Bassani 1

Alessandra Bassani

Mrs. Gephart

AP Chemistry

23 April 2018

Standardization of KMnO₄ and the Mass (mg) of Fe²+ in

Commercial Iron Pills

Abstract

A redox titration was performed between potassium permanganate (KMnO₄) and

CareOne iron pills, lot #6HN1825, expiration date 06/2019, to determine if the concentration of

Fe²+ was accurate to the label (65mg) (5Fe²+ + 8H+ + MnO₄- ⟶5Fe³+ + Mn²+ + 4H₂O). The

KMnO₄ solution was standardized with iron (II) ammonium sulfate hexahydrate (Fe(NH₄)₂(SO₄)₂

・6H₂O) to a molar concentration of 0.00959M and reacted with approximately 0.300g of the iron

pills. The mass of Fe²+ was calculated by the moles of Fe²+ in the flask and the volume of

KMnO₄ delivered. The CareOne label states that the supplements contain 65mg of Fe²+ from the

ferrous sulfate (FeSO4), and they were calculated to have 66.1mg, which is a 7.36% error. The

calculated value of 66.1mg fits within the FDA regulated 95% prediction interval (92).

Introduction

Redox titration is a laboratory method that is used to determine the concentration of an

unknown solution by reacting it with a solution that has a known concentration. To do this, the

KMnO₄ solution was standardized. The titrant (KMnO₄) was put in a buret and secured over an
 Bassani 2

erlenmeyer flask. The tirant was slowly released into the flask until the equivalence point was

reached. The equivalence point of the reaction was reached when the number of moles of

electrons in the oxidation half reaction equaled the number of moles of electrons gained in the

reduction half reaction. This could be determined by a color change in the solution. This color

should have matched the color intensity of the color standard for the reaction. The reaction

reached its equivalence point when the color change remained longer than five seconds in the

solution. Once this occured, the moles of KMnO₄ delivered could be determined by

stoichiometry and the actual concentration of KMnO₄ could be calculated.

Stoichiometry is the relationship between different species in a reaction, and it was used

to standardize the KMnO₄ and determine the concentration of Fe²+ in CareOne iron pills. By

using the number of moles of (Fe(NH₄)₂(SO₄)₂・6H₂O) (FAS) in the flask (Fe²+ ⟶Fe³+), which

was a standard, it could be converted to the number of moles of KMnO₄ required to reach the

equivalence point (5Fe²+ + 8H+ + MnO₄- ⟶5Fe³+ + Mn²+ + 4H₂O). This comes from the balanced

reaction between Fe(NH₄)₂(SO₄)₂・6H₂O and KMnO₄. This is because the FAS provided Fe²+ to

be oxidized to Fe³+. By dividing the moles of KMnO₄ by the volume delivered, the concentration

of KMnO₄ could be determined more precisely. This was important when the KMnO₄ was

titrated into the iron pills, since the known concentration and volume of titrant delivered could be

used to find the mass of Fe²+ in the supplements. By performing this standardization, a more

precise concentration was able to be calculated, which helped with the validity of the experiment.

An oxidation-reduction reaction is a type of reaction that involves the transfer of

electrons between species. The reactant that loses electrons is oxidized, and is the reducing agent

since it causes other species to reduce. The reactant that gains electrons is reduced, and is the
 Bassani 3

oxidizing agent since it causes other substances to be oxidized. This can be determined by the

oxidation numbers of each element in the species. The oxidation-reduction reaction that occurred

between KMnO₄ and FAS caused the Fe²+ to be oxidized to Fe³+ (Fe²+ ⟶Fe³+) (Equation 1) and

the MnO₄¯ to be reduced to Mn²+ (8H+ + MnO₄- ⟶Mn²+ + 4H₂O) (Equation 2). The net-ionic

oxidation reduction reaction between KMnO₄ and FAS is (5Fe²+ + 8H+ + MnO₄- ⟶5Fe³+ + Mn²+

+ 4H₂O) (Equation 3).

The purpose of this lab was to analyze the Fe²+content in CareOne iron pills and

determine if the stated Fe²+ concentration of 65 mg on the label was accurate to the calculated

concentration. The Fe²+ comes from ferrous sulfate (FeSO4) which makes up the iron pill. It is

important that the amount of iron a person takes matches what is printed on the label, since the

supplement is taken to increase someone’s iron levels. People take different amounts of iron

depending on their age, gender, and health, and it is vital for the transportation of oxygen in the

blood. Without the proper Fe²+ levels, the body is unable to make red blood cells which are

needed for the body to function properly (Watson). When too much Fe²+ is taken, serious health

problems can develop, since there is too much free iron in the body. This can affect the brain and

liver, which can then damage vital cells (Arnarson). However, when too little Fe²+ is taken, a

person becomes anemic. This is a result of there being a low amount of hemoglobin in the body,

which causes the body not to get enough oxygen (WebMD).

