Tafila Technical University

Department of Chemistry and Chemical Technology

Manual for Physical Chemistry Laboratory 1

(Chem. 345)

Prepared and revised by

Dr. Taher S. Ababneh

Version 1.2
Oct. 2017

Version History
Ver 1.0 June 2016
Ver 1.1 Jan 2017
 Contents

Title Page Week

Lab Check-in 2 1
Determination of the Heat Capacity of a Calorimeter 3 2
Heat of Neutralization 7 3
Heat of Solution from Solubility 11 4
Freezing Point Depression of Non-Electrolytes 14 5
Adsorption of Acetic Acid by Activated Carbon in Aqueous Medium 17 6-7
Distribution Coefficient of Acetic Acid in Butanol and Water 23 8
Determination of Critical Temperature of Phenol-Water System 27 9
Heating and Cooling Curve of Sodium Thiosulfate 30 10
Lab Check-out - 11

1
 ‫‪Week 1: Lab Check-in‬‬

‫الرقم الجامعي‪............................ :‬‬ ‫اسم الطالب ‪............................... :‬‬

‫‪ .1‬االلتزام بالحضور على موعد المختبر المحدد‬

‫‪ .2‬االلتزام بارتداء مريول المختبر من بداية المختبر و حتى نهايته‬
‫‪ .3‬عدم االكل و الشرب داخل المختبر‬
‫‪ .4‬عدم التدخين داخل المختبر‬
‫‪ .5‬االلتزام بجميع التحذيرات و التوجيهات التي تعطى من قبل المدرس و المشرف‬
‫‪ .6‬عدم العبث بأي ادوات او مواد كيميائية ال تخص التجربة المقررة‬
‫‪ .7‬المحافظة على نظافة المختبر خالل اجراء التجربة و ذلك يتضمن‪ :‬عدم القاء المخلفات مثل‪ -:‬اعواد الثقاب‪ ,‬ورق‬
‫الترشيح‪ ,‬ورق قياس درجة الحموضة‪ ,‬االنابيب الشعرية داخل االحوض او على ارض المختبر‬
‫‪ .8‬االلتزام بارتداء النظارة الواقية خالل عمل التجربة‬
‫‪ .9‬عدم الخروج من المختبر خالل عمل التجارب اال بإذن المدرس او المشرف المسؤول و ال يكون ذلك اال للضرورة‬
‫‪ .11‬عدم المزاح مع الزمالء خالل التواجد في المختبر‬
‫‪ .11‬التعامل مع المواد الكيميائية و االدوات حسب تعليمات و ارشادات المدرس و المشرف‬
‫عدم استخدام اي مادة كيميائية قبل قراءة التعليمات المكتوبة على العبوة‬ ‫‪‬‬
‫عدم استخدام نفس الملعقة او الماصة ألكثر من مادة كيميائية‬ ‫‪‬‬
‫عدم وضع الملعقة او الماصة مباشرة داخل العبوة‬ ‫‪‬‬
‫‪ .12‬عدم استخدام الهواتف داخل المختبر‬
‫‪ .13‬االلتزام بلبس حذاء غير كاشف للقدم‬
‫‪ .14‬عند حدوث اي مشكلة خالل سير التجربة يجب اللجوء الى المدرس او المشرف و عدم ابداء اي تصرف فردي‬
‫‪ .15‬عدم الخروج من المختبر بعد االنتهاء من عمل التجربة اال بعد تسليم االدوات نظيفة و موافقة المشرف‬

‫العقوبات‪:‬‬
‫كل من يخالف يعرض نفسة للعقوبات المنصوص عليها في نظام منح درجة البكالوريوس والمعمول به في جامعة‬
‫الطفيلة التقنية‪.‬‬

‫توقيع الطالب‬

‫‪2‬‬
 Week 2: Determination of the Heat Capacity of a Calorimeter

Objective: To determine the heat capacity (𝐶) of a coffee-cup calorimeter

Introduction: Calorimetry is the measurement of heat changes associated with chemical

reactions, physical changes or phase transitions under specific conditions. Such measurements
are performed in a device called a calorimeter, an apparatus for measuring the amount of heat
involved in a chemical reaction or other process. The heat associated with any chemical or
physical change can be calculated using this equation:

𝑞 = 𝑚. 𝑠. ∆𝑇

𝑞: Heat gained or lost (J)

𝑚: Mass of the solution (g)
𝑠: Specific heat capacity of solution (J/g.°C)
∆𝑇: Temperature change (°C) of the solution = (𝑇𝑓 – 𝑇𝑖 )

If a chemical reaction is carried out at constant pressure, heat (𝑞) lost or gain associated with the
reaction is called the enthalpy of reaction which is given the symbol ∆𝐻 (often expressed in units
of KJ/mol).

In these experiments, we have to account for the heat loss through the container (the
calorimeter). This amount of heat is given by this equation:

𝑞𝑐𝑎𝑙𝑖𝑟𝑖𝑚𝑒𝑡𝑒𝑟 = 𝐶. ∆𝑇

𝐶: Heat capacity of the calorimeter (J/°C)

To determine the heat capacity of the calorimeter (𝐶), we can use the first law of
thermodynamics (law of conservation of energy). A measured amount of cold water is placed in
a calorimeter to be calibrated and allowed to come to thermal equilibrium with the calorimeter,
and then a measured amount of hot water is added to the cold water in the calorimeter:

𝑞𝑙𝑜𝑠𝑡 𝑏𝑦 ℎ𝑜𝑡 𝑤𝑎𝑡𝑒𝑟 = −[𝑞𝑔𝑎𝑖𝑛𝑒𝑑 𝑏𝑦 𝑐𝑜𝑙𝑑 𝑤𝑎𝑡𝑒𝑟 + 𝑞𝑔𝑎𝑖𝑛𝑒𝑑 𝑏𝑦 𝑐𝑎𝑙𝑜𝑟𝑖𝑚𝑒𝑡𝑒𝑟 ]

The minus sign in this equation is necessary since the hot water is losing energy, thus making
𝑞ℎ𝑜𝑡 a negative quantity.

