QUANTITATIVE DETERMINATION OF SODA ASH COMPOSITION BY DOUBLE INDICATOR TITRATION

YZZA CAMILLE A. DIAZ

DEPARTMENT OF FOOD SCIENCE AND NUTRITION, COLLEGE OF HOME ECONOMICS UNIVERSITY OF THE PHILIPPINES DILIMAN, DILIMAN, QUEZON CITY 1101, PHILIPPINES

DATE SUBMITTED: 25 JULY 2013 DATE PERFORMED: 18 JULY 2013

ABSTRACT In this experiment, the composition of soda ash is quantitatively determined by the use of double-indicator titration method. The indicators used were phenolphthalein 8.3 <pH< 10.0 which accounts for basicity and methyl orange 3.1 <pH< 4.5 which accounts for acidity[3], has close equivalence point to our desired endpoint. This titration involves a weak base- strong acid titration. The standardization of HCl was done using Na2CO3 as primary standard. Latterly, since Vph < Vmo Na2CO3 and NaHCO3 were determined as the components of soda-ash. For the first trial 32.9% Na2CO3 and 72. 1 %NaHCO3; for the second trial 24.1 % N a2CO3 and 76. 1% NaHCO3; and lastly the third trial 23.8 % N a2CO3 and 94.6% NaHCO3.It is rational therefore that the soda ash sample consists NaHCO3 since it is a product of the thermal decomposition of sodium carbonate. This experiment is significant to know the total acid neutralizing capacity of soda ash which can be used in the industry for the production of soap, glasses, paper etc.

INTRODUCTION Soda ash is an unrefined product acquired from the thermal decomposition of Sodium carbonate (NaHCO3)[1]. In this experiment, the goal is to determine quantitatively, its composition by double indicator titration method. Moreover, it aims to relate the concept of strong acid-strong base and weak acid-weak base titrations and carbonate system titration. Titration of substances basically is used to determine the amount of acid or base in a solution[2]. In a double indicator titration method, we use two indicators namely phenolphthalein and methyl orange instead of the common titration wherein there is only one indicator used. It is used only if there are two bases present in the solution. These indicators are qualified to be used in the experiment because the endpoints which are at 8.3 <pH< 10.0 and 3.1 <pH< 4.5 respectively, are close to the desired titration equivalence point. The solution is said to have reached the endpoint if it changed color, in this case solutions turn to yellow or near orange or in some, red because of over titration.

Before starting the experiment, solutions of a 250 mL 1.0 M stock HCl and 250 mL 0.050 M standard HCl solution from 1.0 M HCl were prepared. After this, we proceeded to the standardization of the 0.050 M HCl solution. First, we weighed 0.1 g of the primary standard Na2CO3. This was then dissolved by 75 mL boiled distilled water, then we added 3 drops of the methyl orange indicator and titrated it with 0.050 M HCl. When the solutions turn to yellow or near orange, we temporarily stopped the titration to boil the solution for two to three minutes. When it again turns to yellow, we continue its titration to end point. After this, the analysis of soda ash sample is started by weighing 0.5 0.2 g of soda ash sample in an analytical balance and dissolved it using 75 mL of boiled distilled water. We divided the solution into three and added 50 ml of boiled distilled water to each solution. Subsequently, we added 3 drops of the phenolphthalein indicator and titrated it with 0.050 M HCl. When the phenolphthalein endpoint is reached, three drops of methyl orange indicator is then added and titration was continued. When the color changes from yellow to near orange titration is temporarily stopped and then the solution was boiled for two to

