Experiment 3 Titration of Mixed Alkali

Objectives Prepare a standard hydrochloric acid solution. Determine the carbonate and bicarbonate content in a given sample.

Introduction

Alkalimetry Specialized analytic use of acid-base titration to determine the concentration of a base

Determination of Carbonate and Bicarbonate Mixtures

o CO32-, HCO3- and OH- can be titrated with a strong acid in many combinations with conditions: 1. HCO3- and OH- cannot coexist in solution since they react HCO3- + OH- -> CO32- + H2O

Determination of Carbonate and Bicarbonate Mixtures

2. No more than two of these three constituents can exist in any solution because one of the present species will react with another, resulting in CO32- and whatever is in excess in the solution.

Determination of Carbonate and Bicarbonate Mixtures

There are 5 possible combinations:
1. 2. 3. 4. 5. NaOH Na2CO3 NaHCO3 Na2CO3 + NaOH Na2CO3 + NaHCO3

Standardization of HCl

Table 1. Weight of Na2CO3 and volume of HCl used for the standardization of the HCl

Trial 1 2 3 4 Mean Computation:

Weight of Na2CO3 (g)

0.2586 0.3431 0.2001 0.2020 -

Volume of HCl (L)

0.0469 0.0593 0.0375 0.0352 -

Molarity of HCl 0.1040 0.1092 0.1007 0.1083 0.1056

Analysis of Unknown

Table 2. Volume of HCl used to reach phenolphthalein end point

Trial 1 2 3 Mean

Volume of HCl (L) Phenolphthalein end pt. 0.0190 0.0177 0.0222 0.0196

Computation:

Table 3. Volume of HCl used to reach bromocresol green end point

Trial

Volume of HCl (L) Bromocresol Green end pt. 0.0229 0.0218 0.0237 0.0228

Computation:

1 2 3 Mean

Table 3. Volume of HCl used to reach bromocresol green end point

Trial

Volume of HCl (L) Bromocresol Green end pt. 0.0229 0.0218 0.0237 0.0228

Computation:

1 2 3 Mean

Question

Why did we use phenolphthalein and bromocresol green as indicators?

Question
Do we really need to cool down the solution after boiling?

Question
What's the reason behind boiling the solution after the first equivalence point?

Question
What will happen if we do not use CO2- free distilled water?

Question
Is the ice bath important?

Discussion

Carbonate, bicarbonate, and hydroxide constitute a carbonate mixture but a maximum of two can only exist at the same time as the other one will be consumed completely

Table 4. Five possible combinations of sample

Constituen(s) in sample NaOH Na2CO3 NaHCO3 NaOH + Na2CO3

Volumes of Titrant V0->phth = V0->bcg > 0 V0->phth = Vphth->bcg V0->phth = 0 ; Vphth->bcg > 0 V0->phth > Vphth->bcg

Na2CO3 + NaHCO3

V0->phth < Vphth->bcg

Figure 1. Titration curve when sample is only NaOH

Figure 2. Titration curve when sample is only Na2CO3

Figure 3. Titration curve when sample is only NaHCO3

Figure 4. Titration curve when sample is NaOH and Na2CO3

Figure 5. Titration curve when sample is Na2CO3 and NaHCO3

Conclusion

Alkalimetry is the determination of the quantity of real alkaline in alkali solutions or salts, either through gravimetric or volumetric analysis. Observe proper laboratory procedures and techniques

Brown, T., Lemay, E. & Bursten, B. (2003). Chemistry: The central science 9th ed. Singapore: Pearson Education, Inc. Chang, R. (2005). Chemistry 8th ed. Singapore: McGraw Hill Inc.

Hargis, L. G. (1988). Analytical chemistry: principles and techniques. NJ, USA: Prentice Hall.
Skoog, D., West, D., Holler, J. & Crouch, S. (2010).

Fundamentals of analytical chemistry 8th ed.

Philippines: Cengage Learning Asia Pte Ltd.

Fin