CHEM 121L

General Chemistry Laboratory

Revision 2.1

An Analysis of Sodium Bicarbonate

In last weeks laboratory, we synthesized Sodium Bicarbonate (NaHCO3) from Sodium Chloride
(NaCl) via the old Solvay Process.
NaCl(aq) + NH3(aq) + CO2(s) + H2O

NH4Cl(aq) + NaHCO3(s)

(Eq. 1)

A common side-reaction that occurs during the heating of the Bicarbonate to drive off
Ammonium Chloride (NH4Cl) is the conversion of some of the Bicarbonate to Sodium
Carbonate (Na2CO3):
2 NaHCO3(s)

Na2CO3(s) + CO2(g) + H2O(g)

(Eq. 2)

Thus, we wish to analyze our product to determine the percentage Sodium Bicarbonate and
Sodium Carbonate it contains.

Sodium Bicarbonate

Sodium Carbonate

We will use a form of Volumetric Analysis called Titrimetry to analyze our product for these
percentages. A volumetric analysis involves measuring the volume of a solution of known
concentration, the Titrant, which is needed to completely react with an Analyte; Sodium
Bicarbonate and Sodium Carbonate, in the present case. This titration reaction is complete when
a stoichiometrically equivalent amount of titrant has been added to the analyte and all the analyte
has been consumed. The point at which this occurs, called the Endpoint, is visually noted
because an added Indicator changes color, or has some other distinct visual change, when the

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titration reaction is complete. The trick in any titration is to stop adding titrant at the exact point
at which the indicator's color changes because only at this point will a stoichiometrically correct
amount of titrant have been added to the analyte.

A Buret is the volume measuring device used to deliver the titrant into the analyte Solution.

A Graduated 50 mL Burette
(http://en.wikipedia.org/wiki/File:Burette_vertical.svg)

This device is constructed such that it can be read with a high degree of precision. Accepted
tolerances for burets are listed in the Appendix below.
The amount (moles) of analyte present can be calculated from the volume of titrant added to
reach the endopoint via:
# moles Analyte = (Stoich. Ratio) x MTitrant x (Vf - Vi)

(Eq. 3)

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Here, (Stoich. Ratio) refers to the reaction stoichiometry between the Titrant and the Analyte in
the titration reaction. Once the number of moles of Analyte has been determined, its mass can
then be calculated using its molecular weight.
In our case, we have two analytes in our sample; Sodium Bicarbonate and Sodium Carbonate.
Both of these Sodium salts are water soluble and ionize upon solvation in Water:
NaHCO3(aq)

Na+(aq) + HCO3-(aq)

(Eq. 4)

Na2CO3(aq)

2 Na+(aq) + CO32-(aq)

(Eq. 5)

The resulting Bicarbonate (HCO3-) and Carbonate (CO32-) ions are both basic. Hence, they will
react with a strong acid such as Hydrochloric Acid (HCl), which itself ionizes to H+(aq) and Cl(aq) in Water.
CO32-(aq) + H+(aq)

HCO3-(aq)

(Eq. 6)

HCO3-(aq) + H+(aq)

H2CO3(aq)

(Eq. 7)

Therefore, an acid such as HCl can serve as the titrant for our titration.

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Because we have two analytes, HCO3- and CO32-, we will need two different indicators, one to
indicate the endpoint for the reaction between H+ and CO32- and the other to indicate the
endpoint for the reaction between H+ and HCO3-. The indicator Phenolphthalein will serve as an
endpoint indicator for the former reaction and Bromcresol Green will indicate the endpoint for
the latter.
We will add acid to a solution of our sample until the acid completely reacts with the Carbonate
(CO32-) present to form Bicarbonate (HCO3-). The number moles Carbonate present can be
determined from the Volume and Molarity of the acid added:
# moles CO32- = (1 mole CO32-/1 mole H+) x MHCl x VHCl(1st EndPt)

(Eq. 8)

The Endpoint of this reaction can be detected because the Acid-Base Indicator Phenolphthalein
will change color from Pink to Clear at the pH prevailing when this reaction is complete. After
this endpoint is reached, the acid will begin reacting with the Bicarbonate just generated and the
Bicarbonate present in the initial sample. And, again, knowing the Volume and Molarity of the
added acid, we can determine the number moles Bicarbonate:
# moles HCO3- Total = (1 mole HCO3-/1 mole H+) x MHCl x VHCl(1st to 2nd EndPt)
(Eq. 9)

The Endpoint of this reaction can be detected by using the Acid-Base Indicator Bromocresol
Green; which changes from Blue to Yellow at the pH that prevails at the completion of this
reaction. The amount of Bicarbonate present in the original sample will then be the difference
between the total Bicarbonate determined above and the amount generated by the Carbonate
initially present. Thus, the amount of Bicarbonate originally present in our sample is given by:
# mole HCO3- Original = # moles HCO3- Total - # moles CO32-

(Eq. 10)