Or simply:
𝑞ℎ𝑜𝑡 = −[𝑞𝑐𝑜𝑙𝑑 + 𝑞𝑐𝑎𝑙𝑜𝑟𝑖𝑚𝑒𝑡𝑒𝑟 ]

𝑚ℎ𝑜𝑡 . 𝑠. ∆𝑇ℎ𝑜𝑡 = −[𝑚𝑐𝑜𝑙𝑑 . 𝑠. ∆𝑇𝑐𝑜𝑙𝑑 + 𝐶. ∆𝑇𝑐𝑜𝑙𝑑 ]

𝑚ℎ𝑜𝑡 : Mass of hot water in grams

𝑠: Specific heat capacity of water = 4.184 J/g.°C

3
∆𝑇ℎ𝑜𝑡 = 𝑇𝑓 – 𝑇𝑖ℎ
𝑚𝑐𝑜𝑙𝑑 : Mass of cold water in grams
∆𝑇𝑐𝑜𝑙𝑑 = 𝑇𝑓 – 𝑇𝑖𝑐
𝑇𝑖ℎ : The initial temperature of hot water, 𝑇𝑖𝑐 : The initial temperature of cold water

Solving for 𝐶 yields:

−𝑚ℎ𝑜𝑡 . 𝑠. ∆𝑇ℎ𝑜𝑡 − 𝑚𝑐𝑜𝑙𝑑 . 𝑠. ∆𝑇𝑐𝑜𝑙𝑑

𝐶=
∆𝑇𝑐𝑜𝑙𝑑

Procedure:

1. Using a graduated cylinder measure 50.0 ml of cold tap water, then transfer the water into the
calorimeter. Cap the calorimeter with its cover containing a thermometer and a stirring rod.

2. Fill a clean and dry 250 ml or 500 ml beaker with water and heat to about 50-70 ⁰C using a
Bunsen burner. Stir the water with a glass rod during the heating to insure that the temperature is
as uniform as possible.

3. While the water is heating, record the temperature of cold water 𝑇𝑖𝑐 in the calorimeter for
2-3 minutes to make certain that it has become constant.

4. When the water has reached approximately 50-70⁰C, remove the beaker from the heat and
measure 50.0 ml of hot water using a graduated cylinder. Allow the cylinder to stand on lab
bench for 2-3 minutes, stirring the water during this time period, record the temperature of hot
water 𝑇𝑖ℎ after this period.

5. Quickly remove the cover of calorimeter, and pour the hot water into cold water in the
calorimeter. Immediately replace the cover of calorimeter and stir the water with a stirring rod.
Record the water temperature as a function of time (every 10 seconds) on a table data sheet.
(Example table below)
time (s) temperature (ᶹC)
0 𝑇𝑖𝑐 =
10 ?
20 ?
30 ?

6. Plot temperature (y axis) vs. time (x axis) (example graph below). Determine the maximum
temperature reached after mixing (𝑇𝑓 ).

4
5
 Report Sheet
Week 2: Determination of the Heat Capacity of a Calorimeter

______________________________________:‫االسم‬

Data and Calculations:

Run 1 Run 2
𝑚𝑐𝑜𝑙𝑑 Mass of cold water (g)
𝑇𝑖𝑐 Initial temperature of cold water
𝑚ℎ𝑜𝑡 Mass of hot water (g)
𝑇𝑖ℎ Initial temperature of hot water
𝑇𝑓 Final temperature reached
∆𝑇𝑐𝑜𝑙𝑑 = 𝑇𝑓 – 𝑇𝑖𝑐
∆𝑇ℎ𝑜𝑡 = 𝑇𝑓 – 𝑇𝑖ℎ
𝐶: Heat capacity of the calorimeter J/°C (show your calculation below)
Average Heat capacity of the calorimeter 𝐶𝑎𝑣𝑔 from trial 1 and 2

Calculations:
Show your calculations for the heat capacity of the calorimeter (𝐶) from trial 1

Questions:
1. A glass of tea is being cooled from 90 °C to 30 °C. How much heat is lost if the volume of the
tea is 200 cm3. Assume the density of tea is 1g/ml and the specific heat capacity of tea is 4.184
J/g°C.

2. A 75-ml sample of hot water at 88 ˚C is added to 100-ml cold water placed in a calorimeter at
18 ˚C. The final temperature of the mixture is 38˚C. Calculate the heat capacity of the
calorimeter. (Assume the density of water is 1 g/ml)

6
 Week 3: Heat of Neutralization

Objective: To determine the heat of neutralization (∆𝐻𝑛 ) of strong acid by strong base.

Introduction: The heat of neutralization (or enthalpy of neutralization) of an acid is defined as

the amount of heat evolved when one equivalent of an acid and one equivalent of a base undergo
a neutralization reaction to form water and a salt. It is defined as the energy released with the
formation of 1 mole of water.
When a reaction is carried out under standard conditions at the temperature of 298 K (25 ˚C) and
1 atm of pressure and one mole of water is formed it is called the standard enthalpy of
neutralization (∆𝐻𝑛° °).

The heat (𝑞) released during a reaction is:

𝑞𝑟𝑒𝑙𝑒𝑎𝑠𝑒𝑑 𝑏𝑦 𝑟𝑥𝑛 = −[𝑞𝑔𝑎𝑖𝑛𝑒𝑑 𝑏𝑦 𝑠𝑢𝑟𝑟𝑜𝑢𝑛𝑑𝑖𝑛𝑔𝑠 ]

From this, the enthalpy change (∆𝐻𝑛 ) is calculated from the division by the number of moles of
water (in moles) produced:

𝑞𝑟𝑒𝑙𝑒𝑎𝑠𝑒𝑑 𝑏𝑦 𝑟𝑥𝑛
∆𝐻𝑛 =
𝑛

The standard enthalpy change of neutralization for a strong acid and base is -55.8 kJ/mol. For
example:
𝑁𝑎𝑂𝐻(aq) + 𝐻𝐶𝑙(aq) → 𝑁𝑎𝐶𝑙(aq) + 𝐻2 𝑂(l)

When we consider the above reaction it is clear that the net ionic equation is:
+ −
𝐻(𝑎𝑞) + 𝑂𝐻(𝑎𝑞) → 𝐻2 𝑂(l)

The enthalpy change of this reaction is -55.8 kJ/mol. The standard enthalpy of neutralization for
organic acids is slightly less exothermic than that of mineral acids because of the partial
ionization of weak organic acids. To break these bonds, some amount of energy is needed, which
reduces the enthalpy change.