three minutes. Similar to the standardization process, when the solution turns back to yellow, the titration is continued until the methyl orange endpoint. Determining the percent composition of compounds present in a soda ash sample helps in terms of knowing its alkalinity value. The alkalinity value is the total acid neutralizing capacity of soda ash, by knowing how much NaHCO3, Na2CO3 and NaOH (if there is any) is present in the sample, we may also know its acid neutralizing capacity. This implies the behavior of these groups of compounds and can later be convenient for chemical purposes (e.g. manufacture of soap, glass, paper, etc.). [1] RESULTS AND DISCUSSIONS For us to be able to determine the components of the unknown sample, we need to obtain the volume of HCl required to reach two distinct endpoints which are the volume of phenolphthalein endpoint and the volume of methyl orange endpoint. These two indicators are used because the endpoints which are at 8.3 <pH< 10.0 for phenolphthalein and 3.1 <pH< 4.5 for methyl orange, are close to the desired titration equivalence point [2], and at these respective endpoints, the solutions changes their color to signal neutralization of different protons of the complex system. The values of Vph and Vmo are obtained using the average net volume phenolphthalein endpoint and methyl orange endpoint respectively. The solutions shown in the appendix gave the values of Vph = 9.489666667 and Vmo = 45. Using Table 1, we can relate Vph and Vmo and determine the substance present in the soda ash sample. Table 1. The volume relationships for different compositions of soda ash. Relationship of Composition of Moles of Vph and Vmo sample substance present Vph=0; Vmo>0 NaHCO3 M Vmo Vmo=0 NaOH M Vph Vph= Vmo Na2CO3 M Vph or M Vmo Vph > Vmo Na2CO3 and NaOH: M(Vph NaOH Vmo) Na2CO3: M Vmo Vph< Vmo Na2CO3 and NaHCO3: M

NaHCO3

(Vmo Vph) Na2CO3: M Vph

Since, Vph< Vmo the expected compositions of the soda ash sample are Na2CO3 and NaHCO3. A greater Vmo implies that the HCl used to neutralize HCO3 is greater than the amount needed to neutralize CO3. Therefore indicating the presence of NaHCO3[3]. We can determine the percent composition of these compounds by using the Table 1 and equating it as seen in the calculations part of the appendix. The results for the first trial for the % Na2CO3 is 32. 9 % while NaHCO3 is 72. 1 %; for trial 2 24.1 % N a2CO3 and 76. 1% NaHCO3; and lastly for trial 3 23.8 % N a2CO3 and 94.6% NaHCO3. This results are rational because sometimes it is not possible for a 100% composition because the solutions may have impurities. The color change which is from yellow to near orange in the first titration is its fake endpoint. For us to be able to determine the true endpoint, we need to boil the solution for two to three minutes to remove the CO2 formed. After this we can resume titration and get the true endpoint as the solution again turns from yellow to near orange. If the solution turned red, it is over titrated. The absence of NaOH in the composition of the soda ash makes the composition of Na2CO3 and NaHCO3 compatible. The incompatibility of NaOH in the sample is because the presence of OH- will react with the HCO3-. This will cause a decrease in concentration and production of carbonate ions. [3] For this experiment, there are possible sources of error. Firstly, in weighing the soda ash and the primary standard using the analytical balance. Analytical balances, requires weighing by difference, one might have used the opposite of it which is weighing by addition. Secondly, wrong burette reading which can lead to a smaller or larger amount of HCl recorded which will affect on the concentration of phenolphthalein and methyl orange endpoint. And lastly, over titration of the solution. If it is over titrated, we can no longer determine the true endpoint of phenolphthalein and methyl orange in this case.

SUMMARY AND CONCLUSIONS The experiment have shown that Vph< Vmo which implies that the components of the soda ash sample are Na2CO3 and NaHCO3. It is a titration of a weak base with a strong acid, in this particular experiment the weak bases are Na2CO3 and NaHCO3 and their percent composition in the soda ash sample are determined using two indicators, phenolphthalein and methyl orange; and the HCl is the strong acid titrant. In the course of the addition of HCl the solution still contains some unreacted weak base and salt therefore acting as a buffer. The solution will contain salt of the weak base at the endpoint and by hydrolysis of the cation pH can be determined. The pH of the solution is dependent to the excess hydrogen ion from the titrant. [4]