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This entire procedure depends on knowing the concentration of the acid used as the titrant. We
will determine this concentration using a Standardization procedure. This involves performing
the same experiment on a sample of Sodium Carbonate of known mass.
CO32-(aq) + 2 H+(aq)

H2CO3(aq)

(Eq. 11)

Then,
# moles HCl = [mass Na2CO3 / MWNa2CO3] x (2 mole HCl/1 mole Na2CO3)
(Eq. 12)

Molarity HCl = # moles HCl / VHCl[L]

(Eq. 13)

Finally, the Carbonic Acid produced as a result of these titrations can decompose into Carbon
Dioxide (CO2):
H2CO3(aq)

CO2(g) + H2O

(Eq. 14)

We can drive our titration reactions to completion by boiling the analyte solution to drive off any
CO2 producded.
So, we will first Standardize our HCl solution against a known mass of Sodium Carbonate. Then
we will determine the percentage Sodium Carbonate in our sample by titrating it with the
standardized acid to a Phenolphthalein endpoint. We will subsequently determine the percentage
Sodium Bicarbonate by titrating the resulting solution to a Bromocresol Green endpoint.

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Pre-Lab Questions
1.

What volume 8M HCl is required to prepare 400 mL of 0.1M HCl?

2.

How many grams of Na2CO3 Standard must be used if the titration is expected to require
40 mL of 0.1M HCl titrant?

3.

If 15 mL of 0.1M HCl titrant is required to reach the Phenolphthalein endpoint and an

additional 25 mL is required for the Bromcresol Green endpoint, what are the percentages
Sodium Carbonate and Sodium Bicarbonate in our original sample? The mass of the
sample used was 0.25g.

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Procedure
Preparation of ~0.1M HCl Solution
1.

Use the 8M HCl provided to prepare 400 mL of ~0.1M HCl. Have your instructor check
your Pre-Lab calculation before you proceed.

Standardization
1.

Set-up a buret to deliver your acid solution. Your instructor will demonstrate how to
use this device. Do not proceed without this instruction.

2.

Fill your buret with the HCl solution. Your instructor will demonstrate this. Make sure
the buret tip is full. Make an initial volume reading to the correct precision; 0.02 mL for
a 50 mL buret.

3.

Weigh a sample of 0.20g Sodium Carbonate to a precision of 0.1mg on glazed weighing

paper. Add this to a 250 mL Erlenmeyer Flask. Add about 25 mL Water and swirl to
dissolve the Carbonate. Add a few drops of Phenolphthalein.

4.

Begin adding the acid to the flask from the buret no faster than 0.5 mL/second. Swirl the
flask constantly. Continue until the pink color disappears. Now add 2-4 drops of
Bromocresol Green (blue at high pH and yellow at low pH). Titrate to a blue-green color,
which appears just before the Endpoint. Interrupt the titration at this point and boil the
solution carefully for two or three minutes to drive off the Carbon Dioxide. This helps
drive the reaction to completion. The color should revert to blue. Cool the solution to Room
Temperature (~10 minutes) and continue the addition of acid to the pale green Endpoint.
Make a volume reading at this point.

5.

Repeat this procedure twice more.

Analysis of Sample
1.

Weigh a sample of 0.20g Sample to a precision of 0.1mg on glazed weighing paper. Add
this to a 250 mL Erlenmeyer Flask. Add about 25 mL Water and swirl to dissolve the
Carbonate. Add a few drops of Phenolphthalein.

2.

Again fill your buret and make a volume reading.

3.

Add acid until you reach the Phenolphthalein Endpoint. Make a volume reading.

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4.

Add a few drops of Bromocresol Green and finish the addition of acid as before. Make a
volume reading.

5.

Repeat the procedure at least twice more.

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Data Analysis
1.

Determine the Molarity of the HCl solution based on the data for each of the three
Standardization experiments. Report the average value.

2.

Determine the number of moles Sodium Carbonate and Sodium Bicarbonate in each
sample analyzed.

3.

Convert the number of moles of each substance to numbers of grams using the appropriate
molecular weights.

4.

Calculate the Weight Percentage of Sodium Carbonate and Sodium Bicarbonate in each
sample. Report the respective averages.

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Post Lab Questions

1.

Suppose a titration of 0.200g of Sodium Carbonate requires 35.50 mL of HCl. What is the
molarity of the HCl solution?

2.

Suppose the above titration (problem #1) is in error by 0.05 mL; too much. What is the
percentage error introduced into the molarity of the HCl solution?

3.

The indicator Thymol Blue changes color (Blue to Yellow) over the same pH range as
Phenolphthalein. Why is Phenolphthalein a better choice of indicator than Thymol Blue?

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Appendix - Tolerances for Class A Volumetric Burets at 20oC

Capacity (mL)
5
10
25
50
100

Tolerances (mL)
0.01
0.02
0.03
0.05
0.20

With the exception of Graduated Cylinders, the Tolerances for Class B devices is
typically twice that of a Class A device. (ASTM E694)