In this experiment, a measured volume of 𝐻𝐶𝑙(aq) solution of known concentration is allowed to

react with a measured volume of 𝑁𝑎𝑂𝐻(aq) of known concentration in dilute solution. The
temperature change is then recorded. With the known amount of reactants, the heat of
neutralization can be calculated as follows:
𝑞𝑟𝑒𝑙𝑒𝑎𝑠𝑒𝑑 𝑏𝑦 𝑟𝑥𝑛 = −[𝑞𝑔𝑎𝑖𝑛𝑒𝑑 𝑏𝑦 𝑠𝑜𝑙𝑛𝑠 + 𝑞𝑔𝑎𝑖𝑛𝑒𝑑 𝑏𝑦 𝑐𝑎𝑙𝑜𝑟𝑖𝑚𝑒𝑡𝑒𝑟 ] = −[𝑚𝑠𝑜𝑙𝑛𝑠 . 𝑠. ∆𝑇 + 𝐶∆𝑇]

𝑞𝑟𝑒𝑙𝑒𝑎𝑠𝑒𝑑 𝑏𝑦 𝑟𝑥𝑛
∆𝐻𝑛 =
𝑛
Where
𝑚𝑠𝑜𝑙𝑛𝑠 : The total mass of acidic and basic solutions in g (assume density of solutions 1 g/ml)

7
𝑠: Specific heat capacity of water = 4.184 J/g.°C
∆𝑇: Temperature change (°C) of the reaction mixture = (𝑇𝑓 − 𝑇𝑖 )
𝐶: Heat capacity of the calorimeter (from experiment #1)
𝑛: Number of moles of water formed

Procedure:

1. Carefully measure 50 ml of 1 M 𝑁𝑎𝑂𝐻(aq) solution in a graduated cylinder and transfer into

the calorimeter.

2. Carefully measure 10 ml of 5 M 𝐻𝐶𝑙(aq) solution in a graduated cylinder.

3. Let the two solutions come to thermal equilibrium with the surroundings. The initial
temperature of both acidic and basic solutions should be the same. Record the temperature 𝑇𝑖 of
𝑁𝑎𝑂𝐻(aq) solution in the calorimeter for 2-3 minutes to make certain that it has become
constant.

4. Quickly pour the 10 ml of 5 M 𝐻𝐶𝑙(aq) solution into the 𝑁𝑎𝑂𝐻(aq) solution in the calorimeter.
Immediately replace the cover of calorimeter and stir the reaction mixture with a stirring rod.
Record the reaction temperature as a function of time (every 10 seconds) on a table data sheet
(example table below). Determine the highest temperature of the reaction mixture (𝑇𝑓 ).
time (s) temperature (ᶹC)
0 𝑇𝑖 =
10 ?
20 ?
30 ?

8
 Report Sheet
Week 3: Heat of Neutralization

______________________________________:‫االسم‬

Data and Calculations:

Run 1 Run 2
Volume of 𝐻𝐶𝑙(aq) solution (ml)
Mass of 𝐻𝐶𝑙(aq) solution* (g)
Volume of 𝑁𝑎𝑂𝐻(aq) solution (ml)
Mass of 𝑁𝑎𝑂𝐻(aq) solution* (g)
𝑚𝑠𝑜𝑙𝑛𝑠 : The total mass of acid and base solutions (g)
𝑇𝑖 ∶ Initial temperature of the 𝑁𝑎𝑂𝐻(aq) solution (°C)
𝑇𝑓 ∶ Highest temperature reached after mixing acid with base (°C)
∆𝑇: Temperature change (°C) of the reaction mixture = (𝑇𝑓 − 𝑇𝑖 )
𝐶𝑎𝑣𝑔 : Average Heat capacity of the calorimeter from exp.#1 (J/°C)
𝑞𝑟𝑒𝑙𝑒𝑎𝑠𝑒𝑑 𝑏𝑦 𝑟𝑥𝑛 (J) (show your calculation below)
Number of moles of 𝐻𝐶𝑙(aq) used
Number of moles of 𝑁𝑎𝑂𝐻(aq) used
Number of moles of water formed
∆𝐻𝑛 : Heat of neutralization (KJ/mol) (show your calculation below)
𝑎𝑣𝑔
∆𝐻𝑛 Average Heat of neutralization (KJ/mol) from the two trials
*
Assume the density of solutions = 1 g/ml

Calculation:
1. Show your calculations for 𝑞𝑟𝑒𝑙𝑒𝑎𝑠𝑒𝑑 𝑏𝑦 𝑟𝑥𝑛 in Joules and heat of neutralization (∆𝐻𝑛 ) in
KJ/mol for trial 1

𝑎𝑣𝑔
2. Calculate the % error in your average heat of neutralization ∆𝐻𝑛 compared to the accepted
or true value. Note: the “true” or accepted value is mentioned in the introduction section.

9
Questions:

1. A coffee cup calorimeter having a heat capacity of 451 J/˚C was used to measure the heat
evolved when 100 ml of 1 M 𝑁𝑎𝑂𝐻(aq) was added to 20 ml of 5 M 𝐻𝐶𝑙(aq) initially at 23.000
˚C. The temperature of the water rose to 28.855 ˚C. Calculate ∆𝐻𝑛 (in kJ/mol) for this reaction.
Assume the specific heat of the final solution is 4.184 J/g˚C and the density of each solution is
1.00 g/ml.

2. A solution is formed by combining 10 mL of solution A and 40 mL of solution B. Find out the

heat of reaction by assuming that no heat is lost to the calorimeter, if the initial and final
temperature of the system is 20.4 and 28.5 ˚C, respectively. Specific heat of a solution is 4.184
J/g˚C and density is 1.6 g/ml.

10
 Week 4: Heat of Solution from Solubility

Objective: To determine the heat of solution of an organic acid by measuring its solubility in
water at three temperatures and applying the Van’t Hoff equation to the data obtained.

Introduction: The dissolution of a solid into a liquid is usually accompanied with a heat transfer
(heat is either evolved or absorbed). Since the solubility of a substance is a special case of the
equilibrium constant, the Van’t Hoff relation is applicable. Thus, by obtaining the solubility at
different temperatures, and by applying the Van’t Hoff equation, it is possible to determine the
heat of solution (∆𝐻). When applied to solubility, the Van’t Hoff equation can be expressed as:

∆𝐻 1 ∆𝑆
ln 𝑠 = − ( )+
𝑅 𝑇 𝑅

In which 𝑠 is the solubility at different temperatures (𝑇 in Kelvin), ∆𝐻 is the average heat of

solution over the temperature range used, and 𝑅 is the universal gas constant and equals 8.314
J/mol.K. The solubility 𝑠 is expressed as grams of solute per 100 g of solvent. A plot of ln 𝑠 (y-
axis) versus 1/𝑇 (x-axis) gives a straight line with a slope of −∆𝐻/𝑅, then we can calculate ∆𝐻.
The heat of solution so calculated is approximately the average heat of solution over the
temperature range studied and it is the heat of solution at the saturation concentration.

In this experiment, the heat of solution of benzoic acid in water will be measured at 3 different
temperatures (RT, 35 and 50 °C).

Procedure:

1. Weight out a clean and dry 100-ml conical flask

2. Pipette out 10.00 ml of saturated benzoic acid aqueous solution into the pre-weighted conical
flask. If necessary stuff the tip of the pipette with a small piece of cotton so as to prevent solid
particles from entering into the pipette.

3. Weight out the conical flask with the benzoic acid solution.

4. Measure and record the temperature of the 10.00 ml benzoic acid solution at RT.

5. Using 2 drops of phenolphthalein indicator titrate with 0.1 M 𝑁𝑎𝑂𝐻 solution until the
endpoint is colorless to pale pink.

