Titration Techniques

To reduce the concentration of a solution

1. M1V1=M2V2
2. Always use a volumetric flask to achieve a dilution (Calculate volume needed to
achieve dilution in a 250cm^3/100cm^3 volumetric flask)
Prepare standard solution from solid weighed
1. Weigh using electronic balance in a weighing bottle
2. Transfer into 100cm^3 beaker and add 50cm^3 of deionised water using measuring
cylinder. Glass rod to stir and dissolve.
3. Reweigh weighing bottle to ensure __ solid transferred.
4. Transfer all solution and washings into volumetric flask. Use dropper to top up to the
mark. Stopper and shake to obtain homogenous solution.
Titration
1.
2.
3.
4.

Top up 50.00cm^3 burette with ___

Pipette 25/10.0 cm^3 of __ into conical flask.
Add indicator if necessary. Place on white tile if colour change present.
Take initial burette reading, titrate (conical flask) against (burette) and swirl
continuously until colour change.
5. Record final burette reading.
6. Repeat titration until 2 titre values within +- 0.1cm^3 of each other.
7. Preliminary calculation involves ensuring do not use too much of titre
Gravimetric analysis
Gravimetric analysis
1. Weigh crucible and then solid and transfer solid to crucible.
2. Heat solid gently first using Bunsen burner and then strongly for 10 min.
3. Cool solid. Weigh the crucible with solid and repeat heat cool weigh process until
constant mass.
Gas collection
Gas Collection with frictionless graduated gas syringe
1. Set up apparatus (Conical flask connected to gas syringe, Set-up can contain
dropping funnel)
2. Record initial reading of syringe
3. Add all reactants and allow reaction to occur
4. Measure final reading of syringe when it has equilibriated to room temperature and
pressure (no change)
5. If purification of gases is needed, able to pass gas through beaker/U-tube of drying
agents

6. Preliminary calculation involves ensuring volume of gas produced does not exceed
gas syringe volume
Energetics
Determining enthalpy change of solution (involve temperature correction)
1. Use burette to add solvent into Styrofoam cup. Record initial temperature every 30
seconds for a period of 2.5 minutes.
2. At exactly 3 minutes, weigh solid and dissolve in cup. Measure the temperature every
30 seconds from 3.5 minutes to 10 minutes.
3. Plot graph of temperature against time to determine temperature change.
Enthalpy change of reaction
1.
2.
3.
4.
5.

Prepare both solutions in separate Styrofoam cups first.

Measure weighted average of initial temperature of both solutions.
Add both solutions together and measure highest/lowest temperature reached.
Manipulate to obtain enthalpy change.
Assumption is water density is 1g/cm

Thermometric titration
1.
2.
3.
4.

Set up apparatus and fill burette with (reagent to be used as titre)

Fill dry styrofoam cup in beaker with reagent 2.
Record initial temperature.
Add 2.0cm^3 of titre and record max temperature change. Repeat until ___ of titre has
been added. Stir gently after each addition.
5. Plot graph of temperature vs volume of titre added
Calorimeter
1. Set up apparatus
2. Weigh spirit burner containing the fuel to be burnt using
electronic balance.
3. Using burette, place 100cm^3 of water into a copper
calorimeter.
4. Record initial temperature of water.
5. Ignite the fuel and heat up the water until 10 degree increase
in temperature. Record max rise in temperature.
6. Cool and reweigh the spirit burner with the fuel.
7. Calculation
Kinetics
Combination of different techniques to track change over time

1.
2.
3.
4.
5.

Measuring volume of gas produced at regular time intervals

Measuring change in mass at regular time intervals on an electronic balance
Measuring change in colour using colourimeter over time
Measuring change in gas pressure using manometer
Measuring change in electrical conductivity using 2 electrodes and conductivity
meter
6. Measure concentration at intervals via titration (including quenching which
involves addition of large volume of water/base to neutralize acid or plunging
mixture in ice)
7. Ensuring that all other reactants are kept in large excess for concentration time
method
Initial rates method (involves clock reaction)
1. Mix reactants together, but vary the volume of the reactant that we want to determine
order, keeping to other volumes constant, but ensuring TOTAL VOLUME remains
constant.
2. Use stopwatch to measure time taken when distinct visual change observed/X on
white tile cannot be seen anymore.
Electrochem experiments
Measuring cell voltage
1. Ensure that concentration and volume of solutions at each electrode is the SAME
2. Measure cell voltage on voltmeter multiple times and take average
Other experiments (to determine charge/Avogadro/faraday)
1. Involves measurement of cathode/anode mass, time given and current passed should
remain constant at 1A.
Inorganic synthesis/QA
Anions
1. To differentiate SO3- from SO4-, add BaCl2 followed by dilute nitric acid. Precipitate
formed for SO3- will dissolve in dilute nitric acid.
2. To differentiate SO3- from other ions, just add dilute nitric acid, will form SO2 gas
that decolourises KMnO4.
3. To differentiate NO3- from NO2-, add dilute nitric acid, brown gas formed for NO2-.
4. To differentiate NO3-, NO2- from the rest, add aluminium foil and heat, pungent NH3
produced.
5. To differentiate between Cl-, Br-, I-, use silver ions and ammonia.
6. To differentiate carbonate ions, add dilute acid and CO2 liberated.
Organic synthesis Methods
Reflux/distillation

1. Reflux Set-up. Remember to add boiling chips.

2. The round bottom flask can also be cooled in ice-baths.

Separation techniques
1. Using separation funnel (Opening/closing of tap)
a. Obtain Organic layer, discard aqueous layer, add drying agent, filter and
evaporate the solvent away.
2. Using Buchner funnel with vacuum pump
3. Evaporation to dryness of filtrate
Recrystallization
1.
2.
3.
4.
5.

Dissolve solid in minimal volume of hot solvent in conical flask.

Filter hot solution to remove any impurities
Cool saturated solution in ice-bath to obtain solid crystals.
Filter to obtain solid crystals
Wash with small volume of cold solvent and allow to dry