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How do different temperatures of titration (10, 20, 30, 40, 50 degrees Celsius)

affect the pKa1 value of 0.001 molL-1 Thymolphthalein (3,3-bis(4-hydroxy-2-


methyl-5-propan-2-ylphenyl)-2-benzofuran-1-one) when titrated with 0.02 molL-1
Sodium Hydroxide (NaOH), calculated through the half-equivalence method?
Variables:
Independent variable
-Temperature (degrees Celsius) of the water in the water bath (where the conical flask is placed)

Dependent variable
-pH of solution inside the conical flask (solution of initial thymolphthalein, where sodium hydroxide is
added)

Control variables
-Concentration of thymolphthalein
-Concentration of sodium hydroxide
-Initial volume of thymolphthalein
-Total volume of sodium hydroxide added, and the amount added per unit time
-Total time of measurement for each trial
-pH 7 buffer solution (used to calibrate pH probe)
-Date of titration

Apparatus
Chemicals
-21.53g Thymolphthalein powder
-0.80g Sodium Hydroxide (NaOH) powder
-250mL Liquid Ethanol (95%)
-pH 7 Buffer solution

Glassware
-50mL Burette (+/- 0.05mL)
-25mL Pipette (+/- 0.1mL)
-500mL Volumetric flask (+/- 0.1mL)
-1000mL Volumetric flask (+/-)
-15x 250 mL Conical Flasks
-2x Beaker
-Stirring rod

Others
-2x Clamp stands
-Mass balance (+/- 0.01g)
-Water bath
-pH probe (+/-)
-Thermometer (+/- degrees C)
-Timer (+/- s)
-Distilled water
-Filter paper
-Goggles
-Lab coat

Calculations:
Concentration (molL-1)= moles(mol)/volume (L)
Moles (mol)= mass (g)/molar mass (gmol-1)

Thymolphthalein:

Mr of Thymolphthalein= 430.544
0.10 molL-1= (mass/430.54gmol-3)/0.5L
Mass= 21.53g

NaOH:

Mr of NaOH= 40.00
0.02molL-1= (mass/40.00gmol-3)/1.00L
Mass= 0.80g

Methodology
Part I: Preparation of solutions

a) Thymolphthalein Indicator (500mL of a 0.10 molL-1 solution)


1. Weigh with a mass balance, a total of 21.53g (+/- 0.01g) of thymolphthalein powder, on top of folded
filter paper, measuring 5.00g (+/- 0.01g) separately 4 times, then measure the remaining 1.53g(+/-
0.01g) to prevent spillage of large quantities of Thymolphthalein powder.
2. Put the measured Thymolphthalein powder in a beaker and add 250mL of ethanol into the beaker
using a 25mL (+/- 0.1mL) pipette (as thymolphthalein is slightly insoluble in water, hence equal volumes
of liquid ethanol and distilled water will be used as the solvent to dissolve the thymolphthalein).
3. Stir with a stirring rod until the powder gradually dissolves and the solution is clear.
4. Add this solution into a 500mL volumetric flask, and add 250mL distilled water through a funnel until
the bottom of the meniscus nears the marked line (check the level of the meniscus at eye level).
5. Add distilled water to the beaker, and use a pipette to carefully add distilled water drop by drop into
the volumetric flask until the bottom of the meniscus reaches the 500mL marked line, by checking the
level of the meniscus at eye level.
6. Put on the lid/bung of the volumetric flask to prevent evaporation of the solution.

b) Sodium Hydroxide solution (1000mL of a 0.02 molL-1 solution)


1. Weigh with a mass balance of 0.80g (+/- 0.01g) of Sodium Hydroxide powder.
2. Put the measured Sodium Hydroxide powder in a beaker and add 250mL distilled water in the beaker
as a solvent to dissolve the NaOH, measured using a 25mL (+/- 0.1mL) pipette.
3. Stir with a stirring rod until it gradually dissolves.
4. Add this solution in the beaker into the 1000mL (+/- mL) volumetric flask, pouring it through the
funnel.
5. Continue to pour distilled water through a funnel, into the volumetric flask, until the bottom of the
meniscus nears the marked line (check the level of the meniscus at eye level).
6. Add distilled water to the beaker, and use a pipette to carefully add distilled water drop by drop into
the volumetric flask until the bottom of the meniscus reaches the 500mL marked line, by checking the
level of the meniscus at eye level.
7. Put on the lid/bung of the volumetric flask to prevent evaporation of the solution.

Part II: Titration at different temperatures

1. Set the water bath by adding 500mL water and setting it to 10.0 degrees Celsius.
2. Set up another clamp stand beside the water bath to hold the thermometer placed inside the water
bath.
3. Use a 25mL (+/- 0.1mL) pipette to measure 25mL of Thymolphthalein indicator solution, and add it
into a conical flask.
4. Use a clamp stand to set up and hold a burette filled with 50mL (+/- 0.05mL) of 0.02molL -1 Sodium
hydroxide solution.
5. Use a pH 7 buffer solution to calibrate the pH meter with the Vernier logger pro display.
6. Use a pH probe to measure the initial pH of Thymolphthalein in the conical flask.
7. Modify settings on the Vernier Logger display to record the pH every 5.0 seconds.
8. Add 0.50mL of NaOH solution every 10.0 seconds
9. Repeat until the timer reads for 120.0 seconds.
10. Record the time, pH, and volume of the Sodium hydroxide solution added every 5.0 seconds.
11. Repeat steps 1-10 at the same temperature 3 times and calculate the average pH.
12. Repeat steps 1-11 four times in total for 20, 30, 40, and 50 degrees Celsius.

