UNIVERSITI TEKNOLOGI MARA FAKULTI KEJURUTERAAN KIMIA ENGINEERING CHEMISTRY LABORATORY (CHE485) NAME STUDENT NO.

GROUP EXPERIMENT DATE PERFORMED SEMESTER PROGRAMME / CODE SUBMIT TO No. 1 2 3 4 5 6 7 8 9 10 11 12 Title Abstract/Summary Introduction Aims Theory Apparatus Methodology/Procedure Results Calculations Discussion Conclusion Recommendations Reference / Appendix TOTAL MARKS : NUR NAJWA BINTI YUNUS : 2011207298 : EH 222 1A : CONCENTRATION OF ACETIC ACID : 26TH SEPTEMBER 2011 :1 : BACHELOR OF ENGINEERING IN CHEMICAL AND BIOPROCESS : CIK NURUL ASYIKIN MD ZAKI Allocated Marks (%) 5 10 5 10 5 10 10 10 20 5 5 5 100 Marks

Remarks: Checked by :

--------------------------Date :

TABLE OF CONTENTS

Abstract. Introduction.. Aims.. Theory... Methodology. Results... Calculations... Discussion. Conclusion. Recommendations. References.. Appendices.

1 2 3 4 5 8 15 17 19 20 21 22

ABSTRACT

Vinegar is a dilute solution of acetic acid and popular for its domestic use. This experiment was conducted in order to determine the percent by mass of acetic acid in vinegar by titration with a standardized sodium hydroxide solution. The process that plays major role in this experiment was titration whereby the required acid was titrated with sodium hydroxide (NaOH). In this experiment, there were two acids used which were potassium hydrogen phthalate (KHP) as a

primary standard acid and vinegar itself. Both of the solutions were titrated until a sudden change of the pH is noted. The sudden change was referred as the equivalence point. This point indicated the amount of NaOH required to neutralize the acids. The results of both experiment was used to calculate the mass of acetic acid in the vinegar. The average percent of mass of acetic acid is 5.0146 %. Therefore, the experiment was completely and successfully done.

INTRODUCTION

The term of concentration is used by scientist to estimate the amount of solute dissolved in a given quantity of solvent or quantity of solution. The greater the amount of solute dissolved in a particular amount of solvent, the more concentrated the resulting solution. Two specific terms are used to express the concentration, which are molarity and percent by percent by mass. Stoichiometry with the relative quantities of reactants and products in chemical

reactions. After balancing the chemical equation, the relations between quantites of reactants and products form a ratio of whole numbers. Stoichiometry wil be used to calculate quantities such as mass, number of moles, volume and percent yield. Stoichiometry is related to the law of conservation of mass and with a few calculations, we can predict how elements and components diluted in a standard solution react in certain experimental conditions and thus, able to determine the molarity. Molarity (M) expresses the concentration of a solution as the number of moles of solute in a liter of a solution. Therefore, the formula is as below: ( ) whereby percent by mass is the mass in grams of solute per 100 grams of solution and the formula is as below:

Acetic acid, CH3COOH is the main component of vinegar other than water. Typically, vinegar consist of 4 to 18% of acetic acid by mass. Vinegar is always used for medical purposes, culinary and agricultural purposes. Therefore, some country strictly limited the percent of acetic acid inside commercial vinegar for safety. Though acetic acid is considered as weak acid, higher concentration of acetic acid may results to the permanent eye damage, skin burns and irritation to mucous membrane. Titration is a common laboratory method to determine the unknown concentration of an identified analyte. Titration method is the process involved in neutralization of acid-base. The base is added to acid until sudden change of the pH of the solution. The changes of the pH is very sudden. Therefore, by using titration method, the volume of base poured into the acid can be controlled and by small increments. Through this method, the equivalence point in which the solutions are neutralize can be determined. 2

OBJECTIVE

The objective of this experiment is to: apply the process of titration determine the molarity of a solution determine the percent by mass of acetic acid in vinegar by titration with a standardized sodium hydroxide solution.

THEORY

In this experiment, titration is the major process involved to get the most accurate result. In the titration process, a burette is used to dispense solution in a small amount. Most of the burette has the smallest calibration unit of 0.1mL.

