Quantitative Determination of Potassium Acid Phthalate (KHP)

Erick N. Zorrilla Michelle Cruz

Abstract
The experiment focused on the Standardization by titration of a weak acid, potassium acid phthalate (KHP), with a strong base, sodium hydroxide (NaOH) in order to determine the concentration of the NaOH solution and by quantitative analysis of potentiometric data. From the titration of the three trials of the standard KHP solution we obtained an average molarity of 0.12182M. From the three trials of the KHP unknown the average % KHPunknown was 40.80 % and the deviation error (RSD ppth) was 12.653. In the potentiometric titration the pKa average was 8.855 and the RSD ppth 7.4808.

Introduction
Direct Titration End Point Primary Standard
High Purity Stability Non hygroscopic Low cost Reasonable solubility in the titration medium High formula weight to minimize weighing errors We used: KHP

Equivalence Point

KHP in the real world

KHP can be used as a buffering agent. Used in Industry as a Secondary Standard Solution. The Calcium Phosphate-Calcium Carbonate System: Growth of Octacalcium Phosphate on Calcium Carbonates . Stamatia Rokidi, Christele Combes, and Petros G. Koutsoukos. Department of Chemical Engineering and FORTH-ICEHT, University of Patras, GR 26 500, Patras, Greece.

Experimental
APPARATUS AND MATERIALS

Class A Burets, 50.00 (0.05 mL) KHP standard Unknown KHP sample 99.97 % pure NaOH 50% w/v Phenolphthalein Parafilm

Experimental
Sample Preparation Procedure
A class A Buret was filled with the titrant 50 % w/v NaOH solution and used to titrate both the standard and unknown samples until a clear to pink color change was observed that persisted for more than 15 seconds.

KHP standard

KHP Unkwown

Data

Table 1. General specifications of KHP standard % Purity FW: KHP Ratio Rx. (g/mol) (mol/mol) 99.97 204.227 1 Table 2. Gravimetric data for manual titrations Standards Sample Mass (g) NaOH (mL) Sample S1 0.6816 27.97 D1 S2 0.6657 26.57 D2 S3 0.6453 25.57 D3 Table 3. Titrimetric Results Sample 1 2 3 Averages Sample 1 2 3 Averages RSDppth KHP (g) 0.6814 0.6655 0.6451 0.6640 mol NaOH 1.409E-03 1.378E-03 1.290E-03 1.359E-03

Volume KHP (mL)

Unknowns Mass (g) 0.6959 0.6914 0.6530

NaOH (mL) 11.57 11.31 10.59

Standards Mol KHP M NaOH 3.336E-03 1.1929E-01 3.259E-03 1.2264E-01 3.159E-03 1.2353E-01 0.0033 1.2182E-01 Unknowns M KHP KHP (g) % KHP 1.218E-01 0.2879 41.36 1.218E-01 0.2814 40.70 1.218E-01 0.2635 40.35 1.218E-01 2.776E-01 4.080E+01 12.653

Calculations

Potentiometric Data
Quantitative Determination of KHP by Acid-Base Titration Trial 1
14.000 12.000 10.000 pH pH 0.00 5.00 10.00 15.00 8.000 6.000 4.000 2.000 0.000

Quantitative Determination of KHP by Acid-Base Titration Trial 2

14.000 12.000 10.000 8.000 6.000 4.000 2.000 0.000 0.00 5.00 10.00 15.00 20.00

Volume of NaOH (mL)

Volume of NaOH (mL)

Quantitative Determination of KHP by Acid-Base Titration trial 1

20.000 15.000 pH/ V 10.000 5.000 0.000 0.00 5.00 10.00 pH/ V

Quantitative Determination of KHP by Acid-Base Titration trial 2

12.000 10.000 8.000 6.000 4.000 2.000 0.000 0.00 5.00 10.00 15.00

Average V of NaOH (mL)

Average Volume NaOH (mL)

Potentiometric Data
Quantitative Determination of KHP by Acid-Base Titration Trial 1
180.000 140.000 100.000 60.000 20.000 -20.000 0.00 -60.000 -100.000 -140.000 -180.000

Quantitative Determination of KHP by Acid-Base Titration Trial 2

60.000 40.000 20.000 0.000 pH -20.000 0.00 -40.000 -60.000 -80.000 -100.000 2.00 4.00 6.00 8.00 10.00 12.00 14.00 16.00

pH

2.00

4.00

6.00

8.00

10.00

12.00

14.00

Volume NaOH (mL)

Volume NaOH (mL)