6. Record the volume of 𝑁𝑎𝑂𝐻 at the endpoint from the burette.

6. Repeat the procedure twice at the two higher temperatures (first at 35 °C then 50 °C). Step 4
above becomes: [4. Use a hot water bath to bring a 10.00 ml benzoic acid solution to the desired
temperature. Titrate immediately while hot].

11
 Report Sheet
Week 4: Heat of Solution from Solubility

______________________________________:‫االسم‬

Data and Calculations:

RT °C 35 °C 50 °C
Temperatures in Kelvin
1/𝑇 (K-1)
mass of the empty flask (g)
mass of flask plus 10-ml benzoic acid solution (g)
mass of 10-ml benzoic acid solution (g)
𝑉𝑖 : initial Burette reading (ml)
𝑉𝑓 : final Burette reading (ml)
𝑉𝑒𝑛𝑑𝑝𝑜𝑖𝑛𝑡 : volume of 𝑁𝑎𝑂𝐻 at endpoint (ml) = 𝑉𝑓 − 𝑉𝑖
𝑉𝑒𝑛𝑑𝑝𝑜𝑖𝑛𝑡 : volume of 𝑁𝑎𝑂𝐻 at endpoint (L)
number of moles of 𝑁𝑎𝑂𝐻 = 𝑀𝑁𝑎𝑂𝐻 𝑥 𝑉𝑒𝑛𝑑𝑝𝑜𝑖𝑛𝑡
mass of benzoic acid reacted (g)
mass of water (solvent) (g) = mass of 10-ml benzoic
acid solution (g) – mass of benzoic acid reacted (g)
solubility*, 𝑠 = [mass of benzoic acid reacted (g) /
mass of water (solvent) (g)] x 100
𝑙𝑛 𝑠
*
The solubility 𝑠 is expressed as grams of solute per 100 g of solvent

Calculations:
At the endpoint of titration:
Number of moles of 𝑁𝑎𝑂𝐻 = Number of moles of benzoic acid
𝑀𝑁𝑎𝑂𝐻 𝑥 𝑉𝑒𝑛𝑑𝑝𝑜𝑖𝑛𝑡 = Number of moles of benzoic acid
Where 𝑀𝑁𝑎𝑂𝐻 is the concentration of 𝑁𝑎𝑂𝐻 solution (0.1 M). Since

mass of benzoic acid

Number of moles of benzoic acid = molar mass of benzoic acid
Molar mass of benzoic acid C7H6O2 = 122.12 g/mol

Therefore, the mass of benzoic acid can be calculated as follows:

mass of benzoic acid

𝑀𝑁𝑎𝑂𝐻 𝑥 𝑉𝑒𝑛𝑑𝑝𝑜𝑖𝑛𝑡 = 122.12
Mass of benzoic acid = 0.1 𝑥 𝑉𝑒𝑛𝑑𝑝𝑜𝑖𝑛𝑡 𝑥 122.12

Note: 𝑉𝑒𝑛𝑑𝑝𝑜𝑖𝑛𝑡 (the volume of 𝑁𝑎𝑂𝐻 from the burette) should be in L

12
1. Plot 𝑙𝑛 𝑠 versus 1 / 𝑇 (K-1), and obtain ∆𝐻 ( J/ mol) from the slope. Attach the plot to your lab
report.

2. Comment on the nature of the graph.

Question
1. At a certain temperature, a student pipetted out 25 ml of benzoic acid solution sample and
titrated it with 0.1 M 𝑁𝑎𝑂𝐻 solution. It required 44 ml of 0.1 M 𝑁𝑎𝑂𝐻 solution to reach the
endpoint of titration. What is the solubility 𝑠 of benzoic acid expressed as grams of solute per
100 g of solvent? Assume the density of benzoic acid solution to be 1 g/ml.

13
 Week 5: Freezing Point Depression of Non-Electrolytes

Objective: To determine the freezing point depression in a solution when a solute is added to a
pure solvent. To use the freezing-point depression of the solution to determine the molar mass of
the solute.

Introduction: A solution freezes at a lower temperature than does the pure solvent. This
phenomenon is called freezing point depression. The freezing point depression of a solution is a
colligative property of the solution which is dependent upon the number of dissolved particles in
the solution. The higher the solute concentration, the greater the freezing point depression of the
solution. The freezing point plot of a pure solvent and a solution are shown below:

The freezing point of the pure solvent occurs at constant temperature but the freezing point of the
solution slowly decreases. The decrease caused by the increase in solute concentration as the
solvent freezes. The dissolved solutes can be non-electrolytes or electrolytes. Non-electrolytes
are molecules that remain intact when they dissolve in water. Electrolytes are solutes that
dissociate into ions when dissolved in solution to give an electrically conducting solution. The
equation describing the change in freezing point from pure solvent to solution is:
∆𝑇𝑓 = 𝐾𝑓 . 𝑚
𝐾𝑓 : The molal freezing point depression constant of the solvent (1.86 °C/m for water).
𝑚 : Molality = 𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒⁄𝑘𝑖𝑙𝑜𝑔𝑟𝑎𝑚𝑠 𝑜𝑓 𝑠𝑜𝑙𝑣𝑒𝑛𝑡
∆𝑇𝑓 : The freezing point depression = 𝑇𝑠𝑜𝑙𝑣𝑒𝑛𝑡 − 𝑇𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛 (°C)

In this experiment, the freezing point of pure water 𝑇𝑠𝑜𝑙𝑣𝑒𝑛𝑡 and of methanol aqueous solution
𝑇𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛 will be measured. The molality 𝑚 of the solution will be calculated. This will enable us
to calculate the molar mass of methanol.

Procedure:

1. Using a pipette, place 10.00 mL of distilled water in an 8-inch test tube. Insert the stirring
apparatus as shown in the Figure below. Make sure that the thermometer bulb is immersed in the
liquid.
2. Place the entire apparatus in a salt-ice cooling bath. Allow the water to cool down with
continuous stirring while recording the temperature every 10 seconds on a table data sheet.
(Example table below)
14
 time (s) temperature (ᶹC)
0 ?
10 ?
20 ?
30 ?
Record the temperature long enough to be sure that the value becomes indeed constant. This is
the freezing point of pure water 𝑇𝑠𝑜𝑙𝑣𝑒𝑛𝑡 .

3. Remove the test tube from the cooling bath and let the solid ice melt back into liquid water.
Afterwards, add 1.00 g of methanol CH3OH and mix it well with the liquid water sample

4. In a similar manner, repeat step 2 to find the freezing point of the methanol solution 𝑇𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛 .

Figure 1 – Freezing point apparatus in ice-salt water bath.

