1.

0 ABSTRACT The objective of this experiment is to determine the molarity of a solution and the percent by mass of acetic acid in vinegar by titration with a standardized sodium hydroxide solution. 250mL of sodium hydroxide, NaOH solution with approximately 0.6M was prepared from sodium hydroxide pellets. The sodium hydroxide solution was standardized with potassium hydrogen phthalate (KHP) before it is used for the titration with vinegar. The titration was repeated twice. Based on the results, the standardization of sodium hydroxide, the first titration result in 0.6618M of sodium hydroxide which requires 11.10mL of sodium hydroxide solution to neutralize the KHP solution. While the second titration result in 0.8766M of sodium hydroxide which requires 8.38mL of sodium hydroxide solution to neutralize the KHP solution and the average of the molarity if the sodium hydroxide is 0.7692M. For the second experiment, first titration yields 1.4023M of acetic acid, 1.2799M in second titration and the average of the molarity of the acetic acid in vinegar is 1. 3411M. Thus, the average percent by mass of acetic acid in vinegar is 8.05%.

2.0

INTRODUCTION

Concentration of solution is the amount of solute in a given amount of solvent. A concentrated solution contains a relatively large quantity of solute in a given amount of solvent. Dilute solutions contain relatively little solute in a given amount of solvent. There are two specific terms to express concentration, namely molarity and percent by mass: o Molarity is the number of moles solute per liter of solution: ( ) o Percent by mass is the mass in grams of solute per 100 grams of solution

Vinegar is a dilute solution of acetic acid. The molecular formula of acetic acid is CH3COOH. Both molarity and percent by mass of acetic acid in a vinegar solution can be determined by performing a titration. A titration is a process in which small increments of a solution of known concentration are added to specific volume of a solution of unknown concentration until stoichiometry for that reaction is attained. Knowing the quantity of the known solution required to complete the titration enables calculation of the unknown solution concentration. The purpose of titration is to determine the equivalence point of the reaction. The equivalence point is reach when the added quantity of one reactant is the exact amount necessary for stoichiometric reaction with another reactant.

3.0

OBJECTIVES

Determine the molarity of a solution and the percent by mass of acetic acid in vinegar by titration with a standardized sodium hydroxide solution (NaOH). 4.0 THEORY

In the titration process, a burette is used to dispense a small, quantifiable increment of solution of known concentration (Figure 1-1). A typical burette has the smallest calibration unit of 0.1mL (Figure 1-1), therefore the volume dispensed from the burette should be estimated to the nearest 0.05mL.

a)

b)

Figure 4.1: a) Depicts a typical 50-mL burette. b) Indicates smallest calibration unit, 0.1mL, on a typical 50-mL burette

In this experiment, the equivalence point occurs when the moles of acid in the solution equals the moles of base added in the titration. For example, the stoichiometric amount of 1 mole of the strong base, sodium hydroxide (NaOH), is necessary to neutralize 1 mole of the weak acid, acetic acid (CH3CO2H), as indicated in equation below: NaOH(aq) + CH3CO2H(aq) NaCH3CO2(aq) + H2O(l) The sudden change in the solution pH shows that the titration has reached the equivalence point. pH in an aqueous solution is related to its hydrogen ion concentration. Symbolically, the
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hydrogen ion concentration is written as [H30+]. pH is defined as the negative of the logarithm of the hydrogen ion concentration. [ ]

pH scale is a method of expressing the acidity or basicity of a solution. Solutions with pH< 7 are acidic, pH = 7 are neutral and pH > 7 are basic. For example, a solution having H 3O+ concentration of 2.35 x 10-2 M would have a pH of 1.629 and is acidic. pH electrodes will be used in this experiment. The titration is initiated by inserting a pH electrode into a beaker containing the acid solution (pH within 3-5). As sodium hydroxide, NaOH, is incrementally added to the acid solution, some of the hydrogen ions will be neutralized. As the hydrogen ion concentration decreases, the pH of the solution will gradually increase. When sufficient NaOH is added to completely neutralize the acid (most of the H30+ ions are removed from the solution), the next drop of NaOH added will cause a sudden sharp increase in pH (Figure 1.2). The volume of based required to completely neutralized the acid is determined at the equivalence point of titration.

Figure 4.2: Acid-base titration curve of weak acid titrated with NaOH.

