CHM312: INSTRUMENTAL ANALYSIS

IRON IN BREAKFAST CEREAL BY ATOMIC ABSORPTION

SPECTROSCOPY (AAS)

NAME : SHARIFAH NAFILAH BT SYED KHOLED

STUDENT NO: 2015871262

GROUP : RAS1155B

LAB PARTNERS NAME :

NAME MATRIX ID
ALYAA BINTI ABDUL JABAR 2015846872

MUHAMMAD FIRDAUS BIN AHMAD SUHAINI 2015876982

NURUL SYAAHIDA BINTI AULIA SHAM 2015897564

RAFIQ IZZARIL BIN ROSDI 2015883364

LECTURERS NAME: SIR MOHD HAFIZ BIN YAAKOB

DATE THE OF SUBMISSION : 24 NOVEMBER 2017

ABSTRACT

The objective of this experiment is to determine iron content in cereals. The experiment was
conducted by using atomic absorption spectroscopy analysis. Before running the analysis
using AAS, first a series of standard solutions based on iron concentration was established. A
100ppm stock solution of iron is prepared in 100mL flask. From the stock solution, a series of
standard solution of 5ppm, 10ppm, 15ppm, 25ppm and 50ppm was prepared by diluting a
specific volume from the stock solution in five individual flasks to the respected
concentration. For sample analysis, the cereals used are coco crunch, honey star and
cornflake. The Ash solution was prepared by dissolved the cereal with hydrochloric acid
solution and place on the hot plate. Simmer gently about 45 minutes to break down the cereal
and bring the iron into soluble form. To minimize the matrix effect on the analytical signal,
the standard addition method was used in sample preparation prior to the analysis step.
Atomization was accomplished with air/acetylene flame, and the absorbance measurements
were made at the 248.3 nm iron resonance line. We can find the concentration of iron in the
sample running a series of calibration standards through the instrument. By plotting the
absorption versus the concentrations of the standards, a calibration curve can be plotted.
Results obtained the AAS showed good general agreement, with a correlation coefficient of
0.999532. The concentration of Fe in coco crunch is 16.715 mg/L, for honey star is 15.474
and for cornflake is 14.858.

INTRODUCTION

Iron is one of the most important of the essential minerals in our diet, because it is the
element that is responsible for the oxygen-carrying ability of haemoglobin in red blood cells.
Iron is also present in a number of other biologically significant molecules.

In this lab you will analyse breakfast cereals, to find out the actual iron content of different
brands of cereals, and to compare the experimental results with the values listed on the
manufacturers' labels. Typical methods for preparing solutions of these cereal samples
include digestion in acid, oxidation, heating, use of magnets, and filtration. The analytical
technique to be used in this determination is atomic absorption spectrophotometry.
Atomic absorption spectroscopy (AAS) is a widely used technique for determining a large
number of metals. In the most common implementation of AAS, a liquid sample containing
the metal analyte is aspirated into flame using nebulizer, causes the atom to undergo a
transition from the ground state to the first excited state. When the atoms make their
transition, they absorb some of the light from the beam. The more concentrated the solution,
the more light energy is absorbed. The light beam is generated by a lamp that is specific for a
target metal. A line source (hollow cathode lamp) must be perfectly aligned so the beam
crosses the hottest part of the flame and travels into the photomultiplier detector. The detector
measures the intensity of the beam of light. When some of the light absorbed by a metal, the
beams intensity is reduced. The detector records that reduction as absorption. That
absorption is shown on a read out by the data system.

OBJECTIVES

1. To learn how to operate a flame AAS instrument.

2. To plot a standard calibration curve for determination of Fe in a sample.
3. To determine the amount of iron in a sample using the standard calibration curve.