15
 Report Sheet
Week 5: Freezing Point Depression of Non-Electrolytes

______________________________________:‫االسم‬

Data and Calculations:

Volume of Water (ml)
Mass of Methanol (g)
Freezing Point (˚C)
Freezing point depression ∆𝑇𝑓
Calculate the molality 𝑚
(𝐾𝑓 = 1.86 °C/m for water)
Calculate number of moles
Calculate the molar mass of methanol
Pure Water Methanol in Water
10.00 10.00
1.00
𝑇𝑠𝑜𝑙𝑣𝑒𝑛𝑡 = 𝑇𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛 =
∆𝑇𝑓 = 𝑇𝑠𝑜𝑙𝑣𝑒𝑛𝑡 − 𝑇𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛 =
∆𝑇𝑓 = 𝐾𝑓 . 𝑚  𝑚 = ∆𝑇𝑓 /𝐾𝑓 =
𝑚 = moles methanol/ Kg solvent
 moles methanol = 𝑚 x Kg solvent =
moles methanol = mass methanol / molar mass methanol
 molar mass methanol = mass methanol / moles methanol
 molar mass methanol = 1.00 g / moles methanol

%error (actual molar mass of methanol = %error =[ |actual – experimental| / actual ] x 100%
32.04 g/mol)
Question:
1. What is the freezing point of a solution prepared by dissolving 20 g of ethanol (Molar mass =
46 g/mol) in 120 mL of water? The freezing point depression constant 𝐾𝑓 for water is 1.86 C/m.
Assume density of water is 1 g/ml.

16
Week 6 & 7: Adsorption of Acetic Acid by Activated Carbon in Aqueous Medium

Objective: To determine the equilibrium distribution of an organic acid (acetic acid) between an
aqueous solution and the surface of activated carbon as a function of the solute concentration at
constant temperature.

Introduction: Adsorption is a surface phenomenon in which materials from a bulk gas or liquid
are attached to a surface and held by physical or chemical forces. Adsorption can occur at solid
or liquid surfaces, and it may involve one layer or many layers of adsorbed molecules depending
upon the surface and the types of forces involved. The extent of adsorption depends not only
upon the type of surface but also upon the surface area itself so that, for any given material, the
greater the surface area the greater the adsorption. Since liquids have smooth surfaces, their
adsorptive capacities are limited relative to that of a solid which can be subdivided and which
may have cracks and crevices which are available for adsorption. The best adsorbents are those
that exist in a high state of subdivision, and such substances have specific areas of 1000 square
meters per gram or layer. Among the most useful solid adsorbents are silica gel (SiO2) and
activated carbon. They can be subdivided to a high degree so that large areas are exposed for
adsorption.

Many solids have the property of adsorbing large quantities of gases and solutes from liquid
solutions. Often, this action is specific both with respect to the adsorbent and the material
adsorbed (adsorbate). In general, if adsorption is specific and if large amounts of heat are
librated (more than about 40 KJ per mol adsorbed) the process is called chemisorptions. If the
adsorption is non-specific and if only small amounts of heat are librated, comparable to the heat
of vaporization of the adsorbed material, the process is physical adsorption (physisorption).
Other adsorption characteristics such as temperature, bulk concentration dependence and
reversibility are often used to distinguish chemical and physical adsorption.

The adsorption capacity of solid surfaces is determined from measurements of the mass (or
moles) of material adsorbed and the area available for adsorption per unit mass of adsorbent.
Usually, the amount of solute adsorbed from solution per unit mass of adsorbent depends upon
the solute bulk concentration up to its saturation point. Also, the amount adsorbed per unit mass
of adsorbent for a given solute bulk concentration decreases with increasing temperature. If the
adsorption is physical, it is reversible and the solute will leave the surface of the adsorbent to
reestablish equilibrium when the adsorbent is removed from a solution in equilibrium and placed
into a solution of lower solute concentration. Such reversibility may not be shown if the process
is chemisorptions.

Adsorption Isotherms

Different equations (models) have been proposed to investigate the mechanism of adsorption and
describe adsorption behavior over a limited range of measurements at constant temperature
(isotherm). The adsorption isotherm indicates how the adsorption molecules distribute between
the liquid phase and the solid phase when the adsorption process reaches an equilibrium state.
The analysis of the isotherm data by fitting them to different isotherm models is an important
step to find the suitable model that can be used for design purposes. Adsorption isotherm is

17
basically important to describe how solutes interact with adsorbents, and is critical in optimizing
the use of adsorbents.

In this experiment, adsorption isotherm study will be carried out on two isotherm models: the
Langmuir and Freundlich isotherm models. The applicability of the isotherm models to the
adsorption study will be compared by judging the correlation coefficients, R2 values.

Langmuir isotherm assumes monolayer adsorption onto a surface containing a finite number of
adsorption sites of uniform strategies of adsorption with no transmigration of adsorbate in the
plane of surface. Langmuir isotherm is called the ideal localized monolayer model; it was
developed to represent chemisorption. Langmuir isotherm is based on the following assumptions.
These are, adsorption is limited to monolayer coverage, such that; the adsorbed molecule cannot
migrate across the surface or interact with neighboring molecules. Also, the surface of the
adsorbent is uniform. This means that all the adsorption sites are equivalent in energy.

The linear form of Langmuir isotherm equation is given as:

𝐶𝑒 1 1
= 𝑏𝑄 + 𝑄 𝐶𝑒 ……………. Eq. 1
𝑞𝑒 𝑜 𝑜
Where:
𝐶𝑒 is the equilibrium concentration of the adsorbate (mg/L);
𝑞𝑒 is the amount of adsorbate adsorbed per unit mass of adsorbent at equilibrium (mg/g);
𝑏 is the Langmuir affinity constant (L/mg);
𝑄𝑜 is the adsorption capacity at equilibrium corresponding to monolayer coverage (mg/g);

The amount of acetic acid adsorbed per unit mass of charcoal adsorbent, 𝑞𝑒 (mg/g) is calculated
by the following equation:
(𝐶 − 𝐶𝑒 )𝑉⁄
𝑞𝑒 = 𝑜 𝑚 …………….Eq. 2

Where 𝐶𝑜 and 𝐶𝑒 are the initial and equilibrium acetic acid concentration in solution,
respectively (mg/L). 𝑉 is the volume of solution (L) and 𝑚 is the mass of charcoal adsorbent
used (g)

A plot of 𝐶𝑒 /𝑞𝑒 (y-axis) against 𝐶𝑒 (x-axis) gives a straight line with a slope of 1/𝑄𝑜 for
experimental data that are best described by Langmuir isotherm model. The closer the R2 value
to 1.000 the more indication there is that the adsorption data of the adsorbate (acetic acid) onto
the activated carbon at room temperature is best fitted to the Langmuir isotherm model. The
Langmuir constants 𝑏 and 𝑄𝑜 can be obtained from the slope and intercept of the straight line
using Eq. 1

The Freundlich isotherm model is used for heterogeneous surface energy systems and for
description of multilayer adsorption with interaction between adsorbed molecules.