In this experiment, titration of a vinegar sample with a standardized sodium hydroxide solution will be performed. To standardize the solution, a primary standard acid solution is initially prepared. In general, primary standard solutions are produce by dissolving a weighed quantity of pure acid or base in a known volume of solution. Primary standard acid or bases have several common characteristics: They must be available in at least 99.9 purity They must have a high molar mass to minimize error in weighing They must be stable upon heating They must be soluble in the solvent of interest

Potassium hydrogen phthalate, KHC8H4O4 and oxalic acid, (COOH)2, are common primary standard acids. Sodium carbonate, Na2CO3, is the most commonly used base. Most acids and bases (e.g. HCl, CH3COOH, NaOH and KOH) are mostly available in primary standard form. To standardize one of these acidic solutions, titration of the solution with a primary standard should be performed. In this experiment, NaOH solution will be titrated with potassium hydrogen phthalate (KHP). The reaction equation for this is: KHC8H4O4(aq) + NaOH(aq) KNaCH8H4O4(aq) + H2O(l) Once the sodium hydroxide solution has been standardized it will be titrated with 10.00mL aliquots of vinegar. The reaction equation for vinegar with NaOH is: CH3COOH(aq) + NaOH(aq) NaCH3COO(aq) + H2O(l) Knowing the standardized NaOH concentration and using equation above, we can determine the molarity and percent by mass of acetic acid in the vinegar solution.

5.0 5.1

METHODOLOGY Apparatus and Materials 1. 250mL of volumetric flask 2. 250mL of beaker 3. Burette 4. Ring stand 5. Measuring cylinder 6. Hot plate 7. Magnetic stirrer 8. pH meter 9. Distilled water 10. Sodium hydroxide, NaOH 11. Potassium hydrogen phthalate, KHP 12. Vinegar

5.2

Experimental procedure a) Standardization of sodium hydroxide solution

1. 250 mL of approximately 0.6M of sodium hydroxide solution is prepared from NaOH solid. The solution is prepared in a flask. During the preparation of sodium hydroxide solution, the calculation is checked with the laboratory instructor prior and the calculation is recorded. 2. A beaker is weighed and the mass is recorded to the nearest 0.001g. 1.5g of KHP is added to the beaker. The mass of the beaker and KHP is recorded to the nearest 0.001g. The mass of KPH by differences is calculated and the data is recorded. 30mL of distilled water is added to the beaker. The solution is stirred until the KHP has dissolved completely. 3. The solution of KHP is titrated with the NaOH solution. Every reading of pH by 1mL added is recorded. 4. Steps 1 to 3 are repeated for second trial to standardize the NaOH solution.
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5. The graph of pH versus NaOH is plotted. From the plots, the volume of NaOH required to neutralize the KHP solution in each titration are determined 6. The molarity of sodium hydroxide for titration 1 and 2 are calculated. 7. The average molarity of the sodium hydroxide solution is calculated. The resulting sodium hydroxide concentration will be used in part B of the experiment.

b) Molarity of acetic acid and mass percent in vinegar

1. 10.00mL of vinegar was transferred to a clean, dry 250mL beaker using a 10mL volumetric pipette. 100mL of distilled water was added. 2. Every 1mL oh NaOH solution added to the vinegar is recorded with the pH level. 3. Step 1 and 2 are repeated for second and third trial. 4. The graph of pH versus NaOH volume added is plotted and from the plots determines the volume of NaOH required to neutralize the vinegar in each titration. The data is recorded 5. The molarity of acetic acid in vinegar for titration1,2 and 3 are calculated 6. The average molarity of acetic acid for each titration is calculated. 7. The percent by mass of acetic acid in vinegar for titration 1,2 and 3 are calculated 8. The percent by mass of acetic acid in vinegar are calculated.

6.0 6.1

RESULT AND CALCULATIONS Result and Data a) Standardization of sodium hydroxide solution Initial pH reading First titration: 4.43 Second titration: 5.24

Volume of NaOH to neutralize the KHP solution (mL) 1 2 3 4 5 6 7 8 9 10 11 12

Titration 1

Titration 2

4.51 4.71 4.85 4.99 5.13 5.26 5.41 5.57 5.75 5.91 6.47 11.81

5.38 5.43 5.61 5.78 5.86 5.92 6.23 6.45 7.89 11.78 12.13 12.32

b) Molarity of acetic acid and mass percent in vinegar Initial pH reading First titration: 2.69 Second titration: 2.85 Third titration: 3.13 Titration 1 Titration 2

Volume of NaOH to neutralize the vinegar solution (mL) 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20

3.31 3.60 3.75 3.96 4.08 4.24 4.32 4.43 4.55 4.65 4.76 4.86 4.98 5.12 5.18 5.48 5.85 6.23 9.58 11.03

