Date: 3/4/2015

Acid Base Lab

Determination of CaCO​ in Toothpaste
3​
Supakij Sirivech 1104
Yoskorn Mongkolsuk 1104
Pravit Akarapanont 1104
Nam Vanichchai 1104

Introduction
Calcium Carbonate is an abrasive widely used in the production of toothpaste, specialty
10
dentifrices, and oral products.​ The majority of abrasives consisted in toothpaste is not harmful
to enamel, however, it can damage tooth enamel if too much amount of it is used frequently.
Since Calcium Carbonate contains a power of cleaning – most of its usage is to remove tough
stains such as coffee, tea, and soft drinks in oral cavity – its excessive abrasive can also lead to
discoloration and sensitivity of tooth depending on the length of time and the pressure used
11
when brushing teeth.​ That being said, its amount for usage therefore becomes significant for
the consumers, and one of the methods to measure Calcium Carbonate in toothpaste in back
titration.
Back titration is a method of chemical measurement used to determine the quantity of
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an identified analyte by reacting it with an identified amount of excess reactant (acid).​ The
second reactant (base) will be added to the remaining of the first reactant, and that leftover
will be titrated with the second reactant. This will result the amount of the excess reactant
used, which also will reveal the analyte's volume. In addition to this, back titration is commonly
used because it always gives an exact quantity of reactant and a precise endpoint of a reaction.
In order to get accuracy and precision of results, a burette, an indicator, pH meter, and 2
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reactants (normally acid and base) are used to conduct the experiment.​
In this experiment, back titration is applied to measure the quantity of Calcium
Carbonate because it is insoluble in water, thus a normal titration would not be effective. This
experiment, however, only inquired the approximate percentage of Calcium Carbonate in the
9 Darlie Shiny White
toothpaste. Toothpaste​ was an analyte containing Calcium Carbonate,
Hydrochloric (strong acid) and Sodium Hydroxide (strong base) played an important role as
reactants. Additionally, three replicates of this experiment were performed to ensure the
closest percentage of Calcium Carbonate contained in toothpaste.

Purpose
To measure the amount of Calcium Carbonate​
in
​ toothpaste by back titration.
Hypothesis
We predict that the toothpaste contains a high amount of Calcium Carbonate according
to its special characteristic to whiten the teeth. Moreover, the color of solution composed of an
indicator and HCl (acid) will turn into pink, and its pH will be approximately 7-9.

Material
1) Toothpaste
2) Three of 125 mL Erlenmeyer flasks
3) Spatula
4) Stand with double burette holder
5) Buret
6) Stir bar
7) pH meter
8) Graduated cylinder
9) Pipette
10) Heater

Procedure
1. Put 125 mL Erlenmeyer on scale, zero scale
2. Weigh out about 0.50g of toothpaste, using spatula, directly into 125mL Erlenmeyer
flask. Record value weighted.
3. Using a 10 mL graduated cylinder, add 10 mL of distilled water to the toothpaste.
4. Using a 10 mL volumetric pipette exactly 10 mL of 0.10M HCl into toothpaste/water
solution.
5. Add a stir bar, heat and stir for 5 minutes on hot plate -> remove from heat and let cool
to the touch.
6. Add a few drops of Phenolphthalein indicator.
7. Start adding your titrant (0.10 M NaOH in buret) slowly -> check the pH after every 1 mL
of titrant added. Record both the volume and pH. When solution starts to turn pink but
return to transparent, clear after swirling, add slower (drop-wise perhaps)
8. After end point has been reached, record the final pH and final volume.
9. Continue adding titrant, an additional 4 mL of titrant. Again checking the pH after every
1 mL has been added. Record the pH and volume each time.
10. Repeat experiment 2 more times. This will give a total of 3 separate titrations.
11. Dispose of your waste in large beaker provided, do not dispose of down the drain. Leave
leftover NaOH solution in buret after use.
Results
Table 1
Sample 1 Sample 2

Weight(g) 0.70 g 0.53 g

Initial pH 2.53 2.21

Initial volume (mL) 6.41 13.43

Final volume 10.78 17.07

Final pH 8.909 8.87

Total volume 4.37 3.64

Volume HCL reacted with 5.63 6.36

toothpaste
-4 -4
Moles HCl reacted 4.37 x 10​ 6.36 x 10​
-4 -4
Moles CaCO​
3 2.19 x 10​ 3.18 x 10​

Amount of CaCO​
3 (mg)
​ 21.92 mg 31.83 mg

Amount CaCO​(mg/g)*
3​ 31.31 mg/g 60.06 mg/g

Average CaCO​
3(mg/g)
​ 49.63 mg/g 49.63 mg/g

Table 2
Sample 3

Weight(g) 0.56 g

Initial pH 2.37

Initial volume (mL) 17.49 mL

pH #1 2.69(18.40 mL)

pH #2 5.47(19.48 mL)

pH #3 7.32(20.41 mL)

pH #4 8.61(21.05 mL) Pink

pH #5 10.22(22.01 mL)

pH #6 10.91(22.95 mL)

pH #7 11.21(23.92 mL)

pH #8 11.37(24.95 mL)

pH #9 11.51(25.9 mL)