APPARATUS

Beaker Pipette
Dropper Hot plate
Volumetric flask (50ml, 100ml, Watch glasses
250ml)

CHEMICALS

Three brands of breakfast cereals (koko crunch, honey star, cornflake)

Deionized water
1000 ppm Fe stock solution
3M Hydrochloric acid (HCl)
PROCEDURE

A. Preparation of sample
1. Three sample, each 5g of cereal was weighed accurately and was grinded into fine
powder using mortar and pestle.
2. Each sample was put into 250 mL beaker then 50 mL of 3M hydrochloric acid
(HCl) was added.
3. The beaker was covered with watch glasses and placed on the hot plate.
4. The mixture was simmered gently about 45 minutes to break down the cereal and
bring the iron into soluble form.
5. The sample was let to cooled and then the down watch glasses and sides the
beaker was washed with small quantities of distilled water.
6. The sample was stirred thoroughly and filtered into 100 mL volumetric flask.
7. Then, it was diluted to the mark, put a stopper and mixed.

B. Preparation of 100 ppm iron solution

M1V1 = M2V2
(1000 ppm)(V1) = (100 ppm)(100 mL)
V1 = 10 mL

1. 10 mL of 1000 ppm iron solution was pipetted and transferred into a 100 mL
volumetric flask.
2. Deionized water was added to the mark.
3. Volumetric flask was put a stopper and was shaken it several time.

C. Preparation of standard solution

1. 2.50 mL of iron solution was pipetted from 100 ppm iron solution and it was
transferred in a 50 mL volumetric flask.
2. Deionized water was added to the mark and was shaken it well.
3. The solution was transferred into container and was labelled as 5 ppm.
4. Step 1-3 was repeated to prepare 10 ppm, 15 ppm, 25 ppm, and 50 ppm of the
standard solution.
CALCULATION

For preparation of standard solution

1) 5 ppm of standard

M1V1 = M2V2 4) 25 ppm of standard

(100 ppm)(V1) = (5 ppm)(50 mL) M1V1 = M2V2

V1 = 2.50 mL (100 ppm)(V1) = (25 ppm)(50 mL)

2) 10 ppm of standard V1 = 12.50 mL

M1V1 = M2V2 5) 50 ppm of standard

(100 ppm)(V1) = (10 ppm)(50 mL) M1V1 = M2V2

V1 = 5.00 mL (100 ppm)(V1) = (50 ppm)(50 mL)

3) 15 ppm of standard V1=25mL

M1V1 = M2V2

(100 ppm)(V1) = (15 ppm)(50 mL)

V1 = 7.50 mL
Comparing the iron (Fe) from the experiment and product labels.

Koko Krunch
Atomic Absorption Spectroscopy (AAS) Values in manufactures label
method
16.715 mg/L per 5 grams 14.0 mg per 100 grams

Mass= 16.715 0.1 5 gram= 0.7 mg

= 1.6715 mg

Honey Star
Atomic Absorption Spectroscopy (AAS) Values in manufactures label
method
15.474 mg/L per 5 grams 14.0 mg per 100 grams

Mass= 15.474 0.1 5 gram= 0.7 mg

= 1.5474mg
Cornflake
Atomic Absorption Spectroscopy (AAS) Values in manufactures label
method
14.858 mg/L per 5 grams 12.0 mg per 100 grams

Mass= 14.858 0.1 5 gram= 0.6 mg

= 1.4858 mg
DISCUSSION

Many breakfast cereals are fortified with iron, which is essential for transport of oxygen in
blood throughout human bodies. The iron is simply sprayed on the cereal and can be
separated by physical processes. In this experiment, three different cereals are used including
those with different iron concentrations which are coco crunch, honey star and cornflake.

Typical methods for preparing solutions of these cereal samples include digestion in acid,
oxidation, heating, use of magnets, and filtration. For Analysis techniques are most
commonly Atomic Absorption spectroscopy (AAS). Ideally, the outcome would be to have
producible data, indicating high precision, and data similar to the theoretical values reported
by the cereal companies, indicating high accuracy.

Atomic absorption spectroscopy (AAS) is a spectroanalytical procedure for the quantitative

determination of chemical elements using the absorption of optical radiation (light) by free
atoms in the gaseous state. AAS can be used to determine over 70 different elements in
solution or directly in solid samples.

