Title: Metals by-flame atomic absorption spectrometry

Objective: To investigate properties of metals by using flame atomic absorption spectrometer.

Introduction:
Atomic Absorption Spectroscopy (AAS) is a technique for determining the
concentration of a particular metal element within a sample. Atomic absorption spectroscopy
can be used to analyze the concentration of over 62 different metals in a solution.
In this experiment, atomic absorption spectrometry resembles emission flame
photometry in that a sample is aspirated into a flame and atomized. The major difference is
that in flame photometry the amount of light emitted is measured, whereas in atomic
absorption spectrometry a light beam is directed through the flame, into a monochromator,
and onto a detector that measures the amount of light absorbed by the atomized element in
the flame. For some metals, atomic absorption exhibits superior sensitivity over flame
emission. This is due to each metal has its own characteristic absorption wavelength, a source
lamp composed of that element is used, this makes the method relatively free from spectral or
radiation interferences. The amount of energy at the characteristic wavelength absorbed in the
flame is proportional to the concentration of the element in the sample over a limited
concentration range. Most of the atomic absorption instruments also are equipped for
operation in an emission mode.
Solutions more concentrated than 10-3 to 10-5 M should be diluted to bring them into
this range. Only small volumes of solution, on the order of a few millilitres, are required.
The technique makes use of absorption spectrometry to assess the concentration of an
analyte in a sample. It requires standards with known analyte content to establish the relation
between the measured absorbance and the analyte concentration and relies therefore on
the Beer-Lambert Law. The radiation flux without a sample and with a sample in the
atomizer is measured using a detector, and the ratio between the two values (the absorbance)
is converted to analyte concentration or mass using the Beer-Lambert Law.
Applying Lambert-Beers law in atomic absorption spectroscopy is difficult due to
variations in the atomization from the sample matrix and non-uniformity of concentration and
path length of analyte atoms. Concentration measurements are usually determined from a
calibration curve generated with standards of known concentration.
AAS has many uses in different areas of chemistry such as:
- Clinical analysis: Analyzing metals in biological fluids and tissues such as whole
blood, plasma, urine, saliva, brain tissue, liver, muscle tissue, semen
- Pharmaceuticals: In some pharmaceutical manufacturing processes, minute
quantities of a catalyst that remain in the final drug product
- Water analysis: Analyzing water for its metal content.

While in this experiment, we are going to analyse the lake water sample for its metal content
of Pb, Mg and Cu metals.
Although atomic absorption has caught on quickly as a rapid, useful analytical
method, it does have limitations. The chief problems are instrument drift due to changes in
lamp intensity or wavelength calibration with time and, because of the extreme sensitivity of
the method, trace contamination from reagents, water, and surroundings during sample
preparation and analysis. Frequent rechecks of instrument operation with standard solutions
and care in the preparation and handling of both standard and sample solutions contribute to
improved accuracy and precision of the technique

Apparatus: atomic absorption spectrometer, burner, lamp, pressure-reducing agent, vent,

readout
Materials: water sample, Mg,Cu,Pb, deionized water, stock solution

Procedure:
A. Preparation of Standard Solution
1. The following standard solutions of known metal concentrations in water with matrix
similar to the sample are prepared as following:
Cu- 0.5, 1.0, 1.5 and 2.0 ppm
Pb- 1, 5, 10 and 15 ppm
Mg- 0.5, 1.0, 1.5 and 2.0 ppm
B. Sample measurement
The wavelength used is checked before measure for the samples.
i) Standard solution
1. The blanks are measured using the atomic absorption spectrometer.
2. The standards solutions are then measured from low concentration to high concentration.
3. The absorbance for each standard solution is noted and tabulated.
4. The absorbance readings are used to plot graph.
ii) Water sample
1. The water sample is filtered with placing a piece of filter paper on the filter funnel into a
small beaker.

2. The absorbance of water sample is measured using the same atomic absorption
spectrometer.

Results and Calculations:

Pb standard solution
Concentration (ppm)
1.0
5.0
10.0
15.0
Lake water sample: Absorbance = 0.007

Absorbance
0.028
0.123
0.238
0.333

Graph of absorbance vs concentration

0.35
f(x) = 0.02x
R = 1

0.3
0.25
0.2

Absorbance 0.15
0.1
0.05
0
0.0

2.0

4.0

6.0

8.0

10.0

12.0

Concentration (ppm)

According to the graph, when absorbance = 0.007,

0.007 = 0.0228x
x

= 0.3070 ppm

Actual concentration = 10 x 0.3070 ppm

= 3.070 ppm
Therefore, the concentration of Pb in lake water is 3.070 ppm.

14.0

16.0

Cu standard solution
Concentration (ppm)
0.5
1.0
1.5
2.0
Lake water sample: Absorbance = -0.002

Absorbance
0.086
0.181
0.259
0.314

Graph of absorbance vs concentration

0.35
0.3

f(x) = 0.17x
R = 1

0.25
0.2

Absorbance

0.15
0.1
0.05
0
0.40

0.60

0.80

1.00

1.20

1.40

1.60

1.80

2.00

2.20

Concentration (ppm)

Due to some errors, the absorbance that is given by copper composition in the lake water
sample is a negative value, therefore the concentration of copper in the lake water sample
cannot be found.

