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PRACTICAL ASSIGNMENT 1 DETERMINATION OF SOLUTION CONCENTRATION OBEJCTIVES 1. To prepare and standardize the concentration of NAOH solution. 2.

To determine the concentration of an unknown, X solution.

INTRODUCTION In any titration, the analyte (in Erlenmeyer flask) would be determined by knowing the exactly amount of the reagent used (commonly known as titrant in burrette) that is required to completely react with the analyte. Knowledge of the ratio between acid and bases and also concentration of one solution permits calculation of the molarity of the other. The reagent may be standard solution of a chemical or an electrical current of known magnitude. Two basic methods are used to establish the concentration of such solution. There are 1. The direct method in which a carefully weighed quantity of a primary standard compound is dissolved in a soluble solvent and diluted to a known volume in a volumetric flask.
2. Standardization of the solution for titration analysis where the titrant

(or titration reagent e.g NaOH) need to be standardized before using for determination of the concentration of other solution. This process can be performed via titrating the titrant against
a. A weighed quantity of primary standard (in solution form). b. A weight quantity of secondary standard (in solution form).

c. A measured volume of another solution. A titrant that is standardized against a secondary standard or against another solution is sometimes referred to as a secondary standard solution. The concentration of a secondary solution is subject to a larger uncertainty than that to a primary standard solution.

TKA 2013/Analytical Chemistry/Practical 1

APPARATUS 1. Analytical balance 2. Weighing bottle 3. Erlenmeyer flask


4. Beaker 500 cm3

5. Volumetric flask 250 mL 6. Pipette 20 mL and 25 mL 7. Burette 50 mL

CHEMICALS AND MATERIALS 1. Sodium hydroxide powder 2. Solution of acid (HX) 3. Oxalate acid dihyrate 4. Distilled water 5. Phenolphthalein indicator.

PROCEDURE A. Preparation of NaOH Solution

1. Weigh a quantity of NaOH powder (must be calculate) by using analytical balance to prepare 500 mL solution of 0.2 M. 2. Transfer to the 500 mL clean beaker. Add distilled water until 500 mL of volume and swirl the solution using glass rod until homogenize.

B. Standardization of NaOH Solution


TKA 2013/Analytical Chemistry/Practical 1

1. Weigh accurately oxalate acid dehydrate (powder) that will

completely react with 25 35 mL of NaOH of solution (choose one volume for calculate the amount of acid to be weigh) above by using analytical balance. 2. Transfer the powder to the Erlenmeyer flask. Add distilled water to dilute the acid (the original volume is important here, Why?) 3. Prepare 3 to 4 sample. Preparation of sample at difference weigh is better and the reading should be note down.

C. Determination of concentration of X solution.

1. Pipette 25 mL of X acid solution into 250 mL volumetric flask. 2. Dilute with distilled water until reach the mark. Titrate 20 mL to 25 mL of this solution with reagent NaOH solution standardized above (in burrete).

NOTES Repeat the titration process at least three times to calculate the concentration. The relative deviation between the results must be below than 30. Do the calculation of deviation for every set reading. Show your result to your demonstrator and get the real value. Calculate te error percentage of your result.

QUESTIONS 1. Sodium hydroxide adsorbs water and carbon dioxide from air. How to store the sodium hydroxide solution? What is the effect on your titration if this solution will expose to the air?

TKA 2013/Analytical Chemistry/Practical 1

2. Briefly explain the structure of the phenolphthalein indicator and the reaction of the color exchange in your titration.

CALCULATION OF THE DEVIATION

For example, there are three titration results as follows Titration 1 2 3 D=A+B+C Average of concentration, 3 Concentration A B C

D-A Deviation of titration 1 = D D-B Deviation of titration 2 = D D-C Deviation of titration 3 = D x 1000 x 1000 x 1000

TKA 2013/Analytical Chemistry/Practical 1

DATA SHEET COPY PRACTICAL ASSIGNMENT 1 DETERMINATION OF SOLUTION CONCENTRATION Date :__________________________________ Lab :__________________________________

STUDENTS

Name of Group Members 1) ________________________________________________ 2) ________________________________________________ 3) ________________________________________________

Matric No. _______________ _______________ _______________

STEPS A AND B Preparation and standardization of NaOH solution Titration Weight of acid (g) oxalate Volume of needed (mL) NaOH

TKA 2013/Analytical Chemistry/Practical 1

1 2 3

STEP C Determination of solution X concentration Titration 1 2 3 Weight of acid (g) oxalate Volume of needed (mL) NaOH

TKA 2013/Analytical Chemistry/Practical 1

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