mercury
concentration in the sample.

CONCLUSION
In conclusion, Atomic Absorption Spectroscopy (AAS), Graphite Furnace Atomic
Absorption Spectroscopy (GF-AAS), and Cold Vapor Atomic Absorption
Spectroscopy (CV-AAS) are powerful analytical techniques used for the
quantification of trace elements in various samples. AAS is a versatile and widely
used technique with high sensitivity and specificity, while GF-AAS offers improved
detection limits and reduced interference from matrix effects. CV-AAS, on the other
hand, is highly sensitive for the determination of volatile elements such as mercury
and arsenic. Each technique has its own advantages and limitations, and the choice of
method depends on the specific analytical requirements of the sample being studied.
Overall, these techniques play a crucial role in various fields such as environmental
monitoring, clinical diagnostics, and material analysis, providing valuable
information for research and quality control purposes.

INDEX NUMBERS;
Jennifer Addae; UEB3800121
Asante Kate; UEB3800421
Seth Nii Omaboe; UEB3800821
DOMBAYIELE Paul; UEB3801721
Joel Tettey; UEB3802221