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Department of Chemical Engineering, College of Engineering University of the Philippines, Diliman, Quezon City, Philippines Date Due: Jan. 16, 2014 Date Submitted: Jan. 16, 2013

RESULTS AND DISCUSSION In this experiment, the purity of soda ash is determined by performing simple and complex acid-base titrations with the help of concepts about strong acid-strong base and strong acid-weak base titration, carbonate titration and double-indicator titration. Volumetric or titrimetric analyses are quantitative analytical techniques which employ a titration in comparing an unknown with a standard. In a titration, a volume of a standardized solution containing a known concentration of reactant "A" is added incrementally to a sample containing an unknown concentration of reactant "B". The titration proceeds until reactant "B" is just consumed (stoichiometric completion). This is known as the equivalence point. At this point the number of equivalents of "A" added to the unknown equals the number of equivalents of "B" originally present in the unknown. Volumetric methods have the potential for a precision of up to 0.1%.1 A double-indicator titration was used for this experiment since the main component of soda ash, sodium carbonate is polyprotic and is neutralized through two successive acid-base titrations. (Eq. 1 & 2)

Since the analyte is carbonate, the titrant used is HCl which was standardized first using a primary standard. An ideal primary standard must be extremely pure, stable, has no waters of hydration, and has a high molecular weight.2 It must also be weighed accurately.3 For this experiment, Na2CO3 was used as the primary standard because anhydrous Na2CO3 with high purity can be readily obtained.4 Using NaOH as primary standard on the other hand, is not suitable because NaOH is hygroscopic- it absorbs water in the air making it impossible to weigh accurately.3 At the start of the standardization, solid sodium carbonate was weighed and dissolved with boiled distilled water. Boiled distilled water is used not only in the preparation of this particular solution but also in other base solutions to prevent carbonate error. Carbonate error is an error in the determination of endpoint due to carbonic acid formations. This carbonic acid reacts with the base which interrupts the

reaction of the analyte base with the acid. Since, some of the base reacts with the carbonic acid, the amount of HCl used to neutralize the base would be less than the actual value which could cause a higher HCl molarity to be calculated. To prevent this, distilled water is first boiled before use to remove the CO2 that causes carbonate error. After dissolution, 3-4 drops of methyl orange is added to the solution and is then titrated with HCl. Before reaching the endpoint, the solution is boiled first to remove CO2. This improves the accuracy of titration because removing CO2 will change the conditions of the second part of the titration making it a strong base reacting with a strong acid.4 After boiling, the solution is cooled and then the titration is resumed until the endpoint is reached. Three trials were made for the standardization and the volume of HCl obtained from these trials were used to calculate the molarity of HCl. The net volumes of HCl were precise and are considered to be accurate because the computed average molarity (0.0493 M) is very close to the needed molarity which is 0.050 M. (Table 1) Table 1. Standardization of Hydrochloric Acid Solution Trial
1o Standard weight, g Net volume HCl, ml Molarity HCl, moles/L

After standardization, the soda ash sample was analyzed. A weighed sample was dissolved in boiled distilled water to prevent carbonate error. Then 1-2 drops of phenolphthalein was added to the solution and was titrated to endpoint with HCl. After endpoint, 3-4 drops of methyl orange was added and is titrated again with HCl until the color of the solution turns pale yellow. The solution is then boiled to remove CO2, cooled and then titrated again with HCl until it reaches endpoint. For this part, three trials were again conducted. The volume of HCl required to reach the phenolphthalein endpoint was compared to the volume required to reach the methyl orange endpoint. If the two volumes are equal, then the sample contains only Na2CO3. If the second volume is equal to zero, then the sample contains only NaOH. If the first volume is zero, then the sample contains only NaHCO3. If the first volume is greater than the second, then the sample contains a mixture of NaOH and Na2CO3. Lastly, if the first volume is less than the second, then the sample contains a mixture of NaHCO3 and Na2CO3 (Table 2). A third mixture that can be formed from the three compounds present is NaOH and NaHCO3. This mixture however, will not exist because the two compounds will react to form Na2CO3 and either NaOH or NaHCO3-whichever is in excess.

1 0.100 0.001 38.05

2 0.100 0.001 38.7

3 0.102 0.001 38.6

0.0495 0.0487 0.0498 0.005 0.005 0.005

Table 2. Comparison of HCl vol. at phenolphthalein endpoint and methyl orange endpoint. V1 vs V2 V2 = 0 V1 = V2 V1 = 0 V1 > V2 V1 < V2 Component NaOH Na2CO3 NaHCO3 NaOH and Na2CO3 NaHCO3 and Na2CO3

Table 4. %Composition of Soda Ash

% Composition of Soda Ash

Trial 1 Trial 2 Trial 3 15.23 0.388 21.3 11.43













It was observed in two out of three trials that the volume of HCl required to reach the phenolphthalein endpoint is less than the volume required to reach the methyl orange endpoint. From this observation, it is concluded that the soda ash sample analyzed contained both Na2CO3 and NaHCO3. (Table 3) Table 3. Sample Analysis Trial
Sample Weight, g Net vol. HCl at phenolphthalein endpoint, ml Net vol. HCl at methyl orange endpoint, ml

0.101 0.001

0.111 0.001

0.100 0.001

4.1 0.14 7.8 0.14 <

3.1 0.14 6.2 0.14 <

4.8 0.14 4.3 0.14 >

As observed from the data, there is an observed inconsistency in the V1 vs V2 between the three trials. This is may be because of some errors committed during the experiment. One error is the retention of CO2 in both the boiled distilled water and during methyl orange titration. Carbonate error may have been committed and may have caused a decrease in the correct volume of HCl to be used. Another error to be considered is either over or under titration especially using the methyl orange indicator since the color changes are hard to distinguish. Under titration would cause a calculated %composition to be lower and over titration would cause an increase in the calculated %composition. During the experiment, a lot of base solutions were formed and are transferred to glass containers. These solutions, however, should not be kept inside glass containers for a long time because it tends to etch glassware.5 REFERENCES [1] College of Engineering, University Of Massachusetts Amherst. CHAPTER XVI. VOLUMETRIC METHODS.

V1 vs V2

From these data the percent composition of soda ash was calculated with an average of 9.85% for NaHCO3 and 20.35% for Na2CO3. The calculated values were inconsistent for the three trials. This was because for every trial, a different person was doing the titration. (Table 4)

ses/572/572bk16/572BK16.html (accessed: Jan. 15, 2014) [2] The Chemistry Hypermedia Project. Analytical Standards. (accessed: Jan. 15,

2014) [3] Indiana University Southeast. Standardization of a Base, NaOH Class Notes. ek11.htm (accessed: Jan. 15, 2014)

[4] Seely, O. and de la Camp, U. California State University Dominguez Hills. Determination of the Carbonate of a SodaAsh Sample. al/carbnate.htm (accessed: Jan. 15, 2014)

[5] Department of Chemistry, University of Rochester. The Grasshoppers Guide to Cleaning Glassware. glassware.html (accessed: Jan. 15, 2014)