1.

0 INTRODUCTION Titration is a common laboratory method of quantitative chemical analysis that is used to determine the unknown concentration of a known reactant. A reagent is called the titrant, of a known concentration and volume is used to react with a solution of the titrant, whose concentration is not known. Using a calibrated burette to add the titrant, it is possible to determine the exact amount that has been consumed when the endpoint is reached. The endpoint is the point at which the titration is complete, as determined by an indicator. This is ideally the same volume as the equivalent point where the volume of added titrant at which the number of moles of titrant is equal to the number of moles of analyte. In the titration, the endpoint of a titration is the point at which the pH of the reactant is just about equal to 7, and often when the solution permanently changes color due to an indicator. Titration can be used to determine when is the acid and base concentrations are at equilibrium by using indicator. Although other techniques can be used, this method is the most accurate way in order to determine it. The acid being titrated with phenolphthalein indicator and the base (NaOH) will be placed in the burette. The amount of base needed to neutralize or comes to neutralization of the acid is determined by the amount needed to turn the solution to slight pink colour. Therefore, the pH of the solution can be found by using electronic pH meter. By using this meter and titration, the volume of titrant (ml) used throughout the titration and the changes of pH of the acid up to 11 can be recorded. This data will be used to make a titration curve.

2.0 OBJECTIVES The objectives of this experiment are : Being exposed to the correct and proper ways of titration techniques To determine how much strong base (NaOH) is needed to titrate weak acid (CH3COOH) To determine how much strong base (NaOH) is needed to titrate strong acid (HCl) To determine the equivalence point of the reaction To determine the acid dissociation constant, Ka and pKa of acetic acid by using Henderson-Hasselbach equation To determine the titration curve for strong acid-strong base and weak acid-strong base

3.0 METHODOLOGY

1. 50 ml of 10 times dilution of vinegar solution was prepared 2. The apparatus were set up as shown in figure. 3. A burette was filled with 50 ml of 0.1M solution of sodium hydroxide (NaOH) and the liquid in the burette was allowed to come down to zero mark and the tap was closed. 4. 1 ml of NaOH was slowly dripped into the solution to be titrated and was mixed slowly by the stirrer. The pH and the volume of NaOH added was recorded only after the pH is stable. 5. The data was recorded until the pH of solution reach 11. The graph of pH solution against total volume of NaOH added was plotted. 6. Steps 1-5 were repeated by using 50ml of 0.1M of strong acid, HCl being titrated by same amount and molarity of strong base.

4.0 RESULT

pH of weak acid The volume of NaOH added (ml) 0.0 1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0 10.0 11.0 12.0 13.0 14.0 2.95 3.28 3.43 3.64 3.80 3.95 4.04 4.17 4.26 4.34 4.36 4.40 4.50 4.55 4.60 Vinegar (CH3COOH)

pH of strong acid (HCl) 1.40 1.52 1.41 1.45 1.57 1.60 1.56 1.52 1.57 1.60 1.73 1.78 1.77 1.83 1.90

15.0 16.0 17.0 18.0 19.0 20.0 21.0 22.0 23.0 24.0 25.0 26.0 27.0 28.0 29.0 30.0 31.0 32.0 33.0 34.0 35.0 36.0

4.68 4.70 4.76 4.85 4.90 4.95 5.04 5.14 5.24 5.32 5.41 5.45 5.51 5.63 5.83 6.03 6.43 10.40 11.08

1.81 1.92 2.00 2.11 2.13 2.14 2.20 2.30 2.54 3.25 5.83 6.38 6.40 6.85 6.86 6.92 6.93 6.97 7.01 7.02 7.03 7.04

Table 1 : Table data of amount of strong base in ml of NaOH and pH of weak acid, CH3COOH and also strong acid, HCl.

5.0 DISCUSSION

Titration curve of titrating Strong Base and Strong Acid

8 7 6 pH of Strong Acid 5 4 3 2 1 0 0 10 20 30 40 Vol. of Strong Base (ml) titration curve of Strong Base-Strong Acid

Graph 1 : Graph of titration curve of titrating strong base, NaOH and strong acid, HCl

For titration of strong base titrating a strong acid, the reaction can be shown as : NaOH(aq) + HCl(aq) NaCl(aq) + H2O(l) From this experiment, 50 ml of 0.1M of strong acid, NaOH is being titrated to the 50 ml of 0.1M of strong acid HCl. The pH of an acid solution is plotted against the amount of base added during a titration, the shape of the graph is called a titration curve. All acid titration curves follow the same basic shapes.

