CHEM4441 ANALYTICAL CHEMISTRY II

EXPERIMENT 1:An exercise in volumetric analysis

Objective:

This experiment intends to refresh your skills regarding volumetric analysis by preparing primary standards,
standardization of a reagent and analysis of vinegar samples for the content of acetic acid.

Equipment
Analytical balance
10 mL micro-burette
5 mL pipettes Conical
flask (50 mL)
50 and 250 volumetric flasks
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Chemicals

Solid sodium hydroxide – solid potassium hydrogen phthalate

and phenolphthalein indicator
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Experiment
In order to carry out accurate volumetric analysis (In your introduction you should discuss
volumetric titration) , it is necessary to be able to make up a standard solution using the analytical
balance, to be able to accurately pipette solutions, and to be able to carry out a titration to the
required level of accuracy. The following exercise gives practice in all of these. In this experiment,
you will prepare a solution of NaOH with an approximate concentration of 0.1 M, which will be
later standardized by a primary standard acid, sodium or potassium hydrogen phthalate (KHP). (In
your introduction, you need to define primary standards, discuss their characteristics, give
example of acid and base primary standards, and why NaOH is not a primary standard).

Fig. 2 Chemical Structure of NaKHP

(1) Preparation of an approximately 0.1M solution of NaOH

Because it is hygroscopic, NaOH always contains alkali carbonate and water, and cannot be used
directly for the preparation of a standard solution. An approximately 0.1 M solution can be
prepared as follows.
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Weigh out rapidly about 1.0 g of A.R. sodium hydroxide on a weighing boat (using a top loading
balance), dissolve it in about 50 ml of CO2 free distilled water, and transfer it to a 250 mL
volumetric flask and make up to the mark with distilled water.
(Remember: the molarity of this solution is not known accurately)

(2) Preparation of 0.1M potassium hydrogen phthalate

 potassium hydrogen phthalate [KH(C8H4O4)] (KHP) (Analytical reagent grade (A.R.)) has
an RMM of 204.22 and a purity of at least 99.9 % and can be used to make a standard
solution. Before its use, it should be dried at 120 oC for 2 hours and allowed to cool in a
covered desiccator (This has already been done for you by our kind technicians).

 Weigh out accurately about 1.00 g of A.R. potassium hydrogen phthalate, dissolve it in
distilled water, and transfer it to a 50 mL volumetric flask and make up to the mark.
 Calculate the molarity (To four digits) of the solution from the weight of solid taken. (Why
here the concentration of the acid is directly obtained from the weighed mass?)

(3) Standardization of NaOH solution against standard KHP

 Titrate 5.00 mL aliquots of KHP against the approx. 0.1M NaOH using phenolphthalein as
indicator. Titrate to the first permanent (30 sec) pale pink color (You can easily calculate
the approximate volume of NaOH needed to reach the endpoint, MaVa = MbVb for a 1:1
molar ratio reaction).
 Repeat the titration 4 times using fresh aliquots of KH(C8H4O4). Individual titrations
should be within 0.010 or 0.020 mL. Calculate the molarity of NaOH from the equation.

 KH(C8H4O4) + NaOH NaK(C8H4O4) + H2O

 What is the standard deviation on the molarity of NaOH? Using the Student t test from your
textbook calculate the 95 % confidence interval for your results.

Determination of acetic acid in vinegar

Vinegar consists mainly of a 4 to 6 % solution of acetic acid. Acetic acid is a weak acid
and can be titrated with 0.1 M NaOH using phenolphthalein as indicator. Because the
concentration of vinegar is high, it is convenient to dilute the sample and to use aliquots
for the titration.

Transfer 5.0 mL of vinegar to a 50.0 mL volumetric flask and make up to the mark with
deionized water. Pipette a 5.00 mL aliquot into a conical flask, and 2 drops of
phenolphthalein indicator. Titrate against the standardized NaOH to the first permanent
pink endpoint. Carry out the determination in 3-4 times (The more titrations you run the
better results you obtain). Individual titrations should not differ by more than 0.10 mL.

1) Report the percent (weight-volume) acetic acid in the vinegar.

2) From a consideration of errors in the experiment, estimate the precision of the acetic acid
determination.
3) The accurate concentration of KH(C8H4O4) in this experiment was calculated directly from
its mass, whereas that of NaOH was not obtained using its mass Explain.

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Notes
 Dispose the chemical solutions in this experiment under running tap water for 5 minutes.
 Clean your glassware and put them back in their locations (Be careful with the microburette
as it is fragile).
 Leave your bench tidy as before work.
 Sign your notebook from your lab instructor before you leave the lab. An example of an
acceptable notebook is given below!