Lab #12: Quantification of Iron in Whole

Grain Cereal
Brenden Bowerman
6, 2014
Partner: Joseph Messler
Instructor: David Morris

November

LABORATORY WRITTEN REPORT

Objective
The objective of this lab is to develop good lab techniques in data collection using
computers to model and generate a calibration curve. Doing this will help the
experimenter in understanding the relationship between chemistry and food
products using dilution concepts. Other objectives include gaining experience in
writing experimental procedures.

Experimental Method1
Take ten grams of cereal and grind it to a fine powder using an electric grinder.
Transfer the powder to a glass beaker (probably 100mL) and add enough water to
make a mobile slurry. Extract the iron fillings magnetically by stirring the bar for
approximately ten minutes. Remove the stirrer bar from the slurry. Pour off a
majority of the wheat mush, and have another stirrer bar outside of the beaker to
prevent any overflow of iron fillings. Rinse the remaining flakes from the beaker
and stirrer bar using DI water. Rinse the stirrer with DI water and iron into a test
tube. Add six milliliters of 6 M HCl (aq). Place the test tube into a hot water bath.
Wait ten minutes. The dissolution is complete when the solution is a pale green.
Transfer one hundred milliliters of this solution into a one hundred milliliter
volumetric flask. One milliliter of a ten ppm Fe 2+ stock solution is transferred to a
previously calibrated test tube. Add two drops of 6M HCl (aq), 0.5 milliliters of
Hydroxylamine-HCl, six drops of 2M Sodium Acetate, and one milliliter of 0.1%
Dipydridyl solution to the test tube. Fill the test tube to the ten milliliter line with
DI water. Wait fifteen minutes. The final product is a 1 ppm standard solution.
Repeat steps 1-4 using the rest of the ten p pm quantities found in table 12-1.
The absorbance of each solution is measured at 522 nanometers. Depending on
the success of the iron extraction, the sample solution may need to be
quantitatively diluted to make the absorbance lie on the standard curve.

Experimental Data
Table 12-1: Solutions prepared for AA absorption analysis

Solution
(ppm)
1.0
2.0

HCl
(drops)
2
2

Hydroxylami CH3COONa Dipydridyl

ne (mL)
(drops)
(mL)
0.5
6
1.0
0.5
6
1.0

Absorptio
n
0.0897
0.2004

4.0
5.0
8.0
Prepared

2
2
2
2

0.5
0.5
0.5
0.5

6
6
6
6

1.0
1.0
1.0
1.0

0.3454
0.5001
0.6110
0.3977

The table on the previous page shows the amounts of different solutions added to
the prepared iron solution. The table also shows the absorption at 522
nanometers to help the experimenter determine the concentration of the solution.
Figure 12-1: Concentration vs. Absorption graph

This graph shows the linear trend between the different absorptions between the
different standard solutions. The equation allows for the calculation of the
concentration of iron in the prepared solution. The r-squared value dictates if a
linear approximation is appropriate for this data set. Since this r-squared value is
very close to 1 (0.9535), the approximation is appropriate.

Observations
The only observations that I noticed during this experiment fall in the category of
color changes. To elaborate, when placing the HCl and Fe solution into the hot
water bath, I began to notice a color change. The procedure states that the
solution is finished in the bath when the color changes from a somewhat cloudy
but clear solution to a pale green solution. While our solution seemed more of a
pale yellow than a pale green, the color differences were difficult to determine.
The second example of a color change I noticed was within the AA machine.
When the standard solutions were not being analyzed by the AA instrument, the
fire seemed to have a pinkish-orange tint and a small flame. When the standard

solutions were being analyzed, however, the flame seemed to change to a strong
orange color and increase in size as well.

Sample Calculations
Calculation of the concentration of the prepared iron solution
Absorption = 0.3977
y is the absorption and x is the concentration
y = 0.0758x + 0.0461
x = (y 0.0461)/0.0758
x = (0.3977-0.0461)/0.0758
x = 4.6385224274 ppm

Results & Discussion

Looking at the graph, there seems to be one obvious outlier within the stock
solutions (5 ppm). However, the data as a whole does fit a linear model. When we
tried to test our diluted solution in the AA machine, we observed an absorption of
approximately 0.08, which is less than the 1 ppm solution. Fortunately, we were
told to retry our solution, but to use the prepared solution as opposed to the
diluted solution. Doing this yielded what seemed to be an appropriate absorption
of 0.3977. Since the direct analysis was implemented, there was no need to use
dilution calculations to determine the true absorbance.

Experimental Uncertainty
There were several opportunities for uncertainties to arise. For example, in taking
measurements of the iron, random error could have affected the mass of cereal
measured while the scale has its own systematic uncertainties. There are other
systematic uncertainties when the solutions are transferred between the
glassware since there is not a perfect transfer of the solutions held in the
glassware. Again error arises in extracting the iron from the mobile slurry, as the
magnetic stirrer bar does not always attract one hundred percent of the iron in
the slurry. It is obvious that I as an experimenter made an error as the diluted
solution I prepared did not meet the standard and we had to directly analyze our
solution.

Post Laboratory Questions

1. Did the iron measured in the cereal in the laboratory experiment compare
to that provide on the consumer label? Why or why not? The iron measured
in the cereal in the laboratory experiment was less than the iron provided
on the consumer label. This can be explained due to the various

opportunities for errors to arise, thus giving an experimental yield less than
what the consumer label provides.
2. Why was it important to use volumetric glassware to prepare your sample?
It is important to use volumetric glassware to prepare the sample because
volumetric glassware is the most accurate glassware provided in the
laboratory.

Conclusion
The objective of this lab was to develop good lab techniques in data collection
using computers to model and generate a calibration curve and help the
experimenter in understanding the relationship between chemistry and food
products. From this lab, the experimenter gained the skills of writing an
experimental procedure as well as gaining experience using dilution concepts.
Overall, even though there were several mistakes made in following the
experimental procedure, the results ended up being what they should be.

References
1.
Amateis, P. L., V. & Dalton, M., General Chemistry 1045 Laboratory Experiments in
General Chemistry. Hayden-McNeil Publiching: Plymouth, MI, 2015.