Class: SSS 2
Subject: Chemistry
Topic: VOLUMETRIC ANALYSIS
Learning Objectives: At the end of this lesson, learners should be able to;
⦁ define basic terms in volumetric analysis
⦁ list apparatus used in volumetric analysis
⦁ outline the procedures and precautions during acid-base titration.
Carry out acid base titration.
Create acceptable table of titre values
Calculate unknown concentration of quantities in g/dm³ and mol/dm³
Calculate percentage purity and impurity
Calculate water of crystallization and heat of neutralization.
Definition of Basic Terms in Volumetric Analysis
Volumetric analysis is an aspect of quantitative analysis which involves the measurement of the
volume of reacting solutions. The other aspect of quantitative analysis is gravimetric analysis,
which involves weighing and determining the masses of reactants and products of a chemical
reaction.
The most popular aspect of volumetric analysis is the acid-base (neutralization) reactions. The
technique of determination is by titration. Other aspects are redox and precipitation reaction.
Titration: is the technique for carrying out volumetric analysis. Titration is a procedure in which
a solution called the titrant whose concentration is known is dispensed from the burette and
reacted with a known volume of another solution of unknown concentration called the analyte.
End point: is the point at which the chemical reaction is complete during titration. The end point
is detected with the help of an indicator.
Indicators: These are weak organic acids or bases whose colours change with pH of the solution.
Indicators are widely used in monitoring titration involving colourless solutions of acids and
bases.
Different Indicators and their Colours in Different Media
Acid-base indicators are dyes that change colour when according to the pH of the
medium. The table below shows some titration and their suitable indicator:
Acid / base Indicator
Strong acid and strong methyl orange
base or
phenolphthalein
Strong acid and weak methyl orange
base
Weak acid and strong
phenolphthalein
base
No suitable
Weak acid and weak base indicator
Concentration: The concentration of a solution is the amount of solute in a given volume of the
solution. It can be expressed as mol/dm3 or g/dm3.
Molar concentration
The molar concentration of a compound is one which contains one mole or the molar mass of
the compound in 1 dm3 of the solution. It can be expressed as mol/dm3
Mass concentration
The mass concentration of a compound is the mass of the compound contained in 1 dm 3 of
solution. The unit is g/dm3
Relationship between Molar concentration and Mass concentration
Concentration (C) = number of moles (n)
Volume (V)
Number of moles, n = C x V
But, number of moles, n= m/M Where M = molar mass and m = mass
Substituting n=m/M into n = C x V
Therefore, mass concentration = molar concentration x molar mass
Standard Solution: It is a solution containing a known amount of solute in a known volume of
solution. An example of a standard solution is a molar solution.
For instance, a solution known to contain exactly 10.6g of anhydrous sodium
trioxocarbonate (IV), Na2CO3, in 1 dm3 of solution is a standard solution.
Apparatus Used in Volumetric Analysis
The apparatus used in volumetric analysis are: burette, pipette, beaker, flasks, funnel, wash
bottle, chemical balance, dropping pipette and retort stand.
(vii) End Point:
General Procedure and Precautions during Acid-Base Titration
A. Steps Involved in Filling the Burette with Dilute Acids
Step 1: Clamp the burette in a vertical position to avoid error due to parallax while taking
reading. Rinse it with the given acid solution, allowing part of the acid to pass through the tap
and the jet. Then close the tap.
Step 2: With the funnel at the top of the burette, fill the burette with acid to a desired level
ensure that the jet is filled with acid to avoid air bubbles inside [Link] close the burette tap to
avoid leakages. Remove the funnel to avoid droplets of acid from it. Hold a piece of white paper
behind the burette so that the acid level is clearly shown and note the reading of the burette.
B. Steps Involved in Measuring 25.00Cm3 (20.00Cm3) of Standard Base Solution
Step 1: Collect four conical flasks and wash with distiled water only. Make sure that none of the
flasks contain any acid or alkali.
Step 2: Rinse the pipette with the given base solution.
