PRACTICAL LAB

REPORT
Module title: Chemistry for engineers
Module code: CHE 1103(1)
Submitted by: Date of submission: 27/08/2018

Participants

Student name Student ID

 Table of contents

Titles Page

Experiment 1 3
1.0 Introduction 3
1.1 Aims and Objectives 3
1.2 Methodology 4
1.2.1 Apparatus 4
1.2.2 Chemicals used 7
1.2.3 Procedure 7
1.3 Observation 8
1.4 Result and Calculation 9
1.5 Conclusion 10
Experiment 2 11
2.0 Introduction 11
2.1 Aims and Objectives 11
2.2 Methodology 12
2.2.1 Apparatus 12
2.2.2 Chemical used 17
2.2.3 Procedure 17
2.3 Observation 18
2.4 Calculation 20
2.5 Concentration of thiosulfate 21
2.6 Conclusion 21
2.7 Safety 22
2.8 Precaution 22
2.9 References 23

Experiment 1: Acid base titration and quantitative analytical method

1.0 INTRODUCTION
The aim of carrying out an acid base titration is to determine the concentration of the basic
solution by titrating it with an acidic solution of known concentration, or vice-versa, until
neutralisation occurs. This experiment will involve the neutralisation of a strong acid which will
be HCl(aq) with NaOH(aq) which is a strong base. The solution with a known concentration is
called the titrant (HCl(aq) in this case) and the solution whose concentration is yet to be found is
called the analyte (in this case NaOH(aq)). The NaOH(aq) will then be allowed to run out of the
burette and will start neutralising the HCl(aq) in the conical flask. The pH of the solution in the
conical flask will gradually rise and its colour will not have a permanent pink colour until the
solution reaches a pH of 7.

1.1 AIM AND OBJECTIVE

● Understanding the concept of acid-base reaction and quantitative analytical method
● Determining the molarity of hydrochloric acid used.

1.2 METHODOLOGY
1.2.3 APPARATUS
The following apparatus are required for the experiment:
1. A 50cm3 Burette
A graduated glass tube that allow the measurement of a known volume of
solution.

Fig 1.0 50cm3 Burette

2. A 25cm3 Pipette
A narrow glass tube used to precisely measure 25cm3 of solution.

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Fig 1.1 25 cm3 Pipette

3. A Pipette Filler
A more safe way of filling a pipette instead of using the mouth. It draws
the liquid into the pipette, and accurately regulate or release the liquid.
 Fig 1.2 Pipette Filler

4. Conical Flask
An apparatus used to carry transferred solution or to carry experiment.

Fig 1.3 Conical flask

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5. Beakers
Cylindrical container with a flat bottom. Generally used to contain, mix or stir
solutions.
 Fig 1.4 Beaker

6. Funnel
A plastic tube that is wide at the top and narrow at the bottom, used for guiding
liquid or powder into a small opening.

Fig 1.5 Funnel

7. Retort Stand
It is a scientific equipment, clamps can be attached to hold other pieces of
equipment.

Fig 1.6 Retort stand 6

1.2.1 CHEMICALS USED

The following chemicals are required for the experiment:
 ● Hydrochloric acid (HCl)
● 0.5M Sodium Hydroxide (NaOH)
● Phenolphthalein indicator
● Distilled water

1.2.3 PROCEDURE
1. The 50cm3 burette is first washed with distilled water and then rinsed with the 0.5M
NaOH solution.
2. The burette is filled with the NaOH solution, with the aid of the funnel, above the
0cm3 mark and is allowed to run through the tap to ensure that the tip of the
burette is filled.
3. No air bubbles should be trapped below the tap nor should there be any leakages of
the solution.
4. The initial burette reading is recorded in the table given below.
5. The 25cm3 pipette is washed with distilled water, then with the HCl solution.
6. The pipette is used to transfer 25cm3 of HCl into the 250cm3 conical flask.
7. The tip of the pipette is touched onto the surface of the liquid. The last drop should
not be blown out so that the conical flask contains exactly 25cm3 of HCl solution.
8. 1-2 drops of phenolphthalein indicator is added in the flask containing the HCl
solution.
9. The NaOH is run into the HCl while the latter is being a stirred.
10. The NaOH is released dropwise when approaching endpoint so as there is no excess
of NaOH in the flask.
11. Endpoint is denoted by the colour change.
12. The final burette reading is recorded in the table.
13. The titration is repeated at least twice with a difference not more than 0.1cm3
between the values. An average is then calculated to determine the molarity of the
HCl solution.