REFERENCES [2] Zumdahl, Steve. Chemistry 4th edition. Houghton Mifflin Company. 1997. [4] Brady, Humiston. General Chemistry Principles and Structure 3rd edition. John Wiley and Sons Inc. USA. Internet References: [1]www.microlabinfo.com/.../CD...2...Soda.Ash.../11.2. Anal.Soda.Ash.pdf (Accessed July 23, 2013) [3] http://www.scribd.com/doc/92576976/FormalReport-1-Expt-7-Chem-26-1#download (Accessed July 24, 2013)

APPENDIX DATA GATHERED: Standardization of Hydrochloric Acid Solution Primary Standard used: Na2CO3 Percent Purity of Primary Standard: 99.7 % Formula mass of Primary Standard: 105.99 g Na2CO3 Table 1. Obtained values from the Standardization of Hydrochloric Acid Solution. Trial 1 2 Primary Standard weight, g 0.1006 0.0002 0.0954 0.0002 Final volume of HCl, ml 40.5 0.08 35.7 0.08 Initial volume of HCl, ml 1.9 0.08 0.6 0.08 Net volume of HCl, ml 38.6 0.08 35.1 0.08 M HCl 38.6 0.0001 35.1 0.0002 Average M HCl 0.0508 Sample Analysis Sample Stock Solution Mass Sample: 0.5633 0.0002 Total Volume of Sample Stock: 75.00 0.05 Working Sample Solution Volume of Sample Stock: 25.00 0.05 Total volume of Working Sample: 75.00 0.05 Table 2. Obtained values from the analysis of the sample. Trial 1 Phenolphthalein endpoint Final Volume of HCl, mL 11.5 0.05 Initial Volume of HCl, mL 0.03 0.05 Net Volume of HCl, mL 11.47 0.05 Methyl Orange endpoint Final Volume of HCl, mL 54.7 0.05 Initial Volume of HCl, mL 11.5 0.05 Net Volume of HCl, mL 43.2 0.05 Relationship of Vph and Vmo: Vph Vmo Composition of Soda Ash: Na2CO3 and NaHCO3 CALCULATIONS: Determination of the M HCl for the three trials in the Standardization of Hydrochloric Acid solution Trial 1 M HCl= = 0.04903102111 M HCl 0.0001 Trial 2 17.9 0.08 9.5 0.08 8.4 0.08 59.8 0.08 17.9 0.08 41.9 0.08 Trial 3 18.1 0.08 9.801 0.08 8.299 0.08 68 0.08 18.1 0.08 49.9 0.08 3 0.0951 0.0002 35.6 0.08 1.4 0.08 34.2 0.08 34.2 0.0002

Trial 2 M HCl= = 0.051133029 M HCl 0.0002

Trial 3

M HCl= Average M HCl=

=0.05231360787 M HCl =

0.0002

= 0.05082588599 M HCl

Error Propagation Trial 1 R= 0.04903102111 r= R r= Trial 2 R= 0.05231360787 r= Trial 3 R= 0.05082588599 r= 0.05082588599 = 0.0002 = 0.0002 = 0.0001

Determination of Vph and Vmo and their relationship using the data gathered in Table 2. Vph=

= =

= 9.489666667 = 45

Vmo=

Since the calculated value of Vph is 9.489666667 and Vmo is 45 it implies that Vph Vmo, hence the components of the soda ash sample are Na2CO3 and NaHCO3. Determination of the percent composition of Na2CO3 and NaHCO3 in the soda ash sample.

Trial 1 % NaOH = 0 % % Na2CO3= = % NaHCO3= = Trial 2 % NaOH = 0 % % Na2CO3= = % NaHCO3= = Trial 3 % NaOH = 0 % % Na2CO3= = % NaHCO3= = =94.6% NaHCO3 (100%) = 23.8 % N a2CO3 =76. 1% NaHCO3 (100%) = 24.1 % N a2CO3 = 72. 1 % NaHCO3 (100%) = 32. 9 % N a2CO3