It was hypothesized that the Fe²+ mass in CareOne iron pills would be close to the 65 mg

stated on the label, because the Consumer Healthcare Products Association describes how the

manufacturer of dietary supplements must ensure that the information on the label is accurate

(Consumer Healthcare Products Association). Additionally, the Food and Drug Administration

monitors the information on the supplement to assure the labeling is correct (National Institutes
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of Health). By performing a redox titration, the concentration of Fe²+ in the iron pills was able to

be calculated to determine the accuracy of the label. Since the mass of the iron pills were

measured by mass by difference, it was expected that the Fe²+ concentration in the CareOne iron

pills (FeSO4) would be in accordance with the CareOne bottle label’s value of 65 mg.

Materials and Methods

Part I: Standardization of 〜 0.01 M KMnO₄

A 50-mL buret was filled with KMnO₄ by following a standard operating procedure

which included washing the buret with soap, rinsing it with tap water, rinsing it with distilled

water, and rinsing it will small amounts of KMnO₄. The mass of three Erlenmeyer flasks were

then massed along with approximately 0.5 g of Fe(NH₄)₂(SO₄)₂・6H₂O (FAS) (see Table 1, page

7). Each flask received approximately 0.5 g of FAS, but the actual value was calculated by mass

by difference (see Table 1: Determining Mass of (Fe(NH₄)₂(SO₄)₂・6H₂O) in Erlenmeyer Flasks,

page 12). To dissolve the FAS, 10 mL of distilled water and 5 mL of 3M H2SO4 were added to

each flask and swirled. For a reference on the color change that would occur when KMnO₄ was

added to the FAS solution, one drop of KMnO₄ was added to a beaker with 50 mL of water. This

was the color standard, and when the reaction reached its equivalence point, the color intensity

matched the color standard. The color lasted for at least five seconds.
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(Nazarenko) Figure 1.

An example of the redox titration with KMnO₄ as the titrant. The color change shown on the

right is the color change that occurs when the reaction reaches its equivalence point.

The KMnO₄ was then standardized to determine the concentration of the MnO₄- ion. The

initial volume of the buret with the KMnO₄ was recorded to ±0.01 mL, and then it was added to

each flask until the equivalence point was reached. Once this the color change matched the color

standard, the final volume of the buret was recorded (see Table 2, page 8). The amount of titrant

delivered was calculated by subtracting the ending volume of the KMnO₄ in the buret from the

starting volume (see Table 2: Determining Titrant Delivered for KMnO₄ Standardization, page

12). Since the number of grams of FAS in each flask was a known value, it was converted to

moles by dividing the grams by the the molar mass of FAS. This was then converted to the moles

of KMnO₄ by using stoichiometry. Since MnO₄- is a one to one ratio with KMnO₄, the number of

moles of KMnO₄ equaled the number of moles of MnO₄-. This value was then used to determine

the [MnO₄-] This was done for the three trials, and the concentrations were averaged together to

get a single concentration (see Table 3: Determining [MnO₄-], page 13). Once the concentration

of the MnO₄- was determined to be 0.00959 M, it was able to be used as the titrant for the
 Bassani 6

determination of the Fe²+ concentration in the iron pill (see Table 3: Determining [MnO₄-], page

13).

Part II: Analysis of CareOne Iron Pill

The mass of ten iron pills was recorded and averaged to get the mass of one iron pill (see

Table 4: Determining Average Mass of Iron Pill, page 13). Two iron pills were then grinded up

in a mortar and pestle, and approximately 0.300 g of the power was measured. Two Erlenmeyer

flasks were massed before and after the powder was added. The mass of the powder in the flasks

was determined by mass by difference (see Table 5: Determining the Mass of Fe²+ in Erlenmeyer

Flasks, page 14). 25 mL of distilled water and 15 mL of H2SO4 were added to each flask and

swirled to dissolve the iron pill. The initial volume of the KMnO₄ in the buret was recorded, and

it was added to the flask until the equivalence point was reached. Once the color intensity

matched the color standard for at least five seconds, the final volume of KMnO₄ in the buret was

recorded (see Table 6, page 10). The amount of titrant delivered was calculated by subtracting

the ending volume of the KMnO₄ in the buret from the starting volume (see Table 6:

Determining Titrant Delivered for Analysis of Iron Pill, page 14). Since the concentration of the

