Chance Boudreaux

DETERMINATION OF NaCO BY MEANS OF BACK TITRATION Chance Boudreaux, Kennesaw State University Quantitative Analytical Chemistry Lab 2800 Instructor: Dr. H. Z. Msimanga INTRODUCTION: The objective of the experiment is to determine the % mass of sodium carbonate (NaCO) in the unknown sample. This is done by means of a back titration in order to ensure that the titration will be successful due to the possibility that the carbonate ion (CO) can form two different reactions with hydronium (HO). Back titration is a titration done in reverse. Instead of titrating the original sample, a known excess of standard reagent, in this case HCl, is added to the solution, and the excess is titrated. Using a back titration is helpful if the endpoint of the reverse titration is easier to identify than the endpoint of the normal titration. Back titrations are also helpful if the reaction between the analyte and the titrant is very slow, or when the analyte is in a non-soluble solid. Either of these two reactions can occur:

(1)

CO32 H 3O HCO3 H 2O CO32 2H 3O HCO3 H 2O

(2)

These reactions cause a problem due to eq1 needing the indicator phenolphthalein and eq2 using indicator methyl orange.

Chance Boudreaux

In order to perform a back titration of sodium carbonate, a standardized strong acid and base will be required. The data, in this report, was extracted by the use of 0.09731M HCl and 0.09948M NaOH (this means phenolphthalein will be the indicator). The experiment will also require a 50mL buret, 10mL pipet, a graduated cylinder, 250mL volumetric flask, a balance, and a hot plate for each time you run it. Table 1: (preparation of each flask for titration)
Table 1 NaCO (g) HCl (mL) HO (mL) Trial 1 0.3395 50.00 25.00 Trial 2 0.3579 50.00 25.00 Trial 3 0.3049 50.00 25.00 Trial 4 0.3049 50.00 25.00

After the solutions are prepared they should be heated for 3-4 minutes to allow the reaction (eq3) to go until completion, as well as, to allow the CO (g) that is formed to dissipate. This is so that the CO does not adversely react with the phenolphthalein creating an unwanted precipitate.

(3)

Na2CO3 2HCl 2 NaCl CO2 H 2O

After the solutions cool to room temperature begin titrating. The following equations (eq4, eq5, & eq6) are used to obtain grams of NaCO from the sample after titrations are complete.

(4)

M NaOH L NaOH 1 mol HCl 1 mol NaOH M HCl

L HClexcess

(5)

L HCl L HClexcess L HClreacted

Chance Boudreaux

(6)

M HCl L HClreacted 1 mol Na2CO3 MW Na2CO3 2 mol HCl

(MW NaCO= 105.9885 g/mol)

g Na2CO3

(7)

g Na2CO3 g TotalNa 2CO3

*100 % mass % CO3

(8)

Sx
_

*100% % RSD

x
From here find g NaCO, than convert to mass % NaCO as shown in table 2. Table 2: (Experimental results of Trials 1-4, % mean and %RSD)

Table 2 NaOH (mL) NaCO (g) mass NaCO (%) mean NaCO (%) %RSD (%)

Trial 1 Trial 2 Trial 3 Trial 4 24.52 0.1308 38.53 37.80 1 24.42 0.1340 37.44 24.50 0.1148 37.65 24.38 0.1146 37.59

(Unknown code #249 for stock sample) DISCUSSION: This experiment is created to quantify CO in an unknown purity of NaCO. This is done by a means of a back titration technique, due to two possible reactions between HO and CO. This back titration is done by adding a known excess amount of standardized HCl to a weighted
3

Chance Boudreaux

sample of NaCO. The excess HCl was titrated with standardized NaOH, to quantify the amount of HCl that reacted with the sample. Using stoichiometry, the g of analyte (CO) can now be found and then converted to a % mass by dividing the total mass of the sample. The % CO along with the %RSD, approximates the amount of CO in a given sample from the stock bottle. The % relative standard deviation (%RSD) shows the tolerance () of a sample's mean. Due to the low %RSD of this data, it proves the data's mean to be a valid approximation. The %RSD of this data also shows that most of the deviation is from the imperfect blend of the unknown sample and the tolerance error of the instruments used, due to a relatively small amount of deviation in the mean. The other calculations supporting the precision of the data are done by a ttest. A t-test uses a normal distribution curve to see if your data fits within set parameters. The data acquired through this experiment test valid for the 50th confidence level, meaning that the data fits within the 25% of the mean on the normal distribution curve. CONCLUSION: The results of the back titration concluded that we have a mean of 37.80% NaCO with a 1%RSD for the unknown NaCO stock provided in the laboratory. The tcalc = 0.7407 for the 50% confidence level and the tcrit = 0.741 meaning that the data is appropriate for the 50th confidence level. REFERENCE: Harris, D. C. (2010). Quantitative chemical analysis. (Eighth Edition ed.). New York: W.H. Freeman and Company.

Chance Boudreaux

ACKNOWLEGEMENTS: H. Z. Msimanga APPENDIX: The below example calculations are taken from trial 1:
0.09948M NaOH 0.02452L NaOH 1 mol HCl 1 mol NaOH 0.09731M HCl

(4)

0.02507 L HClexcess

(5)

0.05000 L HCl 0.02507 L HClexcess 0.02493 L HClreacted

(6)

0.09731M HCl 0.02493 L HClreacted 1 mol Na2CO3 105.9885MW Na2CO3 2 mol HCl

0.1308g Na2CO3

(7)

0.1308g Na2CO3 0.3395g TotalNa 2CO3

*100 % 38.53 mass % Na2CO3

(eq8 uses data from every trial; standard deviation over the mean of % mass NaCO)

(8)

0.4930 37.80

*100% 1 % RSD