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Titration Page 1 of 5

ACID AND BASE TITRATION

REFERENCES: Nelson, J., Chemistry:The Central Science, 3rd Edition, Prentice-Hall, 1985

This experiment will demonstrate the techniques of volumetric analysis or titration. Here, a quantitative determination of the amount of acid in an unknown sample will be made.

Apparatus and Chemicals

500 mL Erlenmeyer flask

3

1–pint bottles with caps

50

mL Class A buret

Phenolphthalein solution

Buret clamp

Potassium acid phthalate (primary standard)

Ring stand

3

250 mL Erlenmeyer flasks

19

M NaOH

Weighing bottle

Balance

Unknown acid

Wash bottle

600 mL beaker

Discussion

One of the most common and familiar reactions in chemistry is the reaction of an acid with a base. This reaction is termed neutralization, and the essential feature of this process in aqueous solution is the combination of hydronium ions with hydroxide ions to form water:

H 3 O + (aq) + OH (aq) 2H 2 O(l)

In this experiment you will use the above reaction to accurately determine the concentration of a sodium hydroxide solution that you have prepared. The process of determining the concentration of a solution is called standardization. Next you will measure the amount of acid present in an unknown. To do this, you will accurately measure with a buret the volume of your standard base that is required to exactly neutralize the acid present in the unknown. The technique of accurately measuring the volume of a solution required to react with another reagent is termed titration.

An indicator solution is used to determine when an acid has exactly neutralized a base, or vice versa. A suitable indicator changes colors at well-defined pH values; if this pH value corresponds to the pH region in which equivalent amounts of acid and base are present during a trtration experiment, we can use the color change to determine the stoichiometric point. The color change is termed the end point of the titration. Different indicators change colors at different pH values. Phenolphthalein, for example, changes color from colorless to pink at a pH of about 9; in slightly more acidic solutions it is colorless, while in slightly more alkaline solutions it is pink.

Titration Page 2 of 5 In this experiment your solution of NaOH will be standardized by titrating it against a very pure sample of potassium acid phthalate, (KHC 8 H 4 O 4 ) of known mass. Potassium acid phthalate (henceforth abbreviated as KHP) has only one replaceable acid hydrogen (indicated in BOLD). Its structure is shown below. It is a monoprotic acid with the acidic hydrogen bonded to oxygen and has a molecular weight of 204.2 g/mole.

H

H

H O C C H C C O C C O - K + C
H
O
C
C
H
C
C
O
C
C
O - K +
C
C
H O

Or

COO H COOK (in shorthand notation)
COO H
COOK
(in shorthand notation)

In the titration of a base against KHP, an equal number of moles of base and acid are present at the end point (moles NaOH = moles KHP) or

are present at the end point (moles NaOH = moles KHP) or COO H   +

COO H

 

+

Na +

+ OH -

COOK

KHP) or COO H   + Na + + OH - COOK COO N a COOK
KHP) or COO H   + Na + + OH - COOK COO N a COOK

COO

or COO H   + Na + + OH - COOK COO N a COOK Once

Na

COOK

Once the end point has been reached then the exact molarity can be calculated by dividing the volume of base that was titrated (in liters) into the moles of NaOH present.

moles NaOH ÷ volume of base titrated (L) = M of NaOH in stock bottle

Now that the exact concentration of NaOH is known, a sample containing an unknown amount of KHP (or any other acid, for that matter) can then be determined.

Example of Standardization

0.3043 g of pure KHP was weighed out and titrated to an end point with 15.12 mL of a NaOH solution that was approximately 0.1 M. What is the exact concentration of the NaOH titrant?

0.3043 g KHP ÷ 204.2 g/mole = 1.490 x 10 3 mole KHP

At the end point:

1.490 x 10 3 mole KHP = 1.490 x 10 3 mole NaOH titrated

therefore,

1.490 x 10 3 mole NaOH ÷ 0.01512 L of NaOH titrated = 0.09854 M NaOH exactly

Titration Page 3 of 5 Once the exact molarity of the NaOH solution is known, the base can be used to determine the amount of KHP or any other acid present in a known mass of an impure sample.

Example: The percentage determination of an acid in an unknown sample.

0.5366 g of an KHP sample of unknown purity was massed. The sample was dissolved in approximately 100 mL of distilled, degassed water and indicator was added. The end point was reached after 21.35 mL of 0.09854 M NaOH solution was titrated into the solution. What is the percentage of KHP in the original sample?

At the end point:

0.09854 moles/L NaOH x 0.02135 L = 0.002104 moles NaOH

0.002104 moles NaOH = 0.002104 moles JHP = 0.4296 g KHP

therefore,

(0.4296 g KHP ÷ 0.5366 g sample) * 100% = 80.06% KHP in the unknown sample

Procedure

Preparation of approximately 0.1000 M Sodium hydroxide.

Heat a total of 1500 mL of distilled water to boiling using no larger than 600 mL beakers, and after cooling under the water tap, transfer to three 1-pint bottles fitted with caps. Add 3 mL of stock solution of carbonate-free sodium hydroxide (approximately 19 M) to only one of the pint bottles and shake vigorously for at least 1 minute. The other 2 pint bottles containing the CO 2 - free water will be used for the remainder of the experiment.

Preparation of a buret for use.