Quantitative Determination of KHP by Acid-Base Titration

0.000006 0.000005 [H O]*Volume NaOH 0.000004 0.000003 0.000002 0.000001 0 -0.000001 8.608.70 8.808.90 9.009.10 9.209.30 9.409.50 9.709.80 10.00 9.60 9.90 Volume NaOH (mL) [H O]*Volume NaOH

Quantitative Determination of KHP by Acid-Base Titration

5.00E-06 4.00E-06 3.00E-06 2.00E-06 1.00E-06 0.00E+00 8.60 8.70 8.80 8.90 9.00 9.10 9.20 9.30 9.40 9.50 9.60 9.70 9.80 8.65 8.75 8.85 8.95 9.05 9.15 9.25 9.35 9.45 9.55 9.65 9.75 -1.00E-06 Volume NaOH (mL)

Potentiometric Data Results

Table 4. Potentiometric Data Y Sample Trial 1 Trial 2 Sample Trial 1 Trial 2 Sample Trial 1 Trial 2 Sample Trial 1 Trial 2 Final V 9.90 9.90 Final V 9.90 9.90 Final V 9.90 9.90 Final V 9.90 9.90 Final V. (mL) 9.85 9.80 Y' Final V. (mL) 9.88 9.85 Y" Final V. (mL) Tit. Error 9.91 0.01 9.90 0.00 Gran Plot Final V. (mL) Tit. Error 9.81 0.09 9.73 0.17 Tit. Error 0.02 0.05 Tit. Error 0.05 0.10 pKa Avg pKa 8.59 8.8550 9.12

Conclusions
From the titration of the three trials of the standard KHP solution we obtained an average molarity of 0.12182M. From the three trials of the KHP unknown the average % KHPunknown was 40.80 and the deviation error (RSD ppth) was 12.653. A source of error could be in the weighting of the KHP unknown sample that was measured to be approximately 0.6500-0.7000g yet the procedure called for 0.7500-0.8000g. Other errors could be reading the volumes on the buret incorrectly or that the measuring equipment wasn t well calibrated. In the potentiometric titration the pKa average was 8.855 and the RSD ppth 7.4808. Both results are precise but it does not know if are accurate because the concentration of the KHP is unknown.

Additional Applications

Questions
1. Which are the possible sources of error in your experiment and how can you correct them? A possible error might be introduced in the weighing of the unknown KHP sample or the regular KHP sample. Titrating past the equivalence can introduce serious systematical errors. 2. What would happen if you do not boil the water used to prepare your titrant and sample solutions? Impurities in the water such as high concentrations of Mg+ or Cu+ might interfere with the titration reaction taking place. Also water dissociation effects must be insignificant in order to assume that the neutralization of KHP with NaOH be considered a complete reaction. These results can also be affected by the presence of CO2 in the solution because this compound forms HCO3 which can be neutralized by the titrant NaOH. 3. Why does the typical acid/base indicator exhibit its color change over a range of about 2 pH units? The theoretical useful range of an indicator is: 1/10 [In^- ]/[HIn] 10/1 . Since pH = pKa + log (In-/HIn-) then pH =pKa 1 for a change in acid color; pH = pKa + 1 for the basic color. So we can conclude the the pH range = pKa 1. 4. Why the standard reagents used in neutralization titrations are generally strong acids and bases rather than weak acids and bases. The standard reagents used in neutralization titration are strong acids or bases because the strong acids and strong bases tend to react completely with all the reactive present. With the aid of indicators, Chemists can find the equivalence point where the stoichiometric analytical amount of titrant is chemically equivalent to the amount of the analyte reacted.

Questions
5. Explain in your own words how to calibrate a pH electrode. Using a 7.00 pH and a 4.01 buffer solution: Rinse the electrode using distilled water. Gently blot the electrode on a soft tissue to remove the excess rinse water, not rubbing the bulb since it can cause a static charge build-up. Insert the electrode and place a thermometer along with the electrode in the 7.00 pH buffer solution. Allow 30 seconds for the pair to reach thermal equilibrium with the buffer. Adjust the temperature dial on the meter to correspond with the thermometer reading. Then adjust the pH meter with the standardize/zero control for a pH indication equal to 7.00. Repeat Step a, and insert the electrode and the ATC in a 4.01 buffer solution. Allow 30 seconds before adjusting the pH meter with the slope/span control for a pH indication equal to 4.01. Repeat Steps b and c to maximize the precision of the calibration. 6. Do you think that the titration error of your experiment has a significant effect in your analysis? Justify your answer. The titration error does have a significant effect in the analysis because if an error is made during the titration not all the results obtained are going to be accurate.

References
De Jesus, M.A., M. Vera, and J.I. Padovani. "Quantitative Determination of Potassium Quantitative Acid Phthalate Analytical Chemistry for Phthalate." Engineers Laboratory Manual. (2007): 67-73.