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Volumetric Analysis: Lab Report

1) The document is a lab report that details the procedures and results of volumetric analysis experiments to determine the concentration of unknown solutions. 2) Key results include determining the concentration of potassium permanganate, nitrite solution, sodium thiosulphate, and the percentage of chlorine in Clorox. 3) Accuracy could be improved by repeating titrations to obtain consistent results within 0.05 readings and avoiding overshooting of titration volumes.

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Jeff Lim
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395 views6 pages

Volumetric Analysis: Lab Report

1) The document is a lab report that details the procedures and results of volumetric analysis experiments to determine the concentration of unknown solutions. 2) Key results include determining the concentration of potassium permanganate, nitrite solution, sodium thiosulphate, and the percentage of chlorine in Clorox. 3) Accuracy could be improved by repeating titrations to obtain consistent results within 0.05 readings and avoiding overshooting of titration volumes.

Uploaded by

Jeff Lim
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Download as PDF, TXT or read online on Scribd
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Lab Report

Title

VOLUMETRIC ANALYSIS

Name : Lim Kah Hou


Matric No : U2103352/1
Group : Occurrence 2
Experiment no : A2
Date : 10 January 2021
Lecturer : Dr Nor Asrina Binti Sairi
Procedure
The experiment was carried out according to SIC 1011 Basic Laboratory Techniques Manual

Objectives
1. To determine the concentration of an unknown solution using standardised solution

Results
A1. Preparation of standard sodium oxalate solution
Mass of sodium oxalate salt used: 0.3030g
Volume of sodium oxalate prepared: 100ml
Concentration of sodium oxalate solution: 0.0226 mol L-1

Standardisation of Potassium Permanganate solution (KMnO4)


Potassium permanganate solution is standardised by titration against standard sodium oxalate
solution
Trial Initial Reading (ml) Final Reading (ml) Volume used (ml)
1 6.10 16.10 10.00
2 16.10 26.2 10.10

Volume of sodium oxalate used = 25.00 ml


Average volume of KMnO4 used = 10.05 ml

5𝐶2 𝑂4 2− + 2𝑀𝑛𝑂4 − + 16𝐻 + → 10𝐶𝑂2 + 2𝑀𝑛2+ + 8𝐻2 𝑂


5 moles of oxalate ions react with 2 moles of permanganate ions
𝑀𝐾 𝑉𝐾 2
= K = KMnO4 solution, S = Sodium oxalate solution
𝑀𝑆 𝑉𝑆 5

By using the formula above, the concentration of KMnO4 can be calculated


Concentration of KMnO4 = 0.0225 mol L-1
A2. Determination of concentration of Nitrite solution
Trial Initial Reading (ml) Final Reading (ml) Volume used (ml)
1 2.62 29.7 27.08

Volume of nitrite solution used = 8 ml


Volume of KMnO4 used = 10 ml
Volume of iron(II) ammonium sulphate used = 27.08 ml
Concentration of iron(II) ammonium sulphate solution = 0.0104 mol L-1
2𝑀𝑛𝑂4 − + 10𝐹𝑒 2+ + 16𝐻 + → 10𝐹𝑒 3+ + 2𝑀𝑛2+ + 8𝐻2 𝑂……………eq①
2
𝑛= 𝑀𝐹𝑒 𝑉𝐹𝑒 Fe = iron(II) ammonium sulphate solution, n = mole of KMnO4 in excess
10

5𝑁𝑂2 − + 2𝑀𝑛𝑂4 − + 6𝐻 + → 5𝑁𝑂3 − + 2𝑀𝑛2+ + 3𝐻2 𝑂……………eq②


𝑀𝑁 𝑉𝑁 5
= N = nitrite solution, K = KMnO4 solution
𝑀𝐾 𝑉𝐾 −𝑛 2

By applying these formulae, the concentration of nitrite solution can be found


Concentration of nitrite solution = 0.0527 mol L-1

B1. Preparation of standard potassium iodate solution


Mass of potassium iodate salt used: 0.2007 g
Volume of potassium iodate prepared: 100 ml
Concentration of potassium iodate solution: 9.385 × 10-3 mol L-1

Standardisation of sodium thiosulphate solution


Sodium thiosulphate solution is standardised by titration against iodine in potassium iodate
Trial Initial Reading (ml) Final Reading (ml) Volume used (ml)
1 5.00 18.60 13.60

Volume of potassium iodate used = 25.00 ml


Mass of potassium iodide used = 1.0091 g
Volume of sodium thiosulphate used = 13.60 ml
𝐼𝑂3 − + 5𝐼 − + 6𝐻 + → 3𝐼2 + 3𝐻2 𝑂……………eq ①

2𝑆2 𝑂3 2− + 𝐼2 → 𝑆4 𝑂6 2− + 2𝐼 − ………………eq②
By combining eq 1 and eq 2, the overall reaction is:

