ARAKA BRAMWEL MBOGO

EN251-O221/2010
EXPRIMENT 1: VOLUMETRIC ANALYSIS
24TH MAY 2011

Aims:
To determine the RAM of an unknown metal X.
To determine the accuracy of volumetric analysis experiments.
To identify the various errors that arise during titration experiments.
To determine the sources of any errors found.

Introduction:
Volumetric analysis is a type of quantitative analysis.
Quantitative analysis is a method used for the determination of the absolute or relative abundance
(concentration) of one, several or all particular substance(s) present in a sample.
Quantitative analysis is divided into Gravimetric analysis and Volumetric analysis.
Gravimetric analysis refers to a set of methods in analytical chemistry for the quantitative
determination of an analyte based on the mass of a solid.
Though gravimetric analysis takes long time, it has minimal instrument error and is, therefore, much
more accurate.
Volumetric analysis, on the other hand, is a method in which the amount of a substance is determined
by measuring the volume of a second substance that combines with the first in known proportions.
It is used to determine the unknown concentration of a known reactant.
It takes a shorter time and though the results are not very accurate, they are satisfactory.
Volumetric analysis is also called titrimetric analysis or titration.
The solution of unknown concentration is called the analyte or titrand.
The reactant solution whose concentration is known is called the titrant or titrator.
An indicator is used to determine the endpoint of the reaction. At the endpoint, the indicator changes
color permanently.
The endpoint is the point at which the titration is complete, as determined by the indicator.
The volume obtained at the end of the titration is called the titre.
Some examples of indicators are methyl orange, methyl red, phenophthalein and bromothymol blue.
Some titrations, though, do not need indicators; e.g a redox titration using potassium permanganate.
There are various types of titrations.
The two main ones are:
a. Acid-base titration → based on neutralization reactions occurring between an acid and a base
when mixed in solution.
b. Redox titration → based on a redox reaction between an oxidizing agent and a reducing agent.
Other types are complexometric titration and zeta potential titration.
Apparatus:
Electronic balance
250 ml Volumetric Flask
Conical Flask
50 ml Burette
25 ml Pipette
Stand and Clamp

Reagents:
A metal carbonate (X2CO3)
0.1M Hydrochloric acid
Methyl red indicator
Distilled water

Method:
1.32g of the metal carbonate (X2CO3) was weighed out accurately into a clean and dry 250ml volumetric
flask.
About 100ml of distilled water was added and stirred till the crystals dissolved.
The volume of the solution in the volumetric flask was the adjusted to the mark.
This was the analyte.
25ml of the solution was pipette into a 250ml conical flask.
Two to three drops of methyl red indicator were added and titrated with standard 0.1M hydrochloric
acid (the titrant).
The titrations were repeated until the titres agreed to 0.05cm 3 and the results recorded.
Results:

Titration 1 (× 10-5 m3) Titration 2 (× 10-5 m3) Titration 3 (× 10-5 m3)

Final volume 2.360 4.730 2.350

Initial volume 0.00 2.36 0.00

Volume used 2.360 2.370 2.350

Titration1+Titration 2+Titration3
Average titre =
3
2.36+2.37+2.35 7.08
= =
3 3
= 2.36 × 10-5 m3

Weight of X2CO3 = 1.32g

= 1.32 × 10-3 Kg
Calculations:
( H = 1.0 Cl = 35.5 C = 12.0 O = 16.0 )

(a) Write a balanced chemical equation for the reaction between hydrochloric acid and X 2CO3
carbonate solution.
2HCl (aq) + X2CO3 (aq) → 2XCl (aq) + CO2 (g) + H2O (l)

(b) (i) How many moles of the acid took part in the reaction?
Moles = Molarity × Volume (dm3)
= 0.1 × 23.6 ×10-3
=0.00236 moles

(ii) Hence calculate the molarity of the carbonate solution in moles/dm 3.

Mole ratio = 2 : 1
Moles of X2CO3 = 0.00236 ÷ 2
= 0.00118 moles
25ml = 0.00218 moles
1000ml = y
1000× 0.00118
y=
25
= 0.0472 moles/dm3

(iii) Also calculate the concentration of the metal carbonate solution in g/dm 3.
250ml = 1.32g
1000ml = p
1000× 1.32
P=
250
= 5.28 g/dm3

(c) Calculate the relative formula mass (R.F.M) of the metal carbonate X2CO3
RFM = mass ÷ moles
=5.28 ÷ 0.0472
= 111.86
=112

(d) Calculate the atomic mass (R.A.M) of X.

CO3 = 12 + 48 = 60
X2 = 112 – 60 = 52
X = 52 ÷ 2 = 26
Hence RAM of X = 26
 (e) Identify metal X with the help of a periodic table.
Metal X is Sodium (Na)
Discussions:
In any experiment, there can’t be 100% accuracy.
Some errors arise during the course of the experiments, volumetric analysis included.
This is the main reason why the RAM of metal X which is most likely to be Sodium was found to be 26
instead of 23.
The deviation was caused by various errors that probably occurred in the experiment.
These include:
a. Parallax error
b. Instrument error
c. Indicator error
d. contamination
Parallax error might have occurred when adjusting the solution in the volumetric flask to the mark when
making the analyte. It may have occurred also when pipetting the analyte into the flask.
It may also have occurred when making readings of the titrant from the burette.

Instrument error arises from improper calibration of the experimental instruments, e.g the burette,
pipette or electronic balance.
It may have been existing when weighing out the mass of X2CO3 or when making the burette readings.

Indicator error is an indeterminate error characterized by the slight difference between the change in
indicator color and the actual end point of the titration.
This is due to the very sharp nature of the transitions.

Contamination may have occurred in the experiment especially when performing the experiment for
the second and third time due to improper cleaning of the apparatus used.

Systematic errors may also have occurred due to environmental changes when taking the weight or
measurements, e.g changes in temperature or presence of wind.

Conclusion:
The R.A.M of the unknown metal X was found to be 26.
The metal is therefore in the third period.
From the formula X2CO3 the metal X has valency 1.
The metal was therefore predicted to be Sodium.
The real RAM of sodium is 23. The deviation was due to the various experimental errors.
The experiment was therefore successful.
References:

Modern Experiments for Introductory Chemistry

by H.A Neidig and Wilmer J Stratton
http://en.wikipedia.org/wiki/Quantitative_analysis_%28chemistry%29
http://en.wikipedia.org/wiki/Titration