In this experiment, we use Flame Atomic Absorption Spectroscopy (AAS) in order to

determine the concentration of iron in the cereals. In flame atomizer, a solution of the sample
is nebulized by the flow of gaseous oxidant which is nitrous oxide mixed with acetylene as a
gaseous fuel, and carried into a flame where atomization occurs. This experiment consisting
of nebulization, which converts a liquid into a fine spray or mist, called an aerosol.
Concentric tube type was used as a nebulizer in which the liquid sample is sucked through a
capillary tube by a high pressure stream of a gas flowing around the tip of the tube. This
process is called aspiration. Aspiration is the process by which a sample solution is drawn by
suction in atomic spectroscopy. The flame atomizer which is the laminar flow burner
employs a concentric tube nebulizer which acts as atomizer to convert a sample into gas-
phase atom or elementary ion.

The atoms should then be irradiated by optical radiation, and the radiation source that used in
this experiment is Hollow Cathode Lamp (HCL) as a line source. As we used a double beam
instrument, the beam of the hollow cathode lamp is split by a chopper, one half passing
through the flame and the other half around it. Chopper is a device use for source modulation
to eliminate interferences caused by emission of radiation by the flame. The two beams are
then recombined by a half- slivered mirror that returns both beam to a single path then pass
through the monochromator to eliminate most of the radiation originating from the flames,
which is finally measured by a detector. Photomultiplier was used as a detector to convert the
light signal into an electrical signal proportional to the light intensity. The radiation that was
measured by the detector then indicated on the readout.

The concentration of iron in cereals can be finding by running a series of calibration

standards through the instrument. By plotting the absorption versus the concentrations of the
standards, a calibration curve can be plotted. Results obtained the AAS showed good general
agreement, with a correlation coefficient of 0.999532. The standard addition plots yielded
correlation coefficient values close to 1, which implies that the method of standard addition
was successful.

Then, the cereals sample was prepared by dry digestion. The Ash solution was prepared by
dissolved the cereal with hydrochloric acid solution and place on the hot plate. Simmer gently
about 45 minutes to break down the cereal and bring the iron into soluble form. Then, the
cereals were run in the AAS. The concentration of Fe in coco crunch is 16.715 mg/L, for
honey star is 15.474 mg/L and for cornflake is 14.858 mg/L. This shows that iron content in
coco crunch is higher than honey star and cornflake.

There are difference amount of iron in cereals obtained from the experiment with the content
value of iron stated on the manufacturers labels which are Coco crunch is 0.9715 mg lack of
iron in 5 grams per serving. While for Honey Star, 0.8474 mg lack of iron in 5 grams per
serving and Cornflake is 0.8858 mg excess of iron in 5 grams per serving. There are
differences in the results obtained with the content value of iron listed on the manufacturers
labels.

In lab, some interference might happen such as spectral interference, chemical interference
and ionization interference. Interference is any effect that changes the signal while analyte
concentration remains unchanged. Interference can be corrected by removing the source of
interference or by preparing standards that exhibit the same interference.

Some precaution you must take while doing the experiment are make sure the chemical used
was labelled to avoid the confusion of the standards concentration used. Besides that, every
time in measuring the solution must be used the proper flask so that the amount of the
solution is exact.
CONCLUSION

As the conclusion, the experiment has met the objectives which are to plot a standard
calibration curve for determination of iron in a sample and to determine the amount of Fe in a
cereals (coco crunch, honey star and cornflake) using the standard calibration curve. . The
present of iron was identified in the cereals sample by using AAS. The concentration of iron
in cereals can be finding by running a series of calibration standards through the instrument.
From the result, the correlation coefficient of iron standard achieved was 0.999532. The
standard addition plots yielded correlation coefficient values close to 1, which implies that
the method of standard addition was successful. Then, the sample has to be run and and the
result was recorded. The concentration of Fe in coco crunch is 16.715 mg/L, for honey star is
15.474 and for cornflake is 14.858.

REFERENCES

1. file:///C:/Users/User/Desktop/lab%20report/aas/iron.pdf
2. file:///C:/Users/User/Desktop/lab%20report/aas/BW1.pdf
3. CHM 312 Instrumental Analysis Laboratory Lab Manual
4. CHM 260 Basic Instrumental Analysis Lab Manual