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Experiment [7]

Determination of Iron in Cereal by Atomic Absorption Spectrophotometry

Introduction

The nutritional value of trace amount of certain metals, such as iron and
manganese, is well known. In the experiment iron is determined in a dry, breakfast
cereal. The powdered cereal is digested with a nitric acid-perchloric acid solution.
Atomic absorption spectrophotometry is used to determine the concentration of iron
in the resulting solution. The effect of potentially interfering substances in the
cereal is minimized by use of the standard-addition technique.

Apparatus

50mL beaker Iron Hollow Cathode Lamp

10mL graduated cylinder Mortar and Pestle
1mL graduated pipette 4mL pipette
hot plate 5, 13 X 100mm test tube
25mL volumetric flask 250mL volumetric flask

Chemicals

Acetylene Iron (ll) Ammonium sulfate hexahydrate (reagent grade)

Compressed Air Nitric acid-perchloric acid solution (1:1 volume)
Breakfast Cereal

Procedure

1. Obtain at least 1 g of a dry breakfast cereal.

2. Weigh 0.18 g of iron(II) ammonium sulfate hexahydrate to the nearest 0.1 mg.
Transfer the solid to a 250 mL volumetric flask. Add sufficient distilled or
deionized water to dissolve the solid and dilute the solution to the mark. The
iron concentration of the solution is 100 mg/liter.
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3. Place the cereal in a mortar. Use a pestle to grind the cereal into a powder.
Into a 50 mL beaker weigh to the nearest 0.1 mg about 0.5 g of the powdered
cereal.

Caution: The remainder of the experiment could be hazardous. The use of

safety glasses is required at all times.

4. Place the beaker on a hot plate in the hood. Cautiously add 10 mL of the nitric
acid-perchloric acid solution. Gently warm the beaker until the sample is
colourless. Iron in the sample is dissolved in the acid solution during this step.

5. After digestion is complete, transfer the solution to a 25 mL volumetric flask.

Rinse the beaker twice with 5 mL portions of distilled or deionized water. Pour
the rinsings into the volumetric flask. Dilute the solution to the mark with
distilled or deionized water.

6. Label five, 13 x 100 mm test tubes with S, 1, 2, 3, and 4. Use a pipet to add 4
mL of the 25 mL sample solution to each of the five test tubes. Use the 1 mL
graduated pipet to transfer 0.20 mL of the 100 mg/liter iron solution to 1, 0.30
mL to tube 2, 0.40 mL to tube 3, and 0.60 mL to tube 4.

7. Use a graduated 1 mL pipet to add 1.00 mL of distilled or deionized water to

tube S, 0.80 mL to tube 1, 0.70 mL to tube 2, 0.60 mL to tube 3, and 0.40 mL to
tube 4. Each tube should contain a total of 5.00 mL of solution.

8. Insert and iron hollow cathode lamp into the atomic absorption
spectrophotometer. Refer to the supplied instructions and optimize the signal
and prepare for the analysis.

9. Successively aspirate the solutions in the five test tubes into the flame. Record
the instrumental reading from each solution.

10. Close the acetylene quick-shut-off valve and allow the flame to extinguish.
After the flame has extinguished, close the valve on the acetylene tank, open
the quick-shut-off valve and allow the acetylene to drain from the acetylene
line. Shut off the air supply and turn off the instrument. Turn off the hood.
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Calculations

1. Use the mass of the iron(II) ammonium sulfate hexahydrate (MW 392.14) and
the volume of the solution (250.0 mL) to calculate the concentration (mg/liter)
of iron (AW 55.847) in the standard solution.

2. Use the concentration of the standard solution, the volume of the solution
which was added to each of test tubes 1 through 4, and the final solution
volumes (5.00 mL) to calculate the added concentration (mg/liter) of iron which
was in each of the tubes.

3. Prepare a plot of absorbance (or instrumental reading) (y axis) as a function of

the added iron concentration for the solutions that are in tubes S, 1, 2, 3, and
4. Draw a straight line through the data points and extrapolate it to
intersection with the concentration axis. The distance on the concentration
axis between the origin and the intersection with the extrapolated line
corresponds to the concentration of iron which is in tube S.

4. Use the dilution factor (4 mL diluted to 5 mL) and the iron concentration that
is in tube S to calculate the concentration in the undiluted sample solution.
Use that concentration and the total sample-solution volume (25.0 mL) to
calculate the mass (mg) or iron in the weighed dog food. Use the iron mass and
the cereal mass to calculate the concentration (mg/g) of iron that is in the
cereal.