The linear form of Freundlich isotherm equation is given as:

1
log 𝑞𝑒 = log 𝐾𝐹 + 𝑛 log 𝐶𝑒 …………….Eq. 3

18
Where
𝑞𝑒 is the amount of adsorbate adsorbed per unit mass of adsorbent at equilibrium (mg/g);
𝐶𝑒 is the equilibrium concentration of the adsorbate (mg/L);
𝐾𝐹 and 𝑛 are Freundlich constants with 𝐾𝐹 being the adsorption coefficient related to adsorption
capacity while 𝑛 is related to adsorption intensity.

Experimental data that are best fitted by Freundlich isotherm model, gives a straight line with
slope of 1/𝑛 and intercept of log 𝐾𝐹 when the plot of log 𝑞𝑒 (y-axis) versus log 𝐶𝑒 (x-axis) is
constructed.

Procedure:
Week 6 (Period 1)

1. Weight about 1.5 g charcoal into each of six dry 250-ml Erlenmeyer flasks. Record the weight
to ±1 mg. Place a stopper on each Erlenmeyer flask.

2. Using a 100-ml volumetric flask, prepare a series of acetic acid solutions of various
concentrations according to the Table below. Solution #1 will not be diluted. Solutions #2-6 will
be diluted with distilled water in the 100-ml volumetric flask.

Solution # Volume of 0.4 M acetic acid Volume of distilled water

1 100 ml 0 ml
2 75 ml 25 ml
3 50 ml 50 ml
4 25 ml 75 ml
5 10 ml 90 ml
6 5 ml 95 ml

3. Add 100 ml of each solution to each charcoal sample. Place a stopper firmly on each
Erlenmeyer flask

3. Swirl the flasks vigorously for 30 minutes and let them stand overnight.

19
 Week 7 (Period 2)

4. Filter the solutions and pipette a suitable size filtrate sample for titration (refer to the Table
below)

Solution # Volume of filtrate sample for titration

1 10 ml
2 10 ml
3 10 ml
4 25 ml
5 25 ml
6 50 ml

5. Titrate each filtrate sample with standard 0.1 M sodium hydroxide. Use phenolphthalein
indicator. Record the volume of 𝑁𝑎𝑂𝐻 used to reach the endpoint (EP) of titration.

20
 Report Sheet
Week 6 & 7: Adsorption of Acetic Acid by Activated Carbon in Aqueous Medium

______________________________________:‫االسم‬

Data and Calculations:

Record the volume of 𝑁𝑎𝑂𝐻 from the burette at the endpoint of titration for each filtrate sample
and complete the data Table below:

𝑀2 𝐶𝑜 Ce qe
Soln Vol Initial Initial Vol Vol Equ Equ acid
# (ml) acid conc. acid conc. filtrate 𝑁𝑎𝑂𝐻 acid conc acid conc adsorbed / 𝐶𝑒 log 𝑞𝑒 log 𝐶𝑒
(mol/L) (mg/L) (ml) EP (ml) (mol/L) (mg/L) g carbon 𝑞𝑒
(mg/g)
1 100 0.4 24000c 10 d f g

2 100 0.3a 18000 10

3 100 0.2b 10
e
4 100 25
5 100 25
6 100 50

a b
(M1)(V1) = (𝑀2 ) (V2)
(0.4)(75) = (𝑀2 ) (100)
c
(M1)(V1) = (𝑀2 ) (V2) 𝐶𝑜 (mg/L) = 𝑀2 x (molar mass acetic acid) x 1000
= 0.4 mol/L x (60 g/mol) x 1000 = 24000
(0.4)(50) = (𝑀2 ) (100)

d
Mol of acid in filtrate sample = mol 𝑁aOH at endpoint
= [NaOH] x VEP (L) ……. Note: [NaOH] = 0.1 M
Equ acid conc in filtrate sample (mol/L) = Mol of acid in filtrate sample/volume of filtrate (L)
= Mol of acid in filtrate sample/0.01 L

e
Mol of acid in filtrate sample = mol 𝑁aOH at endpoint
= [NaOH] x VEP (L) ……. Note: [NaOH] = 0.1 M
Equ acid conc in filtrate sample (mol/L) = Mol of acid in filtrate sample/volume of filtrate (L)
= Mol of acid in filtrate sample/0.025 L

f
𝐶𝑒 (mg/L) = Equ acid conc in filtrate sample (mol/L) x (molar mass of acetic acid) x 1000

21
g
(𝐶𝑜 − 𝐶𝑒 )𝑉⁄
𝑞𝑒 = 𝑚

Where 𝑉 is the volume of solution (L) and 𝑚 is the mass of charcoal adsorbent used (g)
𝑉 in our experiment is 100 ml = 0.1 L
𝑚 = mass of charcoal = 1.5 g

Show all your calculations for solution # 5

Initial acid conc.(mol/L)

𝐶𝑜

Equilibrium acid conc. (mol/L)

𝐶𝑒

𝑞𝑒

𝐶𝑒
𝑞𝑒

log 𝑞𝑒

log 𝐶𝑒
𝐶
For Langmuir isotherm model fitting: A plot of 𝑞𝑒 (y-axis) vs 𝐶𝑒 (x-axis) gives a straight line
𝑒
with a slope of 1⁄𝑄𝑜 and intercept of 1⁄𝑏𝑄𝑜 . What is the value of R2? Is it close to 1.00?
(Attach this graph to your lab report)

For Freundlich isotherm model fitting: A plot log 𝑞𝑒 (y-axis) vs log 𝐶𝑒 (x-axis) gives a straight
line with a slope of 1⁄𝑛 and intercept of log 𝐾𝐹 . What is the value of R2? Is it close to 1.00?
(Attach this graph to your lab report)

Calculate Langmuir and Freundlich parameters and report your results in the Table below:
Langmuir Model Freundlich Model
𝑄𝑜 𝑏 R2 𝑛 𝐾𝐹 R2

Which isotherm model best describes your equilibrium data? Discuss your results.

22
 Week 8: Distribution Coefficient of Acetic Acid in Butanol and Water
Objective: To determine the distribution coefficient of acetic acid between water and butanol.