KMnO₄ was calculated when the KMnO₄ was standardized, it could be converted to moles by

multiplying the amount of titrant delivered by its concentration. Stoichiometry was then used to

determine the moles of Fe²+, and this was converted to grams of Fe²+ by using its molar mass

(5Fe²+ + 8H+ + MnO₄- ⟶5Fe³+ + Mn²+ + 4H₂O) (see Table 7: Determining the Mass of Fe²+ in

Sample, page 14). The percent of Fe²+ in the sample was found by dividing the calculated mass

of Fe²+, by the mass of the iron that was in the Erlenmeyer flask. This was multiplied by the

average mass of one iron pill to get the amount of Fe²+ in the iron pill. Since the value was in

grams and the CareOne label has the amount of Fe²+ in miligrams, the calculated value was
 Bassani 7

multiplied by 1000 mg. To find the percent error, the amount of Fe²+ calculated was subtracted

from the amount of Fe²+ on the label, and divided by the amount of Fe²+ on the label. This was

then multiplied by one hundred (see Table 8: Determining Mass of Fe²+ in CareOne Iron Pills

and Percent Error from Printed Label, page 15).

Results

It was determined from an average of four trials, that the amount of Fe²+ in Care One Iron

Pills was 66.1 mg. On the label it states that the iron pills have 65 mg of Fe²+, which makes the

calculated value have a 7.36% error from the printed value. There was a standard deviation of

±7.3 from all four trials.

Table 1. Mass of Erlenmeyer Flasks and (Fe(NH₄)₂(SO₄)₂・6H₂O)

Flask Mass of Flask (g) Mass of Flask with FAS (g) Mass of FAS (g)

1 74.681 75.147 0.466

2 79.759 80.280 0.521

3 91.633 92.204 0.571

In Table 1 (page 7) the mass of the Erlenmeyer flasks with and without (Fe(NH₄)₂(SO₄)₂・

6H₂O) FAS are recorded. These values were used to determine the mass of FAS by using the

method of mass by difference. By using this technique, the exact mass of FAS could be used in

the titration with KMnO₄. This method ensured that all the FAS was accounted for. If any of the

FAS was spilled during the transfer from the weighing dish to the Erlenmeyer flask, this would
 Bassani 8

not affect the moles of FAS in the flask. This is because the mass of FAS was calculated after it

was in the Erlenmeyer flask.

Table 2. Volume of KMnO₄ Before and After Being Delivered To Determine [KMnO₄]

Flask Volume Before Volume After Volume of Titrant

Titration (mL) Titration (mL) Delivered (mL)

1 0.00 25.19 25.19

2 0.00 27.15 27.15

3 0.00 30.50 30.50

Table 2 (page 8) shows the volumes of KMnO₄ before and after the equivalence point of

the reaction was reached (5Fe²+ + 8H+ + MnO₄- ⟶5Fe³+ + Mn²+ + 4H₂O). Since KMnO₄ was the

titrant, it was important to record the initial and final volumes. Each time the buret started at 0.00

mL, and the titrant delivered was the value where the KMnO₄ ended in the buret. By determining

the amount of titrant delivered, this value could then be used to calculate the [KMnO₄].

Table 3. Moles of Fe²ᐩ , MnO₄-, and [MnO₄-] Determined After Standardization of KMnO₄

Flask Moles of Fe²+ Moles of MnO₄- [MnO₄-]

1 0.00119 2.38 x 10-4 0.00943 M

2 0.00133 2.66 x 10-4 0.00978 M

3 0.00146 2.91 x 10-4 0.00955 M

Average 0.00959 M
 Bassani 9

Table 3 (page 8) shows the number of moles of Fe²+ and MnO₄- that were calculated,

which were used to determine the [MnO₄-]. Since the mass of FAS in the flask was determined

by mass by difference in Table 1 (page 7), this was a known value. This value was then divided

by the molar mass of FAS to get the moles of FAS. Since Fe²+ was in a one to one ratio with

FAS (Fe(NH₄)₂(SO₄)₂), the number of moles of Fe²+ equaled the moles of FAS. Using

stoichiometry, the moles of Fe²+ was able to be converted to the moles of KMnO₄. Since MnO₄-

is a one to one ratio with KMnO₄ as well, the number of moles of KMnO₄ equaled the number of

moles of MnO₄-. Then by using the volume of KMnO₄ delivered from the buret to the

Erlenmeyer flask in Table 2 (page 8), the [MnO₄-] was determined. This was done by dividing

the moles of MnO₄- by the the volume delivered in liters. The [MnO₄-] for each trial was

averaged together to get a single concentration, see calculations page.