Figure 1: a) Shows a 50-mL burette. b) Smallest calibration unit, 0.1-mL

While conducting this experiment, the equivalence point will occurs when the moles of acid in the solution equals the moles of base added in the titration. For example, amount of 1 mole of sodium hydroxide (NaOH), is necessary to neutralize 1 mole of acetic acid (CH3CO2H), as shown below: NaOH(aq) + CH3CO2H(aq) NaCH3CO2(aq) + H2O(l) [Eq. 3] The titration has reached the equivalence point if there is a sudden change of pH in the solution . pH is the negative logarithm in base 10 of [H+] and related to the hydrogen ion concentration. pH = -log10[H+] pH scale varies according to the basicity and acidity of a solution. The pH of a neutral solution is 7.00 at 25C. If the pH is below 7.00 the solution is considered as an acid whereas if it is above 7.00, it is referred as a basic solution. The pH of a solution can be measured quickly and accurately with a pH meter. The electrode of the pH meter was inserted into a beaker with required acid while the solution was titrated with NaOH solution. The hydrogen ions will be neutralized as NaOH is incrementally added to the acid solution in which resulting to the increased of the pH of that particular acid. After a sufficient amount of NaOH is added, the next drop of NaOH will cause a sudden sharp increase in pH. The equivalence point of titration indicates the volume of based required to completely neutralized the acid.

Figure 2 Titration curve of weak acid titrated with NaOH

During this experiment was conducted, titration of a vinegar sample with a standardized NaOH solution will be performed. In order to standardize the NaOH solution, a primary standard acid solution is initially prepared. Potassium hydrogen phthalate (KHC8H4O4) and oxalic acid (COOH)2 were commonly used as a primary standard acid while sodium carbonate, Na2CO3, is the commonly used base. Potassium hydrogen phthalate (KHP) was used throughout this experiment as a primary standard acid. The KHP was produced by dissolving around 1.500g with 30 mL of distilled water. In order to choose the standard acid or even bases,they must have at least these characteristics: available in at least 99.9 purity have high molar mass stable upon heating must be soluble in the required solvent The reaction equation of this reaction between KHP and NaOH solution is shown below: KHC8H4O4(aq) + NaOH(aq) KNaC8H4O4(aq) + H2O(l) [Eq. 4] After the NaOH solution was standardized, the process of titration with 10.0 mL aliquots of vinegar began. The equation of the reaction is: CH3COOH(aq) + NaOH(aq) NaCH3COO(aq) + H2O(l) [Eq. 5] By referring to the equation above, the molarity and the percent by mass of acetic acid can be determined.

METHODOLOGY

Material and Apparatus Solid NaOH Distilled water KHP Beakers Measuring cylinder Magnetic stirrer pH meter Vinegar 10 mL volumetric pipette Analytical Balance

Prodecure Experiment A Standardization of Sodium Hydroxide Solution 1. 250 mL of approximately 0.6 M sodium hydroxide solution was prepared from NaOH solid. The solution was prepared in a beaker after the calculation was checked with the laboratory instructor. The calculation was recorded. 2. The beaker was placed and tarred on the balance. 1.5 grams of KHP was added to the beaker. The mass of the KHP was recorded to the nearest 0.001 g. 30 mL of distilled water was added. The solution was stirred with magnetic stirrer until the KHP has dissolved completely. 3. The solution was titrated with NaOH and the pH was recorded with 1 mL additions of NaOH solution. 4. Steps 1 to 3 were repeated and two more solutions for NaOH standardization were prepared. 5. The graph of pH versus NaOH was plotted. The volume of NaOH required to neutralize the KHP solution in each titration were determined from the plots 6. The molarity of sodium hydroxide for titrations 1, 2 and 3 was calculated. 7. The average molarity of sodium hydroxide solution was calculated. The resulting sodium hydroxide concentration was used in part B of the experiment. 6

Experiment B Molarity of acetic acid and mass percent in vinegar 1. 10.00 mL of vinegar was transferred to a clean, dry 250 mL beaker using a 10 mL volumetric pipette. 90.0 mL of water was added in order to cover the pH electrode tip during the titration. 2. 1.0 mL of NaOH was added to the vinegar solution and the pH was recorded. 3. The above steps was repeated twice more. 4. The graph of pH vs NaOH was plotted and from the plots, the volume of NaOH required to neutralize the vinegar in each titration. The data was recorded. 5. The molarity of acetic acid was calculated for titrations 1, 2 and 3. 6. The average molarity of acetic acid for each titration was calculated. 7. The percent by mass of acetic acid in vinegar was calculated for titrations 1, 2 and 3. 8. The percent by mass of acetic acid in vinegar was calculated.

RESULTS

Experiment A

KHP Titrated With NaOH

14.00

12.00

10.00

8.00 pH 6.00 4.00 2.00 0.00 0.00 5.00 10.00

12.50

15.00

20.00

Volume of NaOH (mL)

Graph 1 - Titration 1

KHP Titrated With NaOH

14.00

12.00

10.00

8.00

6.00

4.00

2.00

0.00 0.00 5.00 10.00

12.50

15.00

20.00

Volume of NaOH (mL)

Graph 2 - Titration 2

KHP Titrated With NaOH

14.00

12.00

10.00

8.00 pH 6.00 4.00 2.00 0.00 0.00 5.00 10.00 12.00 Volume of NaOH (mL) 15.00 20.00