3.43 3.76 3.92 4.10 4.21 4.34 4.46 4.58 4.69 4.82 4.91 5.03 5.16 5.33 5.56 5.89 7.63 11.28 11.58 11.72

a) Standardization of sodium hydroxide solution Titration 1 Mass of beaker (g) Mass of beaker + KHP (g) Mass of KHP (g) Volume of NaOH to neutralize the KHP solution (mL) 11.10 8.38 0 1.5 1.5 Titration 2 0 1.5 1.5

b) Molarity of acetic acid and mass percent in vinegar Titration 1 Volume of NaOH to neutralize the vinegar solution (mL) 18.23 16.64 Titration 2

6.2

Calculation Preparation of 250mL of approximately 0.6M NaOH:

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a) Standardization of sodium hydroxide solution

13 12 11 10 9 8 pH 7 6 5 4 3 2 1 0 0 1 2 3 4 5 6 7 8 9 10 11 12 13 Volume of NaOH (mL) pH

Volume of NaOH versus pH (Titration 1)

13 12 11 10 9 8 pH 7 6 5 4 3 2 1 0 0

Volume of NaOH versus pH (Titration 2)

pH

10

11

12

13

Volume of NaOH (mL)

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b) Molarity of acetic acid and mass percent in vinegar

12 11 10 9 8 7 pH 6 5 4 3 2 1 0 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 VOlume of NaOH (mL) pH

Volume of NaOH versus pH (Titration 1)

13 12 11 10 9 8 pH 7 6 5 4 3 2 1 0 0 1

Volume of NaOH versus pH (Titration 2)

pH

9 10 11 12 13 14 15 16 17 18 19 20 21

VOlume of NaOH (mL)

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a) Standardization of sodium hydroxide Equivalence point from graph (Titration 1): 11.1 mL of NaOH

KHC8H4O4 (aq) + NaOH (aq)

KNaC8H4O4 (aq) + H2O (l)

1 mol KHP 1 mol of NaOH solution, so for the molarity of sodium hydroxide is:

Equivalence point from graph (Titration 2): 8.38 mL of NaOH

KHC8H4O4 (aq) + NaOH (aq)

KNaC8H4O4 (aq) + H2O (l)

1 mol KHP 1 mol of NaOH solution, so for the molarity of sodium hydroxide is:

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b) Molarity of acetic acid and mass percent in vinegar

Equivalence point from graph (Titration 1): 18.23 mL of NaOH

HC2H3O2 (aq) + NaOH (aq) 1 mol NaOH 1 mol HC2H3O2 Mole HC2H3O2 = 0.01402 mol

NaC2H3O2 (aq) + H2O (l)

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Equivalence point from graph (Titration 2): 16.64 mL of NaOH

HC2H3O2 (aq) + NaOH (aq) 1 mol NaOH 1 mol HC2H3O2 Mole HC2H3O2 = 0.01279 mol

NaC2H3O2 (aq) + H2O (l)

Percent by mass of acetic acid in vinegar ( Titration 1)

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o Assume vinegar= 1g/mL

Percent by mass of acetic acid in vinegar (Titration 2)

o Assume vinegar= 1g/mL

16

Average percent by mass of acetic acid in vinegar

o Assume vinegar= 1g/mL

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7.0

DISCUSSION The pH of KHP solution was recorded that was titrated with every 1mL of sodium