Table 4. Mass of 10 Iron Pills and the Average of One Pill

Mass of 10 Iron Pills (g) Average of One Pill (g)

3.835 0.3835

Table 4 (page 9) shows the mass of ten iron pills which was divided by ten to get the

average mass of a single iron pill. This value was needed when the percent of Fe²+ in the sample

was calculated.

Table 5. Mass of Erlenmeyer Flasks and Fe²+

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Flask Mass of Flask (g) Mass of Flask with Fe²+ (g) Mass of Fe²+ (g)

1 74.756 75.105 0.349

2 94.529 94.955 0.426

Mass by difference was used once again, but this time it was used to determine the

amount of Fe²+ that would be used in the titration. Table 5 (page 10) shows the masses of the two

Erlenmeyer flasks before and after the Fe²+ was added. By subtracting these two values, the mass

of Fe²+ was able to be calculated. This ensured that all the Fe²+ was accounted for, and if any was

spilt it did not impact the calculations for the concentration of Fe²+ in CareOne iron pills.

Table 6. Volume of KMnO₄ Before and After Being Delivered To Determine Mass of Fe²+

Flask Volume Before Volume After Volume of Titrant

Titration (mL) Titration (mL) Delivered (mL)

1 0.00 21.70 21.70

2 0.00 27.20 27.20

The volume of KMnO₄ was recorded in Table 6 (page 10), so the volume of the titrant

delivered could be determined. Each time the buret started at 0.00 mL, and the volume of the

titrant after the equivalence point was reached was the final volume. Since the buret started at

0.00 mL, the volume of titrant delivered was the same as the volume of KMnO₄ after the titration

was complete. By recording these values, the concentration of Fe²+ in the iron pill could be

calculated.

Table 7. Moles of MnO₄-, Fe²+, and Mass of Fe²+ Determined After Known [KMnO₄] Titrated
 Bassani 11

Flask Moles of MnO₄- Moles of Fe²+ Mass of Fe²+ (g)

1 2.08 x 10-4 0.00104 0.0581

2 2.61 x 10-4 0.00139 0.0728

Table 7 (page 11) shows the moles of MnO₄- and Fe²+ that were able to be used to

calculate the mass of Fe²+ in the iron pill. These values were determined by using the volume of

titrant delivered in Table 6 (page 10) and the concentration of MnO₄- that was calculated in Table

3 (page 8). By multiplying the [MnO₄-] by the volume of titrant delivered in liters, the moles of

MnO₄- were calculated. Then by using the moles of MnO₄- and stoichiometry, the moles of Fe²+

were able to be calculated. This value was then multiplied by the molar mass Fe²+ to get the mass

of Fe²+ in grams.

Table 8. Analyzation of CareOne Iron Pills Lot # 6HN1825 From Two Experiments

Trial Mass % Fe in Sample Mass (mg) Fe % Error

1 16.65 63.90 1.770

2 17.10 65.60 0.880

3 18.54 76.20 17.27

4 14.29 58.80 9.54

Average 66.10 7.36

Standard Deviation ± 7.3

Table 8 (page 11) used the previously calculated values to determine the mass of Fe²+ in

CareOne iron pills. This was done by finding the percent of Fe²+ in the iron pills. To do this, the
 Bassani 12

mass of Fe²+ calculated in Table 7 (page 11) was divided by the mass of the iron pill calculated

in Table 5 (page 10). This value was then multiplied by one hundred. Then the average mass of

one iron pill that was calculated in Table 4 (page 9) was multiplied by the percent of Fe²+ in the

sample. This value was the mass of Fe²+ in the iron pills, in grams. By multiplying this value by

1000 mg, the mass of Fe²+ in CareOne iron pills was determined. To compare this to the printed

value, the percent error was determined. The calculated mass of Fe²+ in mg was subtracted from

the printed value, and then divided by the printed value. This number was then multiplied by one

hundred.

Calculations

Table 1: Determining Mass of (Fe(NH₄)₂(SO₄)₂・6H₂O) in Erlenmeyer Flasks

Mass of flask 1 with FAS - Mass of flask 1 = mass of FAS

75.147 g - 74.681 g = 0.466 g FAS

Table 2: Determining Titrant Delivered for KMnO₄ Standardization

Volume of KMnO₄ in buret after titration for flask 1 - initial volume = volume of titrant

delivered

25.19 mL - 0.00 mL = 25.19 mL

 Bassani 13

Table 3: Determining [MnO₄-]