Graph 3 - Titration 3

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Experiment B

Vinegar Titrated With NaOH

14.00

12.00

10.00

8.00 pH 6.00 4.00 2.00 0.00 0.00 5.00 10.00 mL of NaOH

14.00 15.00

20.00

Graph 4 - Titration 1

11

Vinegar Titrated With NaOH

14.00
Graph 7 - TItration 2

12.00

10.00

8.00 pH 6.00 4.00 2.00 0.00 0.00 5.00 10.00

12.00

15.00

20.00

mL of NaOH

Graph 6 - Titration 2

12

Vinegar Titrated With NaOH

14.00

12.00

10.00

8.00 pH 6.00 4.00 2.00 0.00 0.00 5.00 10.00 mL of NaOH

15.00

16.00

20.00

25.00

Graph 8 - Titration 3

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Experiment A Titration 1 Mass of KHP (g) Volume of NaOH to neutralize the KHP solution (mL) Molarity of NaOH (M) Average molarity (M) 0.5884 0.5881 0.5964
Table 1 - Tabulation data for Experiment A

Titration 2 1.5011

Titration 3 1.5015

1.5018

12.50

12.50

12.00

0.6128

Experiment B

Titration 1 Volume of NaOH to neutralize the vinegar solution (mL) Molarity of Acetic Acid (M) Average molarity (M) % by mass of acid in vinegar (%) Average percent by mass of acetic acid in vinegar (%) 14.00

Titration 2

Titration 3

12.00

16.00

0.8350

0.7157

0.9542

0.8350

5.0150

4.2980

5.0146

5.0146

Table 2 - Tabulation Data of Experiment B

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CALCULATIONS

Experiment A Calculation of the moles of KHP used in the first titration:

CH3COOH(aq) + NaOH(aq) NaCH3COO(aq) + H2O(l) From equation above, the moles of NaOH is required to neutralize the moles of KHP can be calculated.

Thus, the molarity of the NaOH can be calculated like below:

The average molarity of NaOH:

0.5964 M

Experiment 2 Calculation of the moles of NaOH that reacted:

CH3COOH(aq) + NaOH(aq) NaCH3COO(aq) + H2O(l) Calculation of the moles of CH3COOH neutralized by the moles of NaOH by using the equation above:

Calculation of the molarity of the CH3COOH solution:

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 Average molarity of acetic acid for each titration:

= 0.8350 M CH3COOH Calculation of the mass of acetic acid in the solution:

Calculation of the mass of the acetic acid solution:

Calculation of the percent by mass of acetic acid in the solution:

Average percentage by mass of acetic acid in vinegar

= 5.0146 %

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DISCUSSION

Acetic acid (CH3COOH) or ethanoic acid as in IUPAC name is the major component of vinegar, other than water. This acid is classified as a type of weak acid. However, concentrated acetic acid is corrosive and harmful to the skin. Vinegar is produces by fermentation of ethanol . The aim of this experiment was to determine the molarity of a solution and the percent by mass of acetic acid in vinegar by titration with a standardized sodium hydroxide (NaOH) solution. The reaction involved can be considered the neutralization of the vinegar and NaOH solution whereby an acid and a base are combined until certain point. The most suitable process to get the most accurate results for this experiment is via titration process. Titration is a process where small increments of a solution are added to a specific volume of solution until the stoichiometry is obtained. Therefore, the equivalence point of the reaction can be determined. By knowing the equivalence point, the molarity, mass and percent by mass of the acetic acid (CH3COOH) can also be determined. In Experiment A, NaOH solution was initially prepared for both of the experiment. In order to standardize the NaOH solution, a primary standard acid solution is initially prepared. In this case, potassium hydrogen phthalate, KHC8H4O4 (KHP) was chosen as they have high molar mass. The KHP was measured at 1.5 g and added with 30 mL of distilled water into a beaker. The solution was stirred until the KHP dissolved completely. After the preparation was done, the KHP solution was titrated with the NaOH solution until sudden change in the pH reading. The experiment was repeated two more times and recorded. After the readings were recorded, the graphs were plotted and thus, the equivalence point can be obtained. By using the Eq. 1, molarity of NaOH solution can be calculated for all the titration. All of the molarity are added and divided with three to get the average molarity of NaOH. The molarity of NaOH are 0.5884 M, 0.5881 M and 0.6128 M for Titration 1, 2 and 3 respectively. The average molarity of NaOH are 0.5964 M. Meanwhile, in Experiment B, the KHP solution was replaced with vinegar. The solution was titrated with NaOH solution that was prepared earlier 1 mL at one time. The solution was titrated until a sudden change in the pH reading noted. The reading were recorded and the 17