1.3 OBSERVATIONS:
● When phenolphthalein is added to the solution in the conical flask (HCl (aq)), the solution
does not change colour. It remains clear.
 ● When the tap of the burette is opened and NaOH (aq) was running out into the conical
flask, a pink solution is obtained. However, upon swirling the solution returned
colourless.

● At endpoint a permanent pale pink solution is obtained.

1.4 Results and calculation

RUN 1 RUN 2 RUN3

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Final burette reading/cm 23.30 46.70 23.30
Initial burette reading/cm3 00.00 23.30 00.00
Volume of NaOH used/cm3 23.30 23.40 23.30
Best titre value ✓ ✓

Average titre value → (23.30+23.30)/2

→ 23.30 cm3

From equation: HCl(aq) + NaOH(aq) → H2O(l) + Na+(aq) + Cl-(aq)

1 mole of HCl react with 1 mole of NaOH
Mole → (conc x V)/1000
→ (0.5 x 23.30)/1000
→ 0.01165 mol
Number of mol of NaOH: 0.01165 mol

From the equation above

1 mole of NaOH reacts with 1 mole of HCl
NaOH : HCl
1 mole : 1 mole

Hence, 0.01165 mol of NaOH reacts with 0.01165 mol of HCl

25 cm3 of HCl solution contains 0.01165 mol of HCl
Therefore, 1000 cm3 of HCl → (0.01165/25.0) x 100
→ 0.466 mol of HCl
∴ Molarity of HCl → 0.466 M

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 1.5 CONCLUSION
The acid-base reaction is considered as a neutralisation reaction. On adding the indicator, a
colour change is seen, showing that there is a change in pH of the solution. In this experiment,
0.5M of NaOH was titrated against an unknown concentration of HCl. Using the data given and
the average volume of HCl obtained, the molarity of the latter was found to be 0.466 mol dm -3.

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EXPERIMENT 2: STANDARDISING SODIUM THIOSULPHATE SOLUTION

 2.0 INTRODUCTION
Iodometry is the quantitative analysis of a solution of an oxidizing agent by adding an iodide
which reacts to form iodine, which is then titrated. Iodometric titration is a method of volumetric
analysis, a redox titration where the appearance or disappearance of elementary iodine indicates
the endpoint. A redox titration is one in which both oxidation and reduction occur
simultaneously. A common iodometric titration is the reaction of Sodium Thiosulphate, the
oxidizing agent, against Iodine, using starch as in indicator.

Half equations for the reaction:

I2(aq) + 2e- → 2I-(aq)

2S2O32-(aq) → S4O62-(aq) + 2e-

Overall equation for the reaction:

I2(aq) + 2S2O32-(aq) → S4O62-(aq) + 2I-(aq)

Throughout the titration, the colour changes that occur are from blue-black to pale yellow and a
colourless solution is obtained at end point when the reaction is complete. At that point, all the
iodine has reacted with the thiosulphate ions.

2.1 AIMS AND OBJECTIVES

● To find the molar concentration of Sodium Thiosulphate solution (Na2SO3.5H2O).
● Dilution of solutions.
● To get a better understanding of redox titration, that is the occurrence of oxidation and
reduction simultaneously.

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2.2 METHODOLOGY
2.2.1 APPARATUS

1. Electronic Balance
This device is used to measure the mass of a substance accurately.

Figure 2.0. An Electronic Balance

2. 50 ml measuring cylinder
It is a graduated glass cylinder used to measure the volume of a liquid solution.

Figure 2.1. A Measuring Cylinder

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3. 50 cm3 burette
It is a graduated glass tube, with a tap at one end, used to deliver a known volume
of a solution.
 Figure 2.3. 50 cm3 Burette

4. 250 ml Conical Flask

It is a glass flask with a narrow neck and a flat larger base used to manipulate
solutions to carry out titrations

Figure 2.4. 250 ml Conical Flask

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5. 250 ml Volumetric Flask

A volumetric flask is a piece of laboratory glassware calibrated to contain a
precise volume particular temperature. Volumetric flasks are used for precise
dilutions and preparation of standard solutions.
 Figure 2.5. 250 ml Volumetric Flask

6. 25 cm3 Pipette
A narrow, usually calibrated glass tube into which small amounts of liquid are
suctioned for transfer or measurement.

