Chapter 3- Experimental techniques and chemical analysis

Measurement apparatus:

1. Time
Unit: minutes, seconds
Apparatus: stop watch, stop clock

2. Volume
● Volume of a gas
Unit: cm3
Apparatus: gas syringe

● Volume of a liquid
Unit: cm3
Apparatus: Burette, pipette, measuring cylinder
most accurate → least accurate

3. Temperature
Unit: °C
Apparatus: Mercury or alcohol Thermometer, Thermometer probe.

4. Mass
Unit: grams (g)
Apparatus: Balance

Experimental techniques:

1. Filtration: The separation of a solid from a liquid using a fine filter paper that does not allow the
solid to pass through

2. Crystallization: The process of forming crystals from a saturated solution.

3. Simple distillation: A distillation method for separating the liquid solvent from a solution
containing dissolved solids.

4. Fractional distillation: A distillation method that uses a fractionating column to separate liquids
with different boiling points
5. Paper Chromatography: A technique used to separate mixtures with different solubilities in a given
solvent.
-It can be used to check the purity of a substance.
- The result of the paper chromatography run can be seen on the chromatogram that
displays the region where the spots of samples have moved to.
- Solvent used: Water, Ethanol or any organic solvent (Ethanoic acid, propanone).
- A locating agent is a chemical used after the chromatogram run to see colorless
substances by producing colored spots or spots that glow under UV light.

IMPORTANT DEFINITIONS

Table 1
 Experimental Techniques and chemical analysis
Interpreting Chromatograms:

1. If two or more substances are the same, they will produce identical chromatograms.
2. If the substance is a mixture, it will separate on the paper to show all the different components as
separate spots.
3. An impure substance will show up with more than one spot, a pure substance should only show up
with one spot.

𝐷𝑖𝑠𝑡𝑎𝑛𝑐𝑒 𝑡𝑟𝑎𝑣𝑒𝑙𝑙𝑒𝑑 𝑏𝑦 𝑠𝑢𝑏𝑠𝑡𝑎𝑛𝑐𝑒

Rf value: 𝐷𝑖𝑠𝑡𝑎𝑛𝑐𝑒 𝑡𝑟𝑎𝑣𝑒𝑙𝑙𝑒𝑑 𝑏𝑦 𝑠𝑜𝑙𝑣𝑒𝑛𝑡 𝑓𝑟𝑜𝑛𝑡

You can increase accuracy of paper chromatography experiment by repeating the experiment, using
different solvents, and measuring Rf values.

Assessing purity.

1. Pure substances melt and boil at specific and sharp temperatures. Eg water has a boiling point of
100°C and a melting point of 0°C
2. Mixtures/ Impure substances have a range of melting and boiling points as they consist of different
substances that melt or boil at different temperatures.
3. Melting and boiling points data can therefore be used to distinguish pure substances from mixtures by
comparing the experimentally derived values to data tables.
example: Melting point analysis is routinely used to assess the purity of drugs. (The closer the
experimentally measured value is to the actual melting or boiling point then the purer the sample is).

Importance of Purity

1. A pure substance consists of only one substance and contains nothing else.
2. To have a pure substance for food and drugs is very important as impurities could be dangerous even
in small amounts
3. For example, if a sample of water melts at exactly 0°C and boils at exactly 100°C then the water is
pure
4. If the melting and boiling points of the water aren’t these exact values then the water must be impure
and contain other substances i.e. it must be a mixture.
 Separation and purification

1) Filtration
Used to separate an undissolved solid from a mixture of the solid and a liquid / solution ( e.g. sand from a
mixture of sand and water.

2) Separating mixture of solids:

- Difference in solubility can be used to separate solids.

- For a difference in solubility, a suitable solvent must be chosen to ensure the desired substance only
dissolves in it and not the other substance or impurity. Eg: to separate a mixture of sand and salt, water is
a suitable solvent to dissolve the salt, but not the sand.