Pilot test methodology: Temp at 10, 30, 50 (3x3 results)

Apparatus
Chemicals
-10.76g Thymolphthalein powder
-0.40g Sodium Hydroxide (NaOH) powder
-125mL Liquid Ethanol (95%)
-pH 7 Buffer solution

Glassware
-50mL Burette (+/- 0.05mL)
-25mL Pipette (+/- 0.1mL)
-250mL Volumetric flask (+/- 0.1mL)
-500mL Volumetric flask (+/- 0.1mL)
-9x 250 mL Conical Flasks
-2x Beaker
-Stirring rod

Others
-2x Clamp stands
-Mass balance (+/- 0.01g)
-Water bath
-pH probe (+/-)
-Thermometer (+/- degrees C)
-Timer (+/- s)
-Distilled water
-Filter paper
-Goggles
-Lab coat

Part I: Preparation of solutions

a) Thymolphthalein Indicator (250mL of a 0.10 molL-1 solution)


1. Weigh with a mass balance, a total of 10.76g (+/- 0.01g) of thymolphthalein powder, on top of folded
filter paper, measuring 5.00g (+/- 0.01g) then measure the remaining 5.76g(+/- 0.01g) to prevent spillage
of large quantities of Thymolphthalein powder.
2. Put the measured Thymolphthalein powder in a beaker and add 125mL of ethanol into the beaker
using a 25mL (+/- 0.1mL) pipette (as thymolphthalein is slightly insoluble in water, hence equal volumes
of liquid ethanol and distilled water will be used as the solvent to dissolve the thymolphthalein).
3. Stir with a stirring rod until the powder gradually dissolves and the solution is clear.
4. Add this solution into a 250mL volumetric flask, and add 125mL distilled water through a funnel until
the bottom of the meniscus nears the marked line (check the level of the meniscus at eye level).
5. Add distilled water to the beaker, and use a pipette to carefully add distilled water drop by drop into
the volumetric flask until the bottom of the meniscus reaches the 250mL marked line, by checking the
level of the meniscus at eye level.
6. Put on the lid/bung of the volumetric flask to prevent evaporation of the solution.

b) Sodium Hydroxide solution (500mL of a 0.02 molL-1 solution)


1. Weigh with a mass balance of 0.40g (+/- 0.01g) of Sodium Hydroxide powder.
2. Put the measured Sodium Hydroxide powder in a beaker and add 125mL distilled water in the beaker
as a solvent to dissolve the NaOH, measured using a 25mL (+/- 0.1mL) pipette.
3. Stir with a stirring rod until it gradually dissolves.
4. Add this solution in the beaker into the 500mL (+/- mL) volumetric flask, pouring it through the funnel.
5. Continue to pour distilled water through a funnel, into the volumetric flask, until the bottom of the
meniscus nears the marked line (check the level of the meniscus at eye level).
6. Add distilled water to the beaker, and use a pipette to carefully add distilled water drop by drop into
the volumetric flask until the bottom of the meniscus reaches the 500mL marked line, by checking the
level of the meniscus at eye level.
7. Put on the lid/bung of the volumetric flask to prevent evaporation of the solution.

Part II: Titration at different temperatures

1. Set the water bath by adding 500mL water and setting it to 10.0 degrees Celsius.
2. Set up another clamp stand beside the water bath to hold the thermometer placed inside the water
bath.
3. Use a 25mL (+/- 0.1mL) pipette to measure 25mL of Thymolphthalein indicator solution, and add it
into a conical flask.
4. Use a clamp stand to set up and hold a burette filled with 50mL (+/- 0.05mL) of 0.02molL -1 Sodium
hydroxide solution.
5. Use a pH 7 buffer solution to calibrate the pH meter with the Vernier logger pro display.
6. Use a pH probe to measure the initial pH of Thymolphthalein in the conical flask.
7. Modify settings on the Vernier Logger display to record the pH every 5.0 seconds.
8. Add 0.50mL of NaOH solution every 10.0 seconds
9. Repeat until the timer reads for 120.0 seconds.
10. Record the time, pH, and volume of the Sodium hydroxide solution added every 5.0 seconds.
11. Repeat steps 1-10 at the same temperature 3 times and calculate the average pH.
12. Repeat steps 1-11 four times in total for 30, and 50 degrees Celsius.

Why does pKa decrease as temperature increases?

pKa decreases as temperature increases

According to Le Châtelier's Principle, if you add heat to an endothermic process, the position of
equilibrium moves to the right. Ka increases, and since pKa=−logKa , an increase in Ka means a decrease
in pKa.

Pilot test preparing solution of 0.1mol/L Thymolphthalein solution, hard to dissolve, turned quite
milky/cloudy, maybe should adjust to a lower concentration, though lower concentration affects…

Find out conditions that affect solubility


e.g. temperature

Prepare Thymolphthalein Indicator


First dissolve it in ethanol and then dilute it with water. Dissolve 0.04 g thymolphthalein in 50 mL of 95%
ethanol. Dilute this solution to 100 mL with distilled water.

100x2.5= 250mL
0.04x2.5= 0.1g powder
+125mL of ethanol

0.000058 mol/L
0.1/250x100= 0.04%
0.001M (mol/L) Thymolphthalein
Warm

As pH is the negative logarithm of the H+ (H3O+) concentration of a foreign substance, the lower the pH
value, the higher the concentration of H+ (H3O+) ions and the stronger the acid. Additionally, the higher
the pH value, the lower the H+ (H3O+) concentration and the stronger the base.
0.005

Green residue when measuring naoh

0.0005 molL-1 NaOH

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