Figure 2.6. 25 cm3 Pipette

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7. Pipette Filler
A pipette filler is used to safely fill a glass or plastic pipette. It draws
the liquid into the pipette, and accurately regulate or release the liquid.
 Figure 2.7. Pipette Filler

8. Beaker
It is a cylindrical glassware with a narrow neck and a larger base used to heat, mix
or stir substances.

Figure 2.8. Beaker

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9. Retort Stand
A retort stand, sometimes called a clamp stand or a ring stand, is a piece of
scientific equipment, clamps can be attached to hold other pieces of equipment.
For instance, burettes, commonly used for titration experiments, test tubes and
flasks.
 Figure 2.9. Retort Stand

10. Wash Bottle

A wash bottle is a squeeze bottle with a nozzle, used to rinse various pieces of
laboratory glassware, such as test tubes, round bottom flasks, among others.

Figure 2.10. Wash Bottle

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2.2.2 CHEMICALS USED

● Sodium Thiosulphate pentahydrate (Na2SO3.5H2O)

● Potassium Iodide (KI)
● Potassium Iodate (KIO3)
● Sulphuric Acid (H2SO4)
● Starch Indicator

2.2.3 PROCEDURES
● All apparatus are rinsed with distilled water.
● 1.08g of KIO₃ is weighed using the electronic balance. It is then dissolved using distilled
water in a 250cm³ volumetric flask and made up to the 250cm³ mark. The solution is
shaken well to allow the contents to be thoroughly mixed to form a uniform solution.
● A small portion of Sodium Thiosulfate Pentahydrate, Na₂SO₃.5H₂O is used to rinse a
burette then filled with the Na₂SO₃.5H₂O solution up to the 0.00 cm³ mark. The Initial
burette reading is recorded in a table.
● A pipette is rinsed with a small portion of Potassium Iodide, KIO3 and 25cm³ of the KIO3
solution is pipetted with the help of a pipette filler and is transfer into a 250cm³ conical
flask.
● Using a 50cm³ measuring cylinder, 20cm³ of 1 mol Sulfuric Acid, H₂SO₄ and 10cm³ of
0.5 mol KI solution, which are both in excess, are added to the conical flask. The solution
turns brown.
● The mixture is then titrated against the Na₂SO₃.5H₂O from the burette until is turns pale
yellow.
● 5 drops of starch indicator is added to the mixture. The solution turns blue-black. The
titration resumes, by adding this time the Na₂SO₃.5H₂O solution dropwise, until the
mixture turns colourless.
● A 30s of waiting time is allowed in case of re-oxidation of the iodine. If it occurs,
titr
ation continues until the solution remains totally colourless even when the solution is
exposed to air. The end-point of the titration, Final burette reading is then recorded in a
table.
● The experiment is repeated two more time and the burette readings are recorded in a
table. The titre value, volume of Na₂SO₃.5H₂O used is calculated using the equation Final
burette reading - Initial burette reading. An average of the two best titre value is
calculated. 17
2.3 OBSERVATIONS
● When H2SO4(aq) and KI is added into the conical flask already containing 25cm3 KIO3, the
solution turns brown.
 Fig 2.11 Brown solution

● The burette’s tap is open and some Na2SO3.5H2O is allow to flow into the conical flask.
The flow of solution is carefully controlled until the mixture completely turns into a pale
yellow solution.

Fig 2.12. Brown solution turned completely pale yellow

● About 5 drops of Starch Indicator is added to the pale yellow solution and stirred. A blue
black solution is then obtained.

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 Fig 2.13 After addition of Starch Indicator

● The Burette is opened again and Na2SO3.5H2O allowed to run, this time dropwise, until
the mixture completely turns colourless.

Fig 2.14 End point of reaction

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2.4 CALCULATIONS
 Mass of KIO3 in 250cm3
Using the equation: I₂(aq) + 2S₂O₃2-(aq) ⟶2I-(aq) + S4O62-(aq)
Ratio of S2O32- : I-
2:2
1:1
0.1 mol : 0.1 mol
Number of mol of I-: 0.1mol

Using the equation involving iodate(V) and iodide:

IO3-(aq) + 6H+(aq) + 5I-(aq) ⟶3I2(aq) + 3H2O(l)
Ratio of I- : IO3-
5:1
0.1 mol : 0.02 mol
Number of mol of IO3-: 0.02 mol