At the beginning, the solution has a low pH as it is a strong acid and climbs as the strong base is added. As the solution nears the point where all of the H+ are neutralized, the pH rises sharply and then levels out again as the solution becomes more basic as more OH- ions are added. The first curve shows a strong acid being titrated by a strong base. There is the initial slow rise in pH until the reaction nears the point where just enough base is added to neutralize all the initial acid. This point is called the equivalence point. For a strong acid or base reaction, this occurs at pH = 7. As the solution passes the equivalence point, the pH slows its increase where the solution approaches the pH of the titration solution. As the OH- is steadily added, the H+ ions are neutralised to water, so the H+ concentration steadily falls and the pH rises as the solution becomes less acid. At pH 7, the amount of NaOH needed to titrate HCl is 33.0 ml. Based on the titration curve, the equivalent point does not lie under pH 7. This might due to some errors. However, the equivalent point is at pH 5.83 which the amount of NaOH added is 25.0 ml. There are very tiny equal concentrations of H+ and OH- (due to the self-ionisation of water). If excess alkali is added the pH steadily rises to around 11 as the concentration of OH- from the alkali rises and the solution becomes more alkaline.

Titration curve of Titrating Strong Base and Weak Acid

12 10 pH of Weak Acid 8 6 4 2 0 0 10 20 30 40 Vol. of strong base (ml) Titration curve of strong base-weak acid

Graph 2 : Graph of titration curve of titrating strong base, NaOH and weak acid, CH3COOH.

For strong base and weak acid titration, CH3COOH which is a weak acid and sodium hydroxide, NaOH which is a strong base. The reaction can be shown as: CH3COOH (aq) + NaOH (aq) CH3COONa (aq) + H2O (l)

From this experiment, 50 ml of 0.1M of strong acid, NaOH is being titrated to the 50 ml of 0.1M of weak acid CH3COOH . The titration curve is shown in figure below. In this reaction, from the weak acid the free H+ ion will neutralized by OH- ions from the base. There are several characteristics that can be seen in the titration curve of weak acid with strong base.

The initial pH (before adding strong base) is higher or less acidic and there is a sharp increase in pH at the beginning of titration due to the anion of the weak acid becomes a common ion that reduces the ionization of the acid. After a sharp increase at the beginning of the titration, the curve only change gradually. This is due to the solution act as buffer. It will be continued until the base overcomes the buffer capacity. The half-neutralization will occur in the middle of the gradually curve. At this point, the concentration of weak acid is equal to the concentration of its conjugant base. Therefore, here the pH = pKa. It is called half-neutralization because half of the acid has been neutralized. At equivalence point the pH is not 7 because the sodium acetate, CH3COONa formed after the neutralization reacts with water to give OH- ions. This decreases H+ ions concentration and pH is about 8.7 at equivalence point. In this experiment, only little amount of strong base, NaOH which is around 31.50 ml needed to raise the large pH of weak acid, CH3COOH from 6.43 to 10.00. Near the equivalence point pH change is observed from about 6.43 to 10.0 by the addition of small amount of NaOH because the conjugant base of the weak acid hydrolyzed and produces the hydroxide ion. While the steep portion of the curve prior to the equivalence point is short. It will be occur until the pH become around 11.

Generally ;

Acid + Base Salt + Water

For weak acid and strong base, the balance chemical equation is :

CH3COOH(aq) + NaOH(aq) CH3COONa(aq) + H2O(l)

For strong acid and strong base, the balance chemical equation is :

HCl(aq) + NaOH(aq) NaCl(aq) + H2O(l)

The concept that were used in this experiment deal with acid-base titration and equilibrium. Most importantly, the concept of the equivalence point was applied. At the equivalence point, the moles of the acid present are equal to the moles of base present. For a reaction a stage which shows the completion of a particular reaction is known as end point. Equivalence point is a stage in which the amount of reagent added is exactly and stoichiometrically equivalent to the amount of the reacting substance in the titrated solution. The end point is detected by some physical change produced by the solution, by itself or more usually by the addition of an auxiliary reagent known as an 'indicator'. The end point and the equivalence point may not be identical. End point is usually detected only after adding a slight excess of the titrant.