Example: how to separate a mixture of salt and sand.

Keypoints:
Sand: insoluble in water.
Salt: Soluble in water.

Step 1: Using a measuring cylinder add water (e.g. 20cm3 ) into the beaker containing mixture of salt and
sand.
[Salt is soluble in water so it will dissolve whereas sand is insoluble so it settles at the bottom.]

Step 2: Filtration
- Sand will be separated out on the filter paper whereas; salt and water solution
will pass through the filter paper.

Step 3: Evaporation.
-Pour the filtrate (salt and water solution in the previous step) into an
evaporating basin and heat it until the water evaporates and have the salt
crystals separated out.
3) Crystallization
Used to separate a dissolved solid from a solution. When the solid is more soluble in hot solvent than in
cold (e.g. copper sulfate from a solution of copper (II) sulfate in water)

Step 1: Place solution into an evaporating dish and heat it until it becomes a saturated solution.

You can test if the solution is saturated by dipping a clean, dry, cold glass rod into the solution. If the
solution is saturated, crystals will form on the glass rod when it is removed and allowed to cool.

Step 2: Leave the saturated solution to cool down.

As the solution cools down, more crystals will form because solids are less soluble at colder temperatures.

Step 3: Filtration.
Filter out the crystals from the remaining solution using the filter paper and funnel.

Step 4: Allow the crystals to dry. (leave them somewhere warm eg. in sunlight or dry them in the oven).

The method used to separate out mixtures that contain liquids is known as distillation. There are
two types, simple distillation and fractional distillation.

4) Simple Distillation

Used to separate a liquid and soluble solids from a solution (e.g. pure water from saltwater or a pure
liquid from a mixture of liquids).

(example: in this case, to separate out the pure water from seawater)

Step 1: Pour the liquid mixture /solution into a round bottom flask
(which in this case is sea water).

Step 2: Seal the flask with a bung so no gas molecules can escape
and place a thermometer inside the bung to measure the
temperature inside the flask.

Step 3: Connect the flask containing the solution into a condenser. The function of this condenser is
to condense the passing gas molecules back into liquid.

Step 4: Place the bunsen burner at the bottom to provide heating.

Process:

 The solution is heated and pure water evaporates producing a vapour which rises
through the neck of the round-bottomed flask.
 The vapor passes through the condenser, where it cools and condenses, turning into
pure water which is collected in a beaker.
 After all the water is evaporated from the solution, only the solid solute will be left
behind.

5) Fractional Distillation.

Used to separate two or more liquids that are miscible with one another (e.g. ethanol
and water from a mixture of the two)
(miscible: when two liquids form a completely uniform mixture when added
together).

Now, say we have a mixture of ethanol and water and since these two liquids are
completely miscible; The process used to separate these two out will be Fractional
distillation.

 This equipment used for fractional distillation is very similar to simple distillation.
- round bottom flask attached to another equipment called a fractionating column. This fractionating
column is attached to a condenser which leads to the conical flask.

 Fractionating column has two imp functions:

- Its tall (the temp. at the top is cooler than it is at the bottom).
- full of little glass rods to provide a high surface area

Process: (e.g. a mixture of ethanol and water)

 The solution is heated to the temperature of the

substance with the lowest boiling point (in this case, it
is heated to 78℃ - which is the boiling point of
ethanol).
 Ethanol will rise and evaporate first, and the vapors produced will pass through a
condenser, where they cool and condense, turning into a liquid that will be collected in a
conical flask.
 All of ethanol is evaporated and collected, leaving behind the other components(s)of the
mixture.
 When the temperature starts to increase to 100 ºC heating should be stopped. Water and
ethanol are now separated.

(For water and ethanol: ethanol has a boiling point of 78 ºC and water of 100 ºC. The mixture is
heated until it reaches 78 ºC, at which point the ethanol boils and distills out of the mixture and
condenses into the flask).