Step 3: Suck the base solution into the pipette until the level is about 1cm3 or2cm3above the
forefinger. Gently release the pressure until the bottom of the concave meniscus is at the
graduation mark,with the eye level aligned.
Step 4: While filing the pipette ensure that the jet lies well inside the base solution to avoid air
bubbles in the pipette.
Step 5: Run the base solution into one of the conical flasks. The sides of the flask should not be
splashed with the solution as the splashings may not be neutralised by acid later in the
experiment. To remove the little alkali retained at the tip of the pipette after delivery, do not
blow out the pipette or shake out the last drop of the solution but allow the pipette to drain for
about 15 seconds and then allow the tip of the pipette to touch the bottom of the flask.
Step 6: Fill the remaining conical flasks as stated above.
C. Steps Involved in the Titration of the Alkali Solution with Diluted Acid Solution
Step 1: Add 2 drops of the given indicator to each conical flask to obtain a shape end-point.
Step 2: Place one of the conical flasks on a piece of white paper or white tile beneath the burette
to aid easy recognition of colour change at the end [Link] in the acid from the burette adding
about 1.00cm3 at a time.
Shake the conical flask gently during titration to ensure homogeneity of the two solutions but
avoid spillage of the reacting solutions. Note the level of the acid when the colour of the
indicator [Link] first titration is the trial or rough titration.
Step 3: Repeat the above procedures for the base in other three conical flasks. Take burette
readings at the lowest concave meniscus for each titration.
These should be taken at the eyes levels to avoid error of parallax. The volumes of the acids
used in the second,third and fourth accurate titrations should agree within ±0.20cm3 and should
always be recorded to two places of decimals. These make a concordant or concurrent results to
be obtained. Record all your readings as they are taken and do not try to remember them or
write on scripts of papers.
Titration Precautions
⦁ The burette must be clamped vertically or not tilted.
⦁ Wash the burette and pipette with water and rinse with distilled water.
⦁ Rinse the burette with acid,the pipette with base (alkali)before putting these solutions into
them.
⦁ Ensure no air bubbles in the burette or pipette.
⦁ Remove the funnel after putting the acid into the burette (if a funnel is used).
⦁ The content of the pipette should be allowed to run into the conical flask without blowing air
into it.
⦁ Use a drop or two (small amount)of indicators.
⦁ Read the lower meniscus.
⦁ Ensure the tap of the burette is not leaking.
NOTE: Most examination bodies have different ways of assessing students practical skills and
report writing procedures. For instance, the following are some of the penalties.
(i) Use of pencil: -2 marks
(ii) Alteration (cancellation) on table of titre values: -2 marks for each, maximum of -4 marks.
(iii) No unit or wrong unit on table: -1 mark.
(iv) Non concordant values (i.e. difference greater than plus or minus 0.2) for average titre
value; -1 mark.
Steps in Recording Observations Made During Acid-Base Titration Experiment
1. Construct the specimen table
Example:
Burette Readings in cm3 Trial or Rough 1st 2nd
Final Burette reading 24.80 24.00 24.00
Initial Burette reading 0.00 0.00 0.00
Volume of Acid used 24.80 24.00 24.00
2. Determine the average volume of acid used (i.e. average titre value).
Thus, Average Titre: 24.00+24.002=24.00cm3
Depending on the differences in readings of the titre values. All your readings must have their
units, i.e.cm3.
NOTE: This value and that of the table should be recorded to two places of decimal.
3. Significant Figures
Student should learn to round off their calculation numbers to three significant figures,since
they are using four figure table for their calculations.
Significant figures start from non-zero digit and all other digits that follow including zero are
considered Significant. As usual the digits, 5,6,7,8,9 are rounded up while 1,2,3,4, are rounded
off.
Numbers Rounded off
299.30 299 to 3 s.f
0.0128 0.0128 to 3 s.f
6.0246 6.02 to 3 s.f
NOTE : for the sake of the examination, prepare your table on a sheet of paper and then neatly
transfer it in INK to the answer sheet.
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