1000cm3 ⟶0.02 mol KIO3

25cm3 ⟶(0.02/1000) x 250
→ 5.0x10-3 mol KIO3
Number of mol of KIO3: 5.0x10-3 mol

Mole = Mass/Mr
Mass = Mole x Mr
Mass = 5.0x10-3 x 214
Mass = 1.07g KIO3

Since KIO3 is 99% pure

99% → 1.07g
100% → 1.08g

Rough 1st Accurate 2nd Accurate

Final burette reading/cm3 31.50 31.20 37.30
Initial burette reading/cm3 00.00 00.00 05.10
Volume of Na2SO3.5H2O/cm3 31.50 31.20 31.20

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Average Titre value = 31.20cm3 Na2SO3.5H2O
 2.5 CONCENTRATION OF THIOSULFATE

0.02 mol of KIO3 was used

1000cm3 → 0.02 mol KIO3
25cm3 → (0.02/1000) x 25
→ 5x10-4 mol KIO3

Using equation: IO3-(aq) + 6H+(aq) + 5I-(aq) → 3I2(aq) + 3H2O(l)

mol ratio of IO3- : I2
1:3
5x10 mol : 1.5x10-3 mol
-4

Using equation: I2(aq) + 2S2O32-(aq) → 2I-(aq) + S4O62-(aq)

mol ratio of I2 : S2O32-
1:2
1.5x10 : 3.0x10-3
-3

Mol = (Conc x Volume)/1000

Conc = (Mol x 1000)/Volume
Conc = (3.0x10-3 x 1000)/31.20
Conc = 0.096

∴ Concentration of Thiosulfate = 0.096M

2.6 CONCLUSION

The experiment was about the standardisation of sodium thiosulfate, calculating it concentration
by titration of potassium iodate and involving an excess of both potassium iodide and sulfuric
acid. After obtaining consistent titre values, an average is calculated, the concentration of
thiosulfate was calculated and obtained as 0.096 mol dm-3. The concentration value would have
been more accurate if the limitation encountered were reduced or eliminated.

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2.7 SAFETY
 ● Safety glasses and gloves are to be worn whenever working with acids, bases, or any
flammable materials.
● Let the instructor know immediately about any glassware breakage or chemical spills that
may occur so that proper clean-up procedures can be instituted.
● Use pipette fillers whenever pipetting any fluid.
● Dispose of all used solutions in an approved manner as directed by the instructor.
● Clean all spatulas, glassware, and dishes after use and before storage to prevent
contamination.

2.8 PRECAUTION

● Usually an air bubble is present in the nozzle of the burette, it must be removed before
taking the initial reading.
● There should not be any leakage from the burette during titration.
● Keep your eye in level with the liquid surface while taking the burette reading or while
reading the pipette or measuring flask among others.
● Always read lower meniscus in case of colourless solution and upper meniscus in case of
coloured solutions.
● Do not blow through the pipette to expel the last drop of solution from it, simply touch
the inner surface of the titration flask with the nozzle of the pipette for this purpose.
● Shaking of the titration flask should be continuous during adding the solution from the
burette.
● Use your index finger while pipetting the solution.

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2.9 REFERENCES
All the photos above mentioned were obtained from the following websites
● http://www.digipac.ca/chemical/mtom/contents/chapter4/titration.htm
● https://www.labdepotinc.com/articles/titration.html
● https://www.sciencecompany.com/LDPE-Narrow-Mouth-Wash-Bottle-500mL-16oz-
P6413.aspx
● https://www.rapidonline.com/rvfm-laboratory-retort-stand-set-13-014
● http://monscientific.com/wp/product/250ml-beaker/
● https://www.amazon.es/dynalon-311105-pi-pump-pipeta-Filler-
volumen/dp/B004AHL73I
● https://www.coleparmer.in/i/cole-parmer-short-length-serological-pipette-25-ml-
ind-pack-100-cs/3456757
● https://www.brandtech.com/product/volumetric-flasks/
● https://www.indiamart.com/proddetail/250ml-conical-flask-17268919355.html
● https://www.coleparmer.in/i/cole-parmer-burette-buret-and-burette-stand-kit-
burette-clamp-and-stand/2500055
● https://www.amazon.com/Graduated-Cylinder-Measuring-Bottle-
Cleaning/dp/B01K6NHPN
● https://www.indiamart.com/proddetail/electronic-balance-10738178962.html

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