Introduction: A substance soluble in a mixture of two immiscible liquids usually distributes

itself in such a way that, at a fixed temperature, the ratio of its concentration in the two liquid
layers is always constant and independent of concentration. The ratio 𝐾𝐷 is known as the
distribution coefficient of the substance between the two particular liquids.
This ratio is therefore a measure of the difference in solubility of the compound in these two
phases. Both phases usually are solvents. Most commonly, one of the solvents is water while the
second is hydrophobic such as 1-octanol. Hence the distribution coefficient measures how
hydrophilic ("water-loving") or hydrophobic ("water-fearing") a chemical substance is, and may
be expressed as:
[𝑠𝑜𝑙𝑢𝑡𝑒]𝑜𝑟𝑔
𝐾𝐷 = …………….Eq. 1
[𝑠𝑜𝑙𝑢𝑡𝑒]𝑎𝑞

Where 𝐾𝐷 is the distribution coefficient (the process equilibrium constant), [𝑠𝑜𝑙𝑢𝑡𝑒] represents
the concentration of solute being tested, and "𝑜𝑟𝑔" and "𝑎𝑞" refer to the organic and aqueous
phases, respectively. In this experiment, we will determine the distribution coefficient of acetic
acid in butanol (organic phase) and water. Thus the above equation can be written as:

[𝑎𝑐𝑒𝑡𝑖𝑐 𝑎𝑐𝑖𝑑]𝑜𝑟𝑔
𝐾𝐷 = …………….Eq. 2
[𝑎𝑐𝑒𝑡𝑖𝑐 𝑎𝑐𝑖𝑑]𝑎𝑞
Procedure:

1. Using a graduated cylinder, measure 40 ml of 2.0 M acetic acid and 40 ml of butanol. Transfer
the two liquids into a separatory funnel. Place a stopper firmly on the funnel.

2. Shake for 10 minutes to establish equilibrium at room temperature.

23
3. Allow the separatory funnel to stand for the phases to separate. (upper: butanol organic phase
and lower: aqueous phase). (Note: density of butanol is 0.81 g/ml).

4. Into a clean 150 mL Erlenmeyer flask, transfer 5 ml of the aqueous phase and mix with 5 ml
of distilled water. Titrate with 0.20 M 𝑁𝑎𝑂𝐻 using phenolphthalein as indicator (record the
volume of 𝑁𝑎𝑂𝐻 from the burette at the endpoint of titration 𝑉𝑎𝑞 ).

5. Into another clean Erlenmeyer flask (or beaker), take 5 ml from the organic phase and mix
with 5 ml of distilled water.

6. Titrate with 0.20 M 𝑁𝑎𝑂𝐻 using phenolphthalein as indicator (record the volume of 𝑁𝑎𝑂𝐻
from the burette at the endpoint of titration 𝑉𝑜𝑟𝑔 ).

7. Repeat step 4 and 5 (for a second trial).

24
 Report Sheet
Week 8: Distribution Coefficient of Acetic Acid in Butanol and Water

______________________________________:‫االسم‬

Data and Calculations:

Report your titration results in the Table below

Volume of NaOH at Trial 1 Trial 2 Average

EP (ml) Distribution
𝑉𝑎𝑞 ………ml ………ml Coefficient
𝑉𝑜𝑟𝑔 ………ml ………ml 𝐾𝐷
𝐾𝐷 ……… ……… ………

To calculate the distribution coefficient 𝐾𝐷 we will use Equation 2:

[𝑎𝑐𝑒𝑡𝑖𝑐 𝑎𝑐𝑖𝑑]𝑜𝑟𝑔
𝐾𝐷 = …………….Eq. 2
[𝑎𝑐𝑒𝑡𝑖𝑐 𝑎𝑐𝑖𝑑]𝑎𝑞

To determine [𝑎𝑐𝑒𝑡𝑖𝑐 𝑎𝑐𝑖𝑑]𝑜𝑟𝑔 : At the endpoint of titration, number of moles of 𝑁𝑎𝑂𝐻 equals
the number of acetic acid in butanol, therefore:
Moles of 𝑁𝑎𝑂𝐻 = Moles of acetic acid
[𝑁𝑎𝑂𝐻] 𝑉𝑜𝑟𝑔 = [𝑎𝑐𝑒𝑡𝑖𝑐 𝑎𝑐𝑖𝑑]𝑜𝑟𝑔 𝑉𝑎𝑐𝑖𝑑
0.20 M . 𝑉𝑜𝑟𝑔 = [𝑎𝑐𝑒𝑡𝑖𝑐 𝑎𝑐𝑖𝑑]𝑜𝑟𝑔 5 ml
 [𝑎𝑐𝑒𝑡𝑖𝑐 𝑎𝑐𝑖𝑑]𝑜𝑟𝑔 = (0.20 M . 𝑉𝑜𝑟𝑔 ) / 5 ml …………….Eq. 3

To determine [𝑎𝑐𝑒𝑡𝑖𝑐 𝑎𝑐𝑖𝑑]𝑎𝑞 : At the endpoint of titration, number of moles of 𝑁𝑎𝑂𝐻 equals
the number of acetic acid in aqueous layer, therefore:
Moles of 𝑁𝑎𝑂𝐻 = Moles of acetic acid
[𝑁𝑎𝑂𝐻] 𝑉𝑎𝑞 = [𝑎𝑐𝑒𝑡𝑖𝑐 𝑎𝑐𝑖𝑑]𝑎𝑞 𝑉𝑎𝑐𝑖𝑑
0.20 M . 𝑉𝑎𝑞 = [𝑎𝑐𝑒𝑡𝑖𝑐 𝑎𝑐𝑖𝑑]𝑎𝑞 5 ml
 [𝑎𝑐𝑒𝑡𝑖𝑐 𝑎𝑐𝑖𝑑]𝑎𝑞 = (0.20 M . 𝑉𝑎𝑞 ) / 5 ml …………….Eq. 4
By substituting Equations 3 and 4 into Equation 2, we get:

[𝑎𝑐𝑒𝑡𝑖𝑐 𝑎𝑐𝑖𝑑]𝑜𝑟𝑔
𝐾𝐷 = …………….Eq. 2
[𝑎𝑐𝑒𝑡𝑖𝑐 𝑎𝑐𝑖𝑑]𝑎𝑞
↓
(0.20 𝑀 𝑥 𝑉𝑜𝑟𝑔) / 5 𝑚𝑙
𝐾𝐷 =
(0.20 𝑀 𝑥 𝑉𝑎𝑞) / 5 𝑚𝑙
By cancelling out similar items we get:
25
 𝑉𝑜𝑟𝑔
𝐾𝐷 = …………….Eq. 5
𝑉𝑎𝑞

Use this equation to calculate 𝐾𝐷 for trial 1 and 2 and average 𝐾𝐷 value and report your results in
the Table above.

Questions:

1. Do your results give you an indication of how hydrophilic ("water-loving") or hydrophobic

("water-fearing") acetic acid is? Explain.