Clean a 50 mL, class A buret with soap solution and a buret brush and thoroughly rinse with tap water. Then rinse with at least five 10 mL portions of distilled water. The water must run freely from the buret without leaving any drops adhering to the sides. Make sure that the buret does not leak and that the stopcock turns freely.

Reading a buret.

All liquids, when placed in a buret, form a curved meniscus at their upper surfaces. In the case of water or water solutions, this meniscus is concave ( ), and the most accurate buret readings are obtained by observing the position of the lowest point on the meniscus on the graduated scales.

To avoid parallax errors when taking readings, the eye must be on a level with the meniscus. Obtain a 3 × 5 card. Color a 2 × 1 box in solid black ink in the center of the card. When taking a volume reading involving the meniscus, hold the card so that the lowest part of the meniscus is even with the "top" of the black colored box.

Titration Page 4 of 5

STANDARDIZATION OF SODIUM HYDROXIDE SOLUTION

Mass from a weighing bottle (your lab instructor will show you how to use a weighing bottle if you do not already know) triplicate samples of between 0.4 and 0.6 grams each of pure KHP into 250 mL Erlenmeyer flasks; accurately weigh to four significant figures. Do not weigh the flasks. Record the masses and label the three flasks in order to distinguish them from one another. Add to each sample about 100 mL of CO 2 -free distilled water and warm gently with swirling until the salt is completely dissolved. Add to each flask two drops of phenolphthalein indicator solution.

Rinse the previously cleaned buret with at least four 5 mL portions of the approximately 0.1000 M sodium hydroxide solution that you have prepared. Discard each portion. Do not return any

Completely fill the buret with the solution and remove the air

from the tip by running out some of the liquid into an empty beaker. Make sure that the lower part of the meniscus is near the zero mark. Allow the buret to stand for at least 30 seconds before reading the exact position of the meniscus. Remove any hanging drop from the buret tip by touching it to the side of the beaker used for the washings. Record the initial buret reading.

of the wash.ings to the bottle.

Slowly add the sodium hydroxide solution to one of your flasks of KHP solution while gently swirling the contents of the flask as illustrated in Figure 1. As the sodium hydroxide solution is added, a pink color appears where the drops of the base come in contact with the solution. This coloration disappears with swirling. As the end point is approached, the color disappears more slowly, at which time the sodium hydroxide should be added drop by drop. It is most important that the flask be swirled constantly throughout the entire titration. The end point is reached when one drop of the sodium hydroxide solution turns the entire solution in the flask from colorless to pink. This solution should remain pink when it is swirled. Allow the titrated solution to stand for at least 1 minute so the buret will drain properly. Remove any hanging drop from the buret tip by touching it to the side of the flask and wash down the sides of the flask with a stream of water from the wash bottle. Record the buret reading. Repeat this procedure with the other two samples.

Level of meniscus
Level of meniscus

Pull the stopcock in against the taper each time you turn it

Swirl the flask continuosly until one drop of titrant causes a color change thruout the entire solution

A sheet of white paper below the flask will help you to see the color change.

From the data you obtain in the three titrations, calculate the molarity of the sodium hydroxide solution to four significant figures.

Titration Page 5 of 5 The three determinations should agree within 1.0 percent. If they do not, the standardization should be repeated until agreement is reached. The average of the three acceptable determinations is taken as the molarity of the sodium hydroxide. Now, label your stock bottle of NaOH solution with this average value.

ANALYSIS OF AN UNKNOWN ACID

Calculate the approximate mass of unknown that should be taken to require about 30 mL of your standardized sodium hydroxide assuming that your unknown sample is 75 percent KHP.

Weigh by difference (from a weighing bottle) triplicate portions of the sample to four significant figures and place them in three separate clean 250 mL flasks. The sample size should be about the amount determined by the above computation. Dissolve the sample in 100 mL Of CO 2 -free distilled water and add two drops of phenolphthalein indicator solution. Titrate with your standard sodium hydroxide solution to the faintest visible shade of pink as described above in the standardization procedure. Calculate the percentage of potassium acid phthalate (KHP) in the samples. For best results the three determination should agree with 1.0 percent. Compute the standard deviation of your results.

Test your results by computing the average deviation from the mean. If one result is noticeably different from the others, perform an additional titration. If any result is more than two standard deviations away from the mean, and has a history of problems and/or possible error in preparation discard it and titrate another sample.

Name:

Titration Experiment Report Sheet

Standardization of NaOH Solution

 

Trial 1

Trial 2

Trial 3

Mass of bottle + KHP

     

Mass of bottle

     

Mass of KHP used

     

Final buret reading

   

Initial buret reading

     

mL of NaOH used

     

Molarity of NaOH

     

Average Molarity:

Standard deviation:

Show calculations for Molarity and standard deviation

Analysis of Unknown Acid

Unknown Number:

Name:

 

Trial 1

Trial 2

Trial 3

Mass of bottle + Unknown

     

Mass of bottle

     

Mass of Unknown used

     

Final buret reading

   

Initial buret reading

     

mL of NaOH used

     

Molarity of NaOH used

     

Moles of NaOH used

     

Mass of KHP in Unknown

     

Percent KHP in Unknown

     

Average Percent KHP:

Standard deviation:

Show calculations of percent KHP and standard deviation.