experiment was repeated twice more. The graphs are plotted and the equivalence points were determined. With these equivalence points, the molarity of acetic acid for each titration were calculated. The molarity of acetic acid in the first titration was 0.8350 M. On the other hand, the molarity of acetic acid in titration 2 and 3 were 0.7157 M and 0.9542 M respectively. All of the molarity reading were added and divided with three to get the average molarity of acetic acid which is 0.8350 M. Last but not least, by using the molarity of acetic acid, the percent by mass of acetic acid in vinegar for each titration can be calculated, and the average percent by mass of acetic acid in vinegar was 5.0146 %. According to a webpage vinegar contains of about 4.0 % of acetic acid[1]. The percentage error was high which is 25.37 %. Therefore, it can be concluded that some errors had occurred. In order to minimize the error, the experiment must be repeated until several times and the average is taken. Other than that, the mass of solid KHP and NaOH must be taken carefully and precisely. The beaker must be tarred to get the exact mass of the solid. In order to have the slightest error, the solid must be placed inside the beaker outside the range of the balance. This is to ensure that there are no solid fall onto the balance and affect the reading. In addition, the reading of the burette must be taken perpendicularly to the meniscus in order to avoid parallex error. Magnetic stirrer and analytical balance must be used throughout this experiment to stir those acids. This is to ensure uniform concentration of the solution inside the beaker. Last but not least, the electrode of the pH meter must be dipped thoroughly to ensure no disturbance in the pH reading.

18

CONCLUSION

From this experiment, it can be concluded that the molarity of a solution and percent by mass of acetic acid in vinegar by titration with a NaOH solution can be determined by the graphs of the results. The graphs contributes a lot to determine the point where both of the solutions are neutralize completely. After the equivalence point was reached, the molarity of NaOH and acetic acid can be calculated. The percent by mass of acetic acid in vinegar for each titration is 5.0146%. The experiment was a success.

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RECOMMENDATIONS

There are a few recommendations in order to minimize the error. First of all, the experiment must be repeated until several times and the average is taken. Other than that, the mass of solid KHP and NaOH must be taken accurately. The solid must be placed inside the beaker outside the range of the balance. This is to ensure that there are no solid fall onto the balance and affect the reading. Other than that, the reading of the burette must be taken perpendicularly to the meniscus in order to avoid parallex error. Magnetic stirrer and analytical balance can be used throughout this experiment to stir those acids as a safety measures. This is to ensure uniform concentration of the solution inside the beaker. Last but not least, the electrode of the pH meter must be dipped thoroughly to ensure no disturbance in the pH reading.

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REFERENCES

[1]Acetic Acid. (2011, October 8). Retrieved October 9, 2011, from Wikipedia: http://en.wikipedia.org/wiki/Acetic_acid [2]Brown, T. L., LeMay, H. E., Bursten, B. E., & Murphy, C. J. (2009). Chemistry The Central Science. NJ: Pearson Education, Inc. [3]Chang, R. (2010). Chemistry Tenth Edition (10th Edition ed.). Singapore: McGraw-Hill. [4] Freddy Thomas, Eric Jamin, 2H NMR and 13C-IRMS analyses of acetic acid from vinegar, 18O-IRMS analysis of water in vinegar: International collaborative study report, Analytica Chimica Acta, Volume 649, Issue 1, 1 September 2009, Pages 98-105, ISSN 0003-2670, 10.1016/j.aca.2009.07.014.
[5]

A. Caligiani, D. Acquotti, G. Palla, V. Bocchi, Identification and quantification of the main

organic components of vinegars by high resolution 1H NMR spectroscopy, Analytica Chimica Acta, Volume 585, Issue 1, 28 February 2007, Pages 110-119, ISSN 0003-2670, 10.1016/j.aca.2006.12.016. [6] ke Olin, Bo Walln, A note on the calculation of acid-base titration curves and their equivalence points, Talanta, Volume 25, Issues 11-12, November-December 1978, Pages 720721, ISSN 0039-9140, 10.1016/0039-9140(78)80186-6.

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APPENDICES

Sample Calculation of Standardizing NaOH with KHP

The figure below presents the titration curve of 1.523 g of KHP dissolved in 20.0 mL of distilled water.

Figure 3 The volume of NaOH used at the equivalence point is 15.3 mL

Calculation of the moles of KHP used in the titration:

From Eq. 5, the moles of NaOH is required to neutralize the moles of KHP can be calculated.

Thus, the molarity of the NaOH can be calculated like below:

Sample calculations to determine the concentration of acetic acid in vinegar Calculation of the moles of NaOH that reacted:

Calculation of the moles of CH3COOH neutralized by the moles of NaOH:

Calculation of the molarity of the CH3COOH solution: 22

 Calculation of the mass of acetic acid in the solution:

Calculation of the mass of the acetic acid solution:

Calculation of the percent by mass of acetic acid in the solution:

Calculation of error in this experiment

23