2. Compound 𝑍 has a solubility of 5.0 g/100 mL in water and 25.0 g/100 mL in ether.

a) Calculate the distribution coefficient 𝐾𝐷 of 𝑍 between water and ether.

b) A solution of 3.0 g of 𝑍 in 100 mL of water is being mixed with 100 ml of ether, what weight
of compound 𝑍 would be removed from water (transferred to the ether layer)? (Answer 2.5 g).
Show your work.

26
 Week 9: Determination of Critical Temperature of Phenol-Water System
Objective: In this experiment, you will draw the phase diagram of the two-component system of
phenol and water and determine the critical solution temperature (CST).

Introduction: When two liquids are mixed together, one of the following cases may arise:
a) The two liquids are completely miscible at all proportions yielding one homogeneous liquid
phase, for example alcohol and water.
b) The two liquids are partially miscible yielding either one or two liquid phases depending on
the conditions, for example phenol and water.
c) The two liquid are practically immiscible yielding always two distinct phases under ordinary
condition, for example carbon disulphide and water.

The mutual solubility of partially miscible liquids usually increases with temperature. In this
case, the solubility curve exhibits a maximum at the critical solution temperature above which
the two liquids become completely miscible at all proportions. For some liquid pairs such as
ether and water, however, the mutual solubility decrease with temperature, and the solubility
curve shows a minimum at the critical solution temperature below which the two liquids become
completely miscible at all proportions. The temperature-composition diagram of the phenol-
water system is shown in Figure 1. Outside the area bounded by the curve ABC there occurs one
unsaturated homogeneous liquid phase. Within that area, two liquid phases in equilibrium with
each other coexist; one is water saturated with phenol and the other phenol saturated with water.
Any point on the curve represents one saturated homogeneous phase.

Figure 1. Phase diagram of the phenol-water system

27
Procedure:

1. In a clean dry test tube weigh about 8 g phenol. Record the weight.

2. Add the calculated volume of water so as to obtain a mixture of 80% phenol and 20% water
by weight.

3. Cover the tube with a cork stopper carrying a thermometer and a stirrer, and then place in a
beaker containing hot water to serve as a bath.

4. Heat gradually while the mixture is constantly being stirred and record the temperature when
the two layers disappear forming one homogeneous layer.

5. Remove the tube from the hot water and let it cool down gradually. The temperature at which
the liquid becomes turbid and two liquid layers are separated should be recorded. These two
temperatures should be nearly the same, and their average gives the miscibility temperature of
the mixture used.

6. To the same mixture add the necessary calculated volume of water so as to obtain a mixture of
70% phenol. Determine the miscibility temperature of the new mixture as described above.

7. Repeat, using mixtures containing 60, 50, 40, 30 and 20% phenol.

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 Report Sheet
Week 9: Determination of Critical Temperature of Phenol-Water System

______________________________________:‫االسم‬

Data and Calculation:

To obtain 80% of phenol (20% water):

8𝑔
0.80 = 𝑥  x = 10 g solution  weight of water = 10 g – 8 g phenol = 2 g water
(Density of water = 1 g/ml  2 g water = 2 ml water)

To obtain 70% of phenol (30% water):

8𝑔
0.70 = 𝑥  x = 11.4 g solution weight of water to be added = 11.4 g – 10 g = 1.4 g water (=
1.4 ml)

To obtain 60% of phenol (40% water):

8𝑔
0.60 = 𝑥  x = 13.3 g solution  weight of water to be added = 13.3-11.4 = 1.9 g water (=1.9
ml)
And so on… (Complete the Table below showing all the calculations)

% of phenol Vol. H2O Temperature at complete miscibility

(ml) T (heating) T (cooling) T (average)
80% 2
70% 1.4
60% 1.9
50%
40%
30%
20%

Questions:
1) a) Construct a phase diagram of the phenol-water system. Plot the graph of phenol %
composition (x-axis) against the average temperature at complete miscibility. Determine the
critical solution temperature (CST).

b) If the accepted value of CST for phenol-water system is 67 °C. Calculate your percent error.
Discus some errors that might occur during conducting the experiment.

29
 Week 10: Heating and Cooling Curve of Sodium Thiosulfate
Objective: To graph the data for both the melting and freezing of a pure substance and to
determine the melting point (m.p.) and freezing point (f.p.) of the substance.

Introduction: In this lab a sample of a pure, solid substance is slowly heated in a warm water
bath until the sample fully melts. The temperature of the sample is measured every 30 sec during
this process and the data is recorded. Next, the liquefied sample is allowed to cool down
gradually in a cool water bath until the sample solidifies (freezes). Again the temperature of the
sample is measured every 30 sec and the data is recorded. Data for the two phase changes is
plotted on a single graph and the graph is used to determine the melting point and freezing points
of the substance.

Safety Notes:

Do not inhale sodium thiosulfate particles; they may cause irritation to the respiratory tract
causing coughing and shortness of breath. Avoid contact of the sodium thiosulfate with the skin.
Irritation may occur from prolonged skin contact. Wear goggles during the entire experiment.
Let glassware cool for several minutes before cleaning to avoid damaging the equipment.
Remember to immediately report accidents to your teacher.

Procedures:

1. Fill a 400-mL beaker with approximately 150 ml water (exact volumes are not necessary).

2. Measure approximately 3 g of sodium thiosulfate and transfer to a test tube.

3. Place the test tube in the beaker of water.

4. Place a thermometer in the test tube and record the initial temperature in the data table (at
time: 0 min).

5. Gently heat the water bath and record the temperature every 30 seconds.

6. Do not heat above 50ᵒC. The sample will decompose resulting in a material that
is very difficult to recrystallize. Once the sodium thiosulfate has melted (mp 48ᵒC),
turn off the heat source, remove the test tube from the water bath and continue to record the
temperature every 30 seconds as the sodium thiosulfate cools. Monitor the temperature of the
sample until about 5 minutes after the sample resolidifies.

30
 Report Sheet
Week 10: Heating and Cooling Curve of Sodium Thiosulfate

______________________________________:‫االسم‬

Data and Calculation:

Record the temperatures at 30-sec time intervals in the data Table below:

Heating Cooling
Time in minutes (x-axis) Temp, ᵒC (y-axis) Temp, ᵒC (y-axis)
0
0.5
1
1.5
2
2.5
3
3.5
4
4.5
5
5.5
6
6.5
7
7.5
8
8.5
9
9.5
10

1) Plot the temperature (y-axis) vs time (x-axis). The heating and cooling curves should be
plotted on the same graph.
2) Use the graph to determine the melting point and freezing point of sodium thiosulfate
3) Calculate the percent error. (Actual value for mp of sodium thiosulfate is 48.3 °C).
4) Explain why the temperature stays constant during melting and freezing.

31