An acid dissociation constant, Ka, (also known as acidity constant, or acid-ionization constant) is aquantitative measure of the strength of an acid in solution. It is the equilibrium constant for a chemical reaction known as dissociation in the context of acid-base reactions. The equilibrium reaction for acetic acid can be written as:

CH3COOH
Acetic Acid (weak acid)

H+ + CH3COO Acetate anion (conjugate base)

Ka =
Whereas;

[ [

] [ ]

Ka = acid dissociation constant [CH3COO -] = concentration of conjugate base [H+] = concentration of hydrogen ion [HA]= concentration of weak acid

Ka for acetic acid is 1.76 x 10-5M. This is because the Ka value is numerically small and inconvenient in calculations. The pKa is defined by analogy with pH.

In this experiment, the pKa = - log10 (1.76 x 10-5) = 4.755

The larger the value of pKa the smaller the extent of dissociation at any given pH. Weak acid has a pKa value in the approximate range 2 to 12 in water. Acids with a pKa value of less than -2 are said to be strong acids. The acid dissociation constants (Ka) provides a measure of the equilibrium position. If Ka is large, the products of the dissociation reaction are favoured meanwhile if the Ka is small, undissociated acid is favoured. Therefore, Ka provides a measure of the strength of an acid. If Ka is large, it shows that the acid is largely dissociated so the acid is strong. However, if the Ka is small, it is very little amount of acid is dissociated so the acid is weak.

The molarity of acetic acid in the titrated solution can be calculated by formula : M1V1 = M2V2 M1 = Molarity of Acetic Acid V1 = Volume of Acetic Acid M2 = Molarity of acetic acid in titrated solution V2 = total volume of acetic acid and titrated solution

0.1M (50ml) = M2 (100ml)

M2 =

= 0.05M

The percentage of acetic acid present in Vinegar can be calculated.

*to neutralize the vinegar , the graph reads 50 ml was needed. 36 mL x 0.1 M = 3.6 millimoles of NaOH 0.0036 mole x 60 g/mole = 0.216g CH3COOH ( 0.00216 g CH3COOH / 50 g of vinegar ) * 100% = 0.432 %

6.0 CONCLUSION

From this experiment, the volume of strong base, NaOH needed to titrate strong acid, HCl until the titrating curve reach the equivalent point which is 7 can be known but in this experiment, pH 7 in not lie under the equivalent line on the titration curve. The suitable pH that lie under the equivalent curve is pH 5.8 where the volume of strong base need in the titration is 25.0 ml. This might be due to some errors. However, the volume of NaOH needed is 33.0 ml. The same things goes to the volume of strong base, NaOH needed to titrate weak acid, CH3COOH until the titrating curve reach the equivalent point which is around 6.43 to 10.0 can be known. The volume of NaOH needed is about 31.50 ml. The titration curve also can be plotted by key in the data. Therefore, there are some errors might occur in this experiment that can affect the results. For example, the apparatus used is contaminated with unneeded substance or solution. However, it can be prevented by rinsing all the apparatus with distilled water. If not, it will affect the results. Secondly is about the electronic pH meter. Make sure it is well function by testing it with the already known pH solution such as buffer solution. Then, the reading can be calibrated to make sure that the results obtained is accurate. Therefore, make sure that amount of solution is accurate by considering the meniscus level. For example the usage of burette and measuring cylinder. Make sure that eyes are parallel to the reading to avoid parallax error. This actions need to be taken in order to make the needed solution is accurate to contribute the more accurate result in the future.

7.0 REFERENCES 1. David E. Goldberg, Mc Graw Hill, Fundamental of Chemistry, 303. 2. Levie, Robert De. Aqueous Acid-Base Equilibrium and Titrations. New York: Oxford
University Press Inc. 1991 3. H. Robert Horton, Laurence A. Moran, K. Gray Scrimgeour, Marc D. Perry, J. David Rawn: Principles of Biochemistry, 4th edition, Pearson Prentice Hall. 2007. 4. http://chemistry.about.com/od/acidsbase1/ss/titrationcurves.htm 5. http://www.scribd.com/doc/20300492/Experiment-3-Acid-and-Base-Titration