Mg standard solution
Concentration (ppm)
0.5
1.0
1.5
2.0
Lake water sample: Absorbance = 2.028

Absorbance
0.786
1.281
1.603
1.785

Graph of absorbance vs concentration

2

f(x) = 1.02x
R = 0.97

1.8
1.6
1.4
1.2

Absorbance

1
0.8
0.6
0.4
0.2
0
0.4

0.6

0.8

1.2

1.4

1.6

Concentration (ppm)

According to the graph, when absorbance = 2.028,

2.028 = 1.0198x
x

= 1.9886 ppm

Actual concentration = 10 x 1.9886 ppm

= 19.886 ppm
Therefore, the concentration of Mg in lake water is 19.886 ppm.

1.8

2.2

Discussion:
In this experiment, the concentration of lead (Pb), magnesium (Mg) and copper (Cu)
in lake water sample are determined by the calibration method using atomic absorption
spectroscopy. Calibration standards are prepared from a 2.0 ppm Cu stock for Cu standards,
15 ppm Pb stock for Pb standards whereas Mg standards are prepared from 2.0 ppm Mg stock
solution. The absorption of each solution was measured on an atomic absorption
spectroscopy.
We are using AAS as the instrument for calibration instead of using UV-Vis
spectrophotometer. This is because there are a few advantages over flame atomic absorption
spectroscopy:
- Solutions, slurries and solid samples can be analysed.
- much more efficient atomization
-greater sensitivity
- smaller quantities of sample (typically 5 50 L)
- provides a reducing environment for easily oxidized elements
In AAS, a substance is vaporized and decomposed into gaseous atoms in flame,
furnace or plasma. It is meant by a gas that is hot enough to contain ions and free electrons.
The concentration of the atoms are measured by absorption or emission of its specific
wavelengths of radiation. The atoms exhibit line absorption and emission spectra because its
electronic transitions are quantized and the atoms are lack of rotational and vibrational states
of molecules.
The linearity of the calibration curve in each standard solution indicates that
absorbance is indeed proportional to analyte concentration and as such is a useful analytical
technique. We were not expecting the level to be way over the limit either because there is no
known sources of contamination from either lead, magnesium or copper in the lake water
sample. The magnesium ion concentration was the highest in the sample and the lowest is
lead in the sample, that is, 19.886 ppm and 3.070 ppm respectively. Due to some errors, the
absorbance that is given by copper composition in the lake water sample is a negative value,
therefore the concentration of copper in the lake water sample cannot be found. Finally, in
this experiment, atomic absorption spectroscopy proved to be a fast and effective method of
measuring levels of the metal content in lake water.
From the calculations, we can see that the concentration of Pb is relatively low. This is
because lead is rarely found in source water, but enters tap water through corrosion of
plumbing materials. If there is excess of lead content in the water, it may lead to lead
poisoning. In babies and children, exposure to lead in drinking water above the action level
can result in delays in physical and mental development, along with slight deficits in attention

span and learning abilities. In adults, it can cause increases in blood pressure. Adults who
drink this water over many years could develop kidney problems or high blood pressure.
In this experiment, the concentration of the Mg content in the lake water sample is too
high compared to the usual water sample. It might be expected as hard water which might be
contaminated with the disposal of factory nearby. Hard water is water that has
high mineral content. Hard water is formed when water percolates through deposits
of calcium and magnesium.
On the other hand, there are a few disadvantages of using AAS, that is, it is an
expensive instrument. It has a low precision and low sample throughput. Besides, it also
requires a high level of operator skill where a student must be guided by lecturer or lab
officer while using this instrument.
As general, the level of copper in surface and groundwater is generally very low. High
levels of copper may get into the environment through mining, farming, manufacturing
operations, and municipal or industrial wastewater releases into rivers and lakes. Copper can
get into drinking water either by directly contaminating well water or through corrosion of
copper pipes if the water is acidic.
For the negative absorbance value of Cu content in the lake water, there might be due
to the error when operating the spectrophotometer. When we are reading the absorbance of a
solution, we always start it by "zeroing" the machine using a blank solution first. The error
might due to the stray light leaked in the machine. If there are light leaks in the machine, in
here we are referring to the flame, or the opening is left cracked, it could get a false reading
of a negative absorbance. Besides, there are a few factors proposed that the reason of getting
a negative absorbance readings. The 1st factor is human error made during the experiment
such as do not add the solution follow the concentration correctly, do not take some
precaution and the solution may be contaminated. The 2nd factor that caused the negative
value of the result obtained may be due to the technical error such as the atomic absorption
spectroscopy (AAS) that is used to determine the absorbance of the ions do not calibrate well.
Besides that, that machine used may not be maintain or repair for a long time, hence it will
caused some inaccurate in the result that obtained.
Therefore, there are some precautionary steps need to be done while conducting this
experiment. The flame should be lit only when measurements are to be made. The standard
solution should be made first before measure it. If the flame is sooty, then the mixture is too
fuel rich; thus we have to decrease the fuel or increase the supporting gas (compressed air). It
is necessary to always aspirate something (usually DI water, or 5% Nitric acid to clean the
inlet tube line) when the flame is on. The flame door is kept closed when making
measurements to prevent air drafts bend the flame over, and leads to uncertainty in results.

Conclusion:
The concentration of lead, magnesium and copper present in the lake water can be
determined by flame atomic absorption spectroscopy. There is only lead and magnesium
metals are detected in the lake water sample collected while the concentration of the copper
we could not detect it. The concentration of lead detected is 3.070 ppm where the
concentration of magnesium is way higher than it, that is, 19.886 ppm.

References:
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