1 𝑚𝑚𝑚
Mass of FAS in flask 1 x 𝑚𝑚𝑚𝑚𝑚 𝑚𝑚𝑚𝑚 𝑚𝑚(𝑚𝑚₄)₂(𝑚𝑚₄)₂・6𝑚₂𝑚= moles FAS

1 𝑚𝑚𝑚
0.466 g FAS x 392.16𝑚= 0.00119 mols FAS

1 𝑚𝑚𝑚 𝑚𝑚(𝑚𝑚₄)₂(𝑚𝑚₄)₂・6𝑚₂𝑚
Moles of FAS x 1 = moles Fe²+
1 𝑚𝑚𝑚 𝑚𝑚²+

1 𝑚𝑚𝑚 𝑚𝑚(𝑚𝑚₄)₂(𝑚𝑚₄)₂・6𝑚₂𝑚
0.00119 moles FAS x = 0.00119 moles Fe²+
1 𝑚𝑚𝑚 𝑚𝑚²+

1 𝑚𝑚𝑚 𝑚𝑚𝑚𝑚₄
Moles of Fe²+ x 5 𝑚𝑚𝑚𝑚𝑚 𝑚𝑚²+= moles KMnO₄ (Refer to Equation 3)

1 𝑚𝑚𝑚 𝑚𝑚𝑚𝑚₄
0.00119 moles Fe²+ x 5 𝑚𝑚𝑚𝑚𝑚 𝑚𝑚²+= 2.38 x 10-4 moles KMnO₄

1 𝑚𝑚𝑚 𝑚𝑚𝑚𝑚₄
Moles KMnO₄ x 1 𝑚𝑚𝑚 𝑚𝑚𝑚₄− = moles MnO₄- (Refer to Equation 3)

1 𝑚𝑚𝑚 𝑚𝑚𝑚𝑚₄
2.38 x 10-4 moles KMnO₄ x 1 𝑚𝑚𝑚 𝑚𝑚𝑚₄− = 2.38 x 10-4 moles MnO₄-

1 𝑚𝑚𝑚
Moles of MnO₄- x 𝑚𝑚𝑚𝑚𝑚𝑚 𝑚𝑚 𝑚𝑚𝑚𝑚𝑚𝑚𝑚 𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚 = [MnO₄-]

1 𝑚𝑚𝑚
2.38 x 10-4 moles MnO₄- x 0.02519 𝑚 = 0.00943 M MnO₄-

𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚 𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚 𝑚𝑚𝑚 𝑚𝑚𝑚𝑚𝑚 1 + 𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚 𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚 𝑚𝑚𝑚 𝑚𝑚𝑚𝑚𝑚 2 + 𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚 𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚 𝑚𝑚𝑚 𝑚𝑚
3
= average molarity

0.00943 𝑚 + 0.00978 𝑚 + 0.00955 𝑚

= 0.00959 M MnO₄-
3

Table 4: Determining Average Mass of Iron Pill

𝑚𝑚𝑚𝑚 𝑚𝑚 10 𝑚𝑚𝑚𝑚 𝑚𝑚𝑚𝑚𝑚

= Average mass of one iron pill
10

3.835 𝑚
=0.3835 g
10
 Bassani 14

Table 5: Determining the Mass of Fe²+ in Erlenmeyer Flasks

Mass of flask 1 with Fe²+ - Mass of flask 1 = mass of Fe²+

74.756 g - 75.105 g = 0.349 g

Table 6: Determining Titrant Delivered for Analysis of Iron Pill

Volume of KMnO₄ in buret after titration for flask 1 - initial volume = volume of titrant

delivered

21.70 mL - 0.00 mL = 21.70 mL

Table 7: Determining the Mass of Fe²+ in Sample

𝑚𝑚𝑚𝑚𝑚 𝑚𝑚 𝑚𝑚𝑚𝑚₄
Volume of KMnO₄ delivered in trial 1 in liters x = moles of KMnO₄
𝑚𝑚𝑚𝑚𝑚

0.00959 𝑚𝑚𝑚𝑚𝑚
0.02170 L x = 2.08 x 10-4 moles KMnO₄
𝑚𝑚𝑚𝑚𝑚

1 𝑚𝑚𝑚 𝑚𝑚𝑚𝑚₄
Moles KMnO₄ x 1 𝑚𝑚𝑚 𝑚𝑚𝑚₄− = moles MnO₄- (Refer to Equation 3)

