Experimental Techniques

Time, Temperature, Mass & Volume

Time

 Time can be measured using a stopwatch or stopclock which are usually accurate to one or two
decimal places

 The units of time normally used are seconds or minutes although other units may be used for
extremely slow reactions (e.g. rusting)

 1 minute = 60 seconds

Temperature

 Temperature is measured with a thermometer or digital probe

 Laboratory thermometers usually have a precision of a half or one degree

 Digital temperature probes are available which are more precise than traditional thermometers
and can often read to 0.1 oC

 Traditional thermometers rely upon the uniform expansion and contraction of a liquid substance
with temperature; digital temperature probes can be just as, if not, more accurate than
traditional thermometers

 The units of temperature are degrees Celsius (ºC)

Mass

 Mass is measured using a digital balance which normally gives readings to two decimal places

 Balances must be tared (set to zero) before use

 The standard unit of mass in kilograms (kg) but in chemistry grams (g) are most often used

 1 kilogram = 1000 grams

Volume-liquids

 The volume of a liquid can be determined using several types of apparatus, depending on the
level of accuracy needed

 For approximate volumes where high accuracy is not an important factor, measuring ( or
graduated) cylinders are used

 These are graduated (have a scale so can be used to measure) and are available typically in a
range of sizes from 10 cm3 to 1 litre (1 dm3)

 Volumetric pipettes are the most accurate way of measuring a fixed volume of liquid, usually 10
cm3 or 25 cm3
 o They have a scratch mark on the neck which is matched to the bottom of the meniscus
to make the measurement

 Burettes are the most accurate way of measuring a variable volume of liquid between 0 cm3 and
50 cm3 (e.g. in a titration)

 The tricky thing with burettes is to remember to read the scale from top to bottom as 0.00 cm 3 is
at the top of the column

 Whichever apparatus you use, you may see markings in ml(millilitre) which is the same as a cm3

Diagram of a burette with conical flask and pipette with filler

Volume-gases

 The volume of a gas sometimes needs to be measured and is done by collecting it in a graduated
measuring apparatus

 A gas syringe is usually the apparatus used

 A graduated cylinder inverted in water may also be used, provided the gas isn't water-soluble

 If the gas happens to be heavier than air and is coloured, the cylinder can be used upright
Diagram of the set-up for an experiment involving gas collection

Exam Tip

Be careful when recording time not to mix up seconds and minutes in the same table. If a table heading
shows Time/mins and you record a stop watch display of 1.30, meaning 1 minute and 30 seconds, that is
wrong as it should be 1.5 mins. To avoid any confusion, if the time intervals are less than a minute, its
best to change the recorded units to seconds. That same stopwatch display would therefore be
recorded as 90 seconds.

Advantages & Disadvantages of Methods & Apparatus

 In the lab we often have choices of different apparatus to do the same job

 Evaluating what is the best one to use is part of good experimental planning and design

 This means appreciating some of the advantages and disadvantages of laboratory apparatus
Table showing examples of Advantages and Disadvantages of Lab Apparatus

Five pieces of apparatus that can be used to measure the volume of a liquid. They all have their pros
and cons
Planning your method

 Good experimental design includes the answers to questions like

o Have I chosen a suitable apparatus for what I need to measure?

o Is it going to give me results in an appropriate time frame?

o Is it going to give me enough results to process, analyse and make conclusions?

o Does it allow for repetitions to check how reliable my results are?

o Does my plan give a suitable range of results?

o How can I be sure my results are accurate?

o Have I chosen an appropriate scale of quantities without being wasteful or unsafe?