hydroxide solution. The data was then used to plot the graph and the equivalence point was obtained as shown in the graph in the calculation section. As the first graph that was the first titration, the equivalence point was observed to be 11.10mL of sodium hydroxide solution to the KHP solution. The equivalence point occurs when the moles of acid in the solution equal to the moles of base added in the titration. From the graph, we can see a sudden change of pH from 11mL to 12mL of NaOH solution where the pH increased suddenly from 6.47 to 11.81. The sudden change in the solution pH shows that the titration has reached the equivalence point. While for the second titration, the amount of sodium hydroxide solution needed to neutralize the unknown acid was different with the first titration which was 8.38mL. The equivalence point of the second titration lies between 8mL and 9mL which result in 6.45 and 7.89 where a sudden change of pH shows that the titration has reached the equivalence point. The amount of NaOH solution needed to neutralize the KHP solution then used to calculate the molarity of the sodium hydroxide where 1 mol of KHP is equal to 1 mol of NaOH. The pH of vinegar was recorded from the titration of every 1mL of sodium hydroxide solution and used to plot the graph where the equivalence point was obtained as shown in the graph in the calculation section. The first graph shows that there was a sudden change of pH from 18mL to 19mL of titrated unknown acid which result in 6.23 and 9.58. The equivalence point for the first titration was observed to be at 18.23mL of NaOH solution to the vinegar. As the second graph, the equivalence point was observed to be at 16.64mL of NaOH solution to vinegar solution. The sudden change in the pH of vinegar solution shows that the solution has completely reacted or has been neutralized by the NaOH solution where the equivalence point was obtained. Then, each amount of NaOH solution needed to neutralize the vinegar was used to calculate the molarity of the sodium hydroxide solution where 1 mol of NaOH is equal to 1 mol of acetic acid. The first and second titration yields 0.6618M and 0.8766M of sodium hydroxide where it is calculated from the number of moles of sodium hydroxide solution divided with the amount of sodium hydroxide solution needed to neutralize the KHP solution. Therefore, the average of the molarity of the sodium hydroxide solution is 0.7692M where this is the standardized NaOH
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concentration. As the standardized NaOH concentration obtained, only then the molarity and the percent by mass of acetic acid in the second experiment can be calculated. The standardized NaOH concentration was used to calculate the molarity of acetic acid in vinegar for each titration by multiplying it with the amount of NaOH solution needed to neutralize the vinegar solution and divided with the volume of vinegar used. The first titration result in 1.4023M of acetic acid while the second titration result in 1.2799M of acetic acid and therefore the average of the molarity of the acetic acid was 1.3411M. The percent by mass of acetic acid for each titration can be obtained by calculating the mass of acetic acid in the vinegar and divide it with the mass of the vinegar. Percent by mass for the first titration obtained was 8.42% while the second titration was 7.69%. Therefore, the average percent by mass of acetic acid in vinegar was 8.05% The amount of sodium hydroxide solution needed to neutralize the unknown acid was different from the first titration with the second one was probably because of the human error that occurs during the experiment. The stirring rate might be different from one titration to another and may affect the result of the experiment. Error also can occur during the KHP solution preparation, as the beaker used for the titration contain several mL of distilled water from the rinsing activity which can cause the changes of molarity of the solution from the calculated value. The other reason might be due to the bubbles that appear at the tip of the burette. Bubble that appeared at the tip of the burette during the titration can affect the result of the experiment.

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8.0

CONCLUSION The common ion effect tends to suppress the ionization of a weak acid or a weak base.

This action can be explained by La Chteliers priciple. A buffer solution is a combination of either weak acid and its weak conjugate base (supplied by a salt) or a weak base and its weak conjugate acid (supplied by a salt); the solution reacts with small amounts of added acid or base in such a way that the pH of the solution remains nearly constant. Buffer systems play a vital role in maintaining the pH of body fluids. The pH at the equivalence point of an acid-base titration depends on hydrolysis of the salt formed in the neutralization reaction. For strong acid-strong base titrations, the pH at equivalence point is 7; for weak acid-strong base titrations, the pH at equivalence point is greater than 7, for strong acid-weak base titrations, the equivalence point is less than 7. From the first experiment which is standardization of sodium hydroxide with KHP solution, the average molarity of sodium hydroxide is 0.7692M. From the second experiment, the average molarity of acetic acid and average percent by mass of acetic acid in vinegar was calculated which result in 1.3411M and 8.05%.

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9.0

RECOMMENDATIONS A few recommendations are suggested on the techniques employed during the

experiment. First, make sure all the equipment used for the experiment is cleaned and dried before start the experiment. Second, make sure the tip of the burette is filled by the base (NaOH) completely (no air bubble) before the experiment start. Third, make sure there is no KHP liquid splashed from the beaker when the titration was done. Forth, make sure to rinse the burette with base solution following with distilled water before doing the experiment. Also, for future studies, it is recommended to use different approach, instead of using NaOH as a base, we can use Na(OH)2 as a base. We can see what changes in the calculations would then have to be made to determine the molar concentration of the base. Another recommendation is by using indicators. Indicators are substances that have distinctly different colors in acidic and basic media. One commonly used indicator is phenolphthalein, which is colorless in acidic and neutral solutions but reddish pink in basic solutions. At the equivalence point, all the KHP present has been neutralized by the added NaOH and the solution is still colorless. However, by adding just one more drop of NaOH solution, the solution will immediately turn pink because the solution is a base.

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10.0 [1]

REFERENCE Chang, R. and Cruickshank, B. (2005). Chemistry. 8th ed. International Edition: Mc Graw Hill. Pg: 145 147, 690 699.

[2]

Sibert, G. (unknown) Determination of Acetic Acid in Commercial Vinegar (on-line) http://www.files.chem.vt.edu/RVGS/ACT/lab/Experiments/Exp_21-Vinegar.html (5 OCTOBER 2013)

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11.0

APPENDICES

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