Final volume 21.05 mL

Final pH 8.61

Total volume 3.56 mL

Volume HCL reacted with 6.44 mL

toothpaste
-4​
Moles HCl reacted 6.44 x 10​ mL
-4 ​
Moles CaCO​ 3.22 x 10​ mL
3

Amount of CaCO​ 32.22 mg

3 (mg)
​

Amount CaCO​(mg/g)* 57.53 mg/g

3​

Average CaCO​ 49.63 mg/g

3(mg/g)
​
pH graph

Average CaCO​
3

Total numbers: 3

Mean value: 49.6333333333

Sample standard 15.9188138168

deviation:

Relative standard 32.07%

deviation:

Observation
As we added more Sodium Hydroxide into the solution in order to observe its end point,
the solution was turning more pink, demonstrating that it was becoming more basic and the pH
was increasing. Each drop of Sodium Hydroxide turned the solution to more pink as we swirled
the flask, however, the solution turned to be clear again after we left it for awhile. Eventually,
we needed to add 3.86 mL Sodium Hydroxide thus the solution would not turn back to
transparent white again.
From the experiment, some errors that occurred impacted our results. First, the weight
of sample 1 is 0.70 g. than the other two samples, the amount of Calcium Carbonate of it
should be more than those two. However, the amount of Calcium Carbonate measured in
sample (2 and 3 are 31.83 mg and 32.22 mg. but the amount of it found in sample (1) is 21.92
mg. We believe that this mistake is caused by the misestimation of Sodium Hydroxide’ s
amount put in the solution. To illustrate, we estimated the color change by our eyes which
impacted the result to be inaccurate.

Discussions
Back titration is a quantitative chemical analysis method that requires a lot of
procedures and thorough experiment. The significant procedures for the titration is heating the
solution, adding acid and base in it, and measuring pH of the solution.
The purpose of heating the solution was to remove Carbon Dioxide ​ out of the solution
8
in order to only concentrate on Calcium Carbonate.​Also, to increase the rate of activity
because the heat would increase kinetic energy, and made the Calcium Carbonate and
1​
Hydrochloric collide more frequently.​ The solution would therefore mix better.
The next procedure is adding acid and base into the solution. The acid was added
because we used titration method to find average of Calcium Carbonate by excess of
Hydrochloric (acid). First, we mixed Hydrochloric with toothpaste. Some of Hydrochloric
reacted with toothpaste and some remained Hydrochloric. After that we added Sodium
Hydroxide (base) to titrate with the remaining Hydrochloric, the amount of Sodium Hydroxide
that we added was equal to amount of the remaining Hydrochloric according to chemical
formula. In the end, were able to determine the amount of Calcium Carbonate by minus the
amount of Sodium Hydroxide that is equal to the amount of Hydrochloric reacting with the
toothpaste, with Hydrochloric that we put at first ( 10 mL).
The other important process we needed to observe is an end point. It occurred when
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the solution’s color changed from transparent white into pink as the flask was stirred.​
3​
Furthermore, equivalence point is when two solutions were added at exact same amount​ .
These two points are closely related. Based on our experiment, they were same when 3.86 of
Sodium Hydroxide was added (Sample standard deviation of 0.45 and Relative standard
deviation of 11.57%) because we observed the equivalence based on the end point.
During the experiment, we were able to observe the end point when the solution in a
2
flask turned pink.​ Since the indicator, Phenolphthalein, was added into the solution before, it
2
would indicate the solution to be either basic or acidic when the solution’s color changed.​ Base
on our experiment, the solution’s color changed to pink at a pH of 8.79 that is in the given
range. (Sample standard deviation of 0.16 and Relative standard deviation of 1.81%)
In order to get the most precise average of Calcium Carbonate the experiment needed
to be repeated for accuracy and precision of results. ​ There could be some misconducts in our
experiment that would alter the data. Replications guaranteed the precise average of all three
–​
results​ if all results are in the same range ​we can ensure that the final result would be explicit.
Conclusion
In this experiment, we learned about the concept of bark titration through the
measurement of Calcium Carbonate in toothpaste. We were able to understand the reaction of
the analyte (CaCO​ 3)​and other two reactants (HCl and NaOH) through the back titration, as well
as were able to determine the amount of Calcium Carbonate in toothpaste. According to our
hypothesis, we predicted that the toothpaste contains a high amount of Calcium Carbonate,
and the solution’s color will turn into pink as its pH increases up to 7-9. The results from the
experiment, however, did not support our hypothesis because the concentration of Calcium
Carbonate in this toothpaste is only 0.049% while toothpaste generally contains 20% as an
abrasive (Loos n.d.; Evans n.d.)
Nevertheless, our misconducts during the experiment may lead us to the alternative
results. For instance, the amount of toothpaste in sample (1) was approximately 0.20 g. more
than the other two, and its volume after heated was also more than those samples’. This could
affect its final quantity of Calcium Carbonate to be the largest which. Throughout the
experiment, however, there were a lot of procedures that needed humans to conduct the
experiment, thus errors could easily occur such as when measuring the toothpaste, measuring
Sodium Hydroxide by an eyesight, and swirling the solution with Sodium Hydroxide.
In the future, we can further improve this experiment by using more effective
measuring tools in order to get more accurate and precise results. In addition to this, instead of
determining the average, we will be able to get the exact amount of Calcium Carbonate
contained in toothpaste.
uiReference:

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 ​
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