 You may be asked about experimental methods in exam questions and your experience and
knowledge of practical techniques in chemistry should help you to spot mistakes and suggest
improvements

Exam Tip

Make sure you know the names of common laboratory apparatus

 Titrations are a method of analysing the concentration of solutions

 They can determine exactly how much alkali is needed to neutralise a quantity of acid – and vice
versa

 You may be asked to calculate the moles present in a given amount,

 Titrations can also be used to prepare salts

Describing how to carry out a titration

 The typical materials needed are:

o 25 cm3 volumetric pipette

o Pipette filler

o 50 cm3 burette

o 250 cm3 conical flask

o Small funnel

o 0.1 mol/dm3 sodium hydroxide solution

o Sulfuric acid – concentration unknown

o A suitable indicator

o Clamp stand, clamp & white tile

Describing the method:

1. Use the pipette and pipette filler and place exactly 25 cm3 sodium hydroxide solution into the
conical flask

2. Place the conical flask on a white tile so the tip of the burette is inside the flask

3. Add a few drops of a suitable indicator to the solution in the conical flask

4. Perform a rough titration by taking the burette reading and running in the solution in 1 – 3
cm3 portions, while swirling the flask vigorously

5. Quickly close the tap when the end-point is reached (sharp colour change) and record the
volume, placing your eye level with the meniscus

6. Now repeat the titration with a fresh batch of sodium hydroxide

7. As the rough end-point volume is approached, add the solution from the burette one drop at a
time until the indicator just changes colour

8. Record the volume to the nearest 0.05 cm3

9. Repeat until you achieve two concordant results (two results that are within 0.1 cm 3 of each
other) to increase accuracy

Indicators

 Indicators are used to show the endpoint in a titration

 Wide range indicators such as litmus are not suitable for titration as they do not give a sharp
enough colour change at the endpoint

 However, methyl orange and phenolphthalein are very suitable

 Some of the most common indicators with their corresponding colours are shown below:

Common Acid-Base Indicators

 This technique is used to separate substances that have different solubilities in a given solvent
(e.g. different coloured inks that have been mixed to make black ink)

 A pencil line is drawn on chromatography paper and spots of the sample are placed on it. Pencil
is used for this as ink would run into the chromatogram along with the samples

 The paper is then lowered into the solvent container, making sure that the pencil line
sits above the level of the solvent so the samples don´t wash into the solvent container

 The solvent travels up the paper by capillary action, taking some of the coloured substances
with it

 Different substances have different solubilities so will travel at different rates, causing the
substances to spread apart. Those substances with higher solubility will travel further than the
others

 This will show the different components of the ink / dye

Analysis of the composition of ink using paper chromatography

Interpret Simple Chromatograms

 If two or more substances are the same, they will produce identical chromatograms

 It is common practice to include a known compound as a reference spot

o This can help match up to an unknown spot or set of spots in order to identify it

 If the substance is a mixture, it will separate on the paper to show all the different components
as separate spots

 An impure substance will show up with more than one spot, a pure substance should only show
up with one spot

Exam Tip

Paper chromatography is the name given to the overall separation technique while a chromatogram is
the name given to the visual output of a chromatography run. This is the piece of chromatography
paper with the visibly separated components after the run has finished.
 Filtration & Crystallisation

 The choice of the method of separation depends on the nature of the substances being
separated

 All methods rely on there being a difference of some sort, usually in a physical property such as
boiling point between the substances being separated

Separating a mixture of solids

 Differences 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 other substances or impurities, e.g. to separate a mixture of sand and
salt, water is a suitable solvent to dissolve the salt, but not the sand

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). Centrifugation can also be used for this mixture

 Filter paper is placed in a filter funnel above another beaker

 The mixture of insoluble solid and liquid is poured into the filter funnel

 Filter paper will only allow small liquid particles to pass through in the filtrate

 Solid particles are too large to pass through the filter paper so will stay behind as a residue

Filtration of a mixture of sand and water

 Used to separate a dissolved solid from a solution, when the solid is more soluble in hot solvent
than in cold (e.g. copper sulphate from a solution of copper (II) sulphate in water)

 The solution is heated, allowing the solvent to evaporate and leaving a saturated solution
behind

 You can test if the solution is saturated by dipping a clean, dry, cold glass rod into the solution

o If the solution is saturated, crystals will form on the glass rod when it is removed and
allowed to cool

 The saturated solution is allowed to cool slowly and solids will come out of the