1 𝑚𝑚𝑚 𝑚𝑚𝑚𝑚₄
2.08 x 10-4 moles KMnO₄ x 1 𝑚𝑚𝑚 𝑚𝑚𝑚₄− = 2.08 x 10-4 moles MnO₄-

5 𝑚𝑚𝑚𝑚𝑚 𝑚𝑚²+
Moles of MnO₄- x = moles of Fe²+ (Refer to Equation 3)
1 𝑚𝑚𝑚 𝑚𝑚𝑚₄−

5 𝑚𝑚𝑚𝑚𝑚 𝑚𝑚²𝑚
2.08 x 10-4 moles MnO₄- x = 0.00104 moles Fe²+
1 𝑚𝑚𝑚 𝑚𝑚𝑚₄−

𝑚𝑚𝑚𝑚𝑚 𝑚𝑚𝑚𝑚 𝑚𝑚 𝑚𝑚²+

Moles of Fe²+ x = mass of Fe²+ in sample (Refer to Equation 3)
1 𝑚𝑚𝑚

55.85 𝑚
0.00104 moles Fe²+ x = 0.0581 g Fe²+ in sample
1 𝑚𝑚𝑚
 Bassani 15

Table 8: Determining Mass of Fe²+ in CareOne Iron Pills and Percent Error from Printed Label

𝑚𝑚𝑚𝑚 𝑚𝑚 𝑚𝑚²+ 𝑚𝑚 𝑚𝑚𝑚𝑚𝑚𝑚

x 100 = Percent Fe²+ in sample
𝑚𝑚𝑚𝑚 𝑚𝑚 𝑚𝑚²+ 𝑚𝑚 𝑚𝑚𝑚𝑚𝑚 1

0.0581 𝑚
x 100 = 16.65% Fe²+ in sample
0.0349 𝑚

Percent Fe²+ in sample x average mass one of iron pill = mass of Fe²+ in one iron pill in grams

0.1665 (0.3835 g) = 0.0639 g Fe²+ in one iron pill

1000 𝑚𝑚
mass of Fe²+ in one iron pill in grams x = mass of Fe²+ in one iron pill in milligrams
1𝑚

1000 𝑚𝑚
0.0639 g x = 63.85 mg Fe²+ in one iron pill
1𝑚

|𝑚𝑚𝑚𝑚𝑚𝑚𝑚 𝑚𝑚²+ 𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚 𝑚𝑚 𝑚𝑚𝑚𝑚𝑚𝑚𝑚 𝑚𝑚𝑚𝑚 𝑚𝑚𝑚𝑚 − 𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚 𝑚𝑚𝑚𝑚𝑚 |

x 100 =
𝑚𝑚𝑚𝑚𝑚𝑚𝑚 𝑚𝑚²𝑚 𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚

percent error

|65 𝑚𝑚 − 63.85 𝑚𝑚 |
x 100 = 1.770% error
65 𝑚𝑚

Discussion

The results from the lab procedure fully support the hypothesis, since the amount of iron

in a CareOne pill was on average 66.1mg, ±7.3mg, a 7.36% error from the printed value on the

bottle of 65 mg.

In order to determine the exact concentration of the KMnO₄, a titration had to occur

between Fe(NH₄)₂(SO₄)₂・6H₂O (FAS) and KMnO₄ (5Fe²+ + 8H+ + MnO₄- ⟶5Fe³+ + Mn²+ +

4H₂O). This is so the KMnO₄ could be standardized, and the concentration of the MnO₄- ion
 Bassani 16

could be calculated. This was important because the concentration of KMnO₄ was approximately

0.01 M, and it needed to be titrated with the iron pills to determine the Fe²+ concentration in

FeSO4. By standardizing the KMnO₄ with the FAS first, the concentration was known more

precisely in the redox titration with the FeSO4. Since MnO₄- was used to determine the moles

reacted of Fe²+, it was better to know exactly its concentration. The Fe²+ concentration was then

the unknown value, and could be calculated using the known volume delivered of KMnO₄ which

had a known concentration.

It was expected that once the equivalence point of the reaction was reached, a light purple

color would be observed in the Erlenmeyer flask. However, Anne Marie Helmenstine, Ph.D.

describes how “the equivalence point is not the same as the endpoint of a titration”

(Helmenstine). Instead, it is where the number of electrons in the oxidation half reaction equal

the number of electrons gained in the reduction half reaction. The endpoint of the reaction “refers

to the point at which an indicator changes color” which was not observed in this redox titration

(Helmenstine). The color change that occured in this reaction (5Fe²+ + 8H+ + MnO₄- ⟶5Fe³+ +

Mn²+ + 4H₂O), was because “oxidation states have different colors” (Helmenstine). It was

expected that the color change would occur faintly when the reaction reached its equivalence

point, and linger for at least five seconds. This is because the electron exchange was equal

between the Fe²+ and the MnO₄-.