𝐼𝑂3 − + 6𝑆2 𝑂3 2− + 6𝐻 + → 3𝑆4 𝑂6 2− + 𝐼 − + 3𝐻2 𝑂

𝑀𝐼 𝑉𝐼 1
= I = potassium iodate solution, S = sodium thiosulphate
𝑀𝑆 𝑉𝑆 6

By using the formula above, the concentration of sodium thiosulphate can be calculated
Concentration of sodium thiosulphate = 0.1035 mol L-1

B2. Determination of concentration of hypochlorite


Trial Initial Reading (ml) Final Reading (ml) Volume used (ml)
1 18.60 27.40 8.80

Volume of Clorox used = 10 ml


Mass of potassium iodide used = 1.0262 g
Volume of sodium thiosulphate used = 8.80 ml
𝐶𝑙𝑂− + 2𝐼 − + 2𝐻 + → 𝐼2 + 𝐶𝑙 − + 2𝐻2 𝑂……………eq①

2𝑆2 𝑂3 2− + 𝐼2 → 𝑆4 𝑂6 2− + 2𝐼 − ……………eq②
By combining eq1 and eq 2,

𝐶𝑙𝑂− + 2𝑆2 𝑂3 2− + 2𝐻 + → 𝐶𝑙 − + 𝑆4 𝑂6 2− + 2𝐻2 𝑂


𝑀𝐶𝑙 𝑉𝐶𝑙 1
= Cl = perchlorite, S = sodium thiosulphate solution
𝑀𝑆 𝑉𝑆 2

By using the formula above, the concentration of perchlorite can be determined


Concentration of perchlorite = 4.554 × 10-2 mol L-1
Concentration of perchlorite in % Cl2:
Mole of Cl2 present in Clorox = 12 𝑐𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑜𝑓 𝑝𝑒𝑟𝑐ℎ𝑙𝑜𝑟𝑖𝑡𝑒 × 0.01𝐿
1
= 2 (4.554 × 10−2 ) × 0.01
= 2.277×10-4 mol
% Cl2 in Clorox = 2.277 × 10−4 × 2(35.45) × 100%
= 1.614%

Discussion
In the first half of the experiment, the concentration of potassium permanganate(KMnO4)
is standardised by direct titration against sodium oxalate with known concentration. Through
titration, the concentration of KMnO4 is calculated, 0.0225 mol L-1, and it is used as the primary
standard for the next part of the experiment, that is to determine the concentration of nitrite solution.
In order to determine the concentration of nitrite solution, a back titration is used instead because
the change when nitrite react with permanganate ion is not as glaring as the reaction of
permanganate ion and iron(II) ion. By means of back titration, the concentration of nitrite was
found to be 0.0527 mol L-1.
Moving on to the second half of the experiment, similar standardisation process is done on
sodium thiosulphate against iodine in potassium iodate and the concentration of sodium
thiosulphate is calculated to be 0.1035 mol L-1. Standardised sodium thiosulphate is then used to
determine the %Cl2 of Clorox, which found to be 1.614%.
In this experiment, the standard solution is the most crucial component at determining the
concentration of an unknown solution. This is because the concentration of the standard solution
will be used to calculate the concentration of that unknown solution. Hence, the procedure of
standardising the solution plays a huge role at the accuracy of the data. To improve the accuracy,
the standardising procedure must be done repeatedly to obtain a consistent reading, which does
not differ more than 0.05.
The results of this experiment are said to be relatively inaccurate because for the most part
of the experiment, the titration was carried out without any repetition. This greatly affect the
accuracy of the reading as first trial was most likely to be overshot due to the volume needed being
uncertain. Hence, to avoid such problem, the experimenter should carry out the titration at least 3
times to obtain precise reading.

Questions
1. What is an acid base indicator and how it is been used for?
Acid base indicator refers to either a weak acid or weak base that shows colour changes
as pH value of the solution changes. It is usually used in acid-base titration to detect the endpoint
of the reaction, in other word, to the determine at which neutralisation is completed.
2. How to determine the equivalance point of a titration?
In order to determine the equivalence point, an indicator is usually required. The most
classic indicator used would be the acid-base indicators such as phenolphthalein or methyl orange.
The equivalence point can be obtained when the colour of the indicator changes, which indicates
the reaction is completed. Alternatively, a pH meter can be used to determine the equivalence point
as well.

Conclusion
The objective was able to achieve. The concentration of nitrite solution was able to be
determined by titration using standardised potassium manganate solution, which is 0.0527 mol L-
1
. On the other hand, the % Cl2 of Clorox is found to be 1.614%.

Reference
• SIC1011 Safety and Basic Laboratory Techniques Lab-Manual
• Equivalent Point. (2019). Retrieved from 12 January 2022,
https://chemdictionary.org/equivalence-point/

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