Even though the experimentally calculated mass of Fe²+ in the iron pills was 66.1 mg,

which is 1.1 mg higher than the printed value of 65 mg, the experiment was valid. Three trials

were performed to standardize the KMnO₄ which allowed for the average [KMnO₄] to be

calculated. Since the concentration of KMnO₄ was approximately 0.01 M, the exact

concentration was calculated to be 0.00959 M, which was a more precise value. This was able to
 Bassani 17

be determined once the reaction reached the equivalence point and a color change occurred for at

least five seconds. Because the titrant was not longer delivered once the equivalence point was

reached, over titration did not occur allowing for an accurate measurement to be taken. With the

exact KMnO₄ concentration being a known, a total of four trials were performed to get an

average Fe²+ mass of 66.1 mg. The standard deviation for all four trials was 7.3, and the percent

error was 7.36%. Because four trials were performed, the data was able to be compared to see if

the experimentally calculated values were consistent with the labeling on the iron pill bottle.

In order “to ensure that label values will have a high probability of being in compliance

with nutrition labeling regulations and accurately represent the nutrient content of food products,

FDA recommends the calculation of a one-sided 95% prediction interval” (Center for Food

Safety and Applied Nutrition). This means that 95% of the time the Fe²+ concentration is

calculated, it would have to be within 5% of the printed value. This means the iron pills could

contain either 2.5% higher or lower of 65 mg. 2.5% of 65 mg is 1.63, so the experimentally

calculated Fe²+ mass can be 1.63 mg higher or lower than 65 mg, and still be considered

accurate. The range of acceptable values is 63.37-66.63 mg. Since the experimentally calculated

Fe²+ mass was 66.1 mg, the CareOne labeling is accurate.

Iron is an crucial mineral for the body, and it is important for hemoglobin found in red

blood cells. This is because hemoglobin is responsible for delivering oxygen throughout the

body. However many people are iron deficient and do not get enough of this mineral in their diet.

This causes them to take iron supplements, such as the CareOne iron pills that were analyzed in

this lab. However, even though it is “an essential mineral...iron is so toxic that its absorption

from the digestive tract is tightly controlled” (Arnarson). Atli Arnarson, Ph. D. describes how

“many serious health problems may be caused by accidental overdoses, taking high-dose
 Bassani 18

supplements for a long time, or chronic iron overload disorders” (Arnarson). This is a result of

there being too high levels of free iron in the body, which acts as a “prooxidant… and may cause

damage to cells” (Arnarson). Additionally, “excess iron accumulates in internal organs, causing

potential fatal damage to the brain and liver” (Arnarson). As a result, a person should only take

iron supplements when they are prescribed to by their doctor. It is also important that people do

not take more than they are supposed to.

From analyzing CareOne iron pills, the calculated mass of Fe²+ supplied by FeSO4 was

able to be compared to the printed label of 65 mg. It was expected that the label was correct,

since

taking too much iron can be detrimental to the body. The Food and Drug Administration also

created a Small Entity Compliance Guide that was in accordance with the Small Business

Regulatory Enforcement Fairness Act. This guide states the legal requirements of dietary

supplements which “require[s] label warning statements for iron-containing dietary supplements

and drug products” (Center for Food Safety and Applied Nutrition). Since the FDA realizes the

potential risk iron supplements can have on the body, the amount of Fe²+ in the pills should be

consist with the printed label. If the Fe²+ mass in CareOne iron pills was more or less than the

printed 65 mg, the warning labels would be insufficient. This would go against the Small

Business Regulatory Enforcement Fairness Act that was created to protect consumers.

Additionally, the Fair Packaging and Labeling Act was created in 1967 to allow the

Federal Trade Commission and Food and Drug Administration to regulate commodities

purchased by consumers. This includes the labeling of “net contents, identity of commodity, and

name and place of business of the product’s manufacturer, packer, or distributor” (Federal Trade

Commission). The Federal Drug Administration also has the authorization for further regulation
 Bassani 19

“to prevent consumer deception… with respect to ingredients, slack of filling packages, use of

‘cents-off’ or lower price labeling, or characterization of package sizes” (Federal Trade

Commission). With these regulations in place, the consumer is given many protections against

inaccurate labelings. However, if the labeling is incorrect, the Federal Drug Administration “may

inform the manufacturer, often in the form of a warning letter, of the violation of law and ask the

firm to correct the problem” (U.S. Food and Drug Administration). The Federal Drug

Administration can take “additional legal action to remove the misbranded products from

commerce” if the problem is not fixed (U.S. Food and Drug Administration). With such heavy

regulations for dietary supplements in place, it was expected that the CareOne company would

ensure the accuracy of their product.

Conclusion

From this lab, redox titration was able to be used to determine the mass of Fe²ᐩ in

CareOne iron pills. This was first done by standardizing the KMnO₄ with Fe(NH₄)₂(SO₄)₂・6H₂O

(FAS) to determine its concentration in three trials. Since the mass of FAS in the Erlenmeyer

flask was a known value, the concentration of KMnO₄ was able to be determined. Once the

equivalence point of the reaction was reached, enough titrant was delivered to make the electron

exchange equal between the oxidation half-reaction and the reduction half-reaction. This was

represented by a color change in the Erlenmeyer flask, which lasted for at least five seconds. By

calculating the [KMnO₄] to an average of 0.00959 M, another two trials were able to be done to

determine the Fe²+ mass in iron pills (5Fe²+ + 8H+ + MnO₄- ⟶5Fe³+ + Mn²+ + 4H₂O). This was

done by another redox titration, since the mass of the iron pill in the Erlenmeyer flask was a

known value along with the [KMnO₄]. The concentration of Fe²+ in CareOne iron pills was
 Bassani 20

calculated by averaging the values of two different experiments, which equaled four trials. The

Fe²ᐩ mass in CareOne iron pills was determined to be 66.1 mg, which is a 7.36% error from the

printed 65 mg. This was expected since the Federal Drug Administration regulates the labels for

dietary supplements. Also, three trials were performed to standardize the KMnO₄, and four trials

were used to calculate the concentration of Fe²+ in the iron pills, making the experiment valid.

The experimentally calculated concentration of Fe²+ also fits within the 95% prediction interval,

since the Fe²+ mass in the supplements can be anywhere from 63.37-66.63 mg. Since the

calculated Fe²+ concentration was 66.1 mg, the experimentally calculated concentration of Fe²+ in

CareOne iron pills proves that the label is accurate.

 Bassani 21

Works Cited

Arnarson, Atli. “The Dark Side of Iron - Why Too Much Is Harmful.” Healthline, Healthline

Media, 4 Jan. 2017, www.healthline.com/nutrition/why-too-much-iron-is-

harmful#section2.

Center for Food Safety and Applied Nutrition. “Dietary Supplements - Guidance for Industry:

Iron-Containing Supplements and Drugs: Label Warning Statements; Small Entity

Compliance Guide.” U S Food and Drug Administration Home Page, Center for Food

Safety and Applied Nutrition,

www.fda.gov/Food/GuidanceRegulation/GuidanceDocumentsRegulatoryInformation/Die

tarySupplements/ucm073014.htm.

Center for Food Safety and Applied Nutrition. “Labeling & Nutrition - Guidance for Industry:

Nutrition Labeling Manual - A Guide for Developing and Using Data Bases.” U S Food

and Drug Administration Home Page, Center for Food Safety and Applied Nutrition,

www.fda.gov/Food/GuidanceRegulation/GuidanceDocumentsRegulatoryInformation/Lab

elingNutrition/ucm063113.htm#stat_5.

Consumer Healthcare Products Association. “FAQs About Dietary Supplements Regulations.”

FAQs About Dietary Supplements Regulations,

www.chpa.org/FAQsDS.aspx#containlabeling.

Federal Trade Commission. “Fair Packaging and Labeling Act.” Federal Trade Commission, 16

Feb. 2018, www.ftc.gov/enforcement/rules/rulemaking-regulatory-reform-

proceedings/fair-packaging-labeling-act.
 Bassani 22

Helmenstine, Anne Marie. “Here's What the Equivalence Point Means in

Chemistry.”ThoughtCo, 8 Mar. 2017, www.thoughtco.com/definition-of-equivalence-

point-605101.

National Institutes of Health. “Dietary Supplements: What You Need to Know.” NIH Office of

Dietary Supplements, U.S. Department of Health and Human Services, 17 June 2011,

ods.od.nih.gov/HealthInformation/DS_WhatYouNeedToKnow.aspx.

Nazarenko, Alexander. Redox Titrations. Potassium Permanganate. .

staff.buffalostate.edu/nazareay/che112/manganate.htm.

U.S. Food and Drug Administration. “Consumer Updates - FDA: Foods Must Contain What

Label Says.” U S Food and Drug Administration Home Page, Office of the

Commissioner, 28 Feb. 2018,

www.fda.gov/ForConsumers/ConsumerUpdates/ucm337628.htm.

Watson, Stephanie. “What You Need to Know About Iron Supplements.” WebMD, WebMD,

www.webmd.com/vitamins-and-supplements/features/iron-supplements#1.

WedMD. “Understanding Anemia -- the Basics.” WebMD, WebMD, www.webmd.com/a-to-z-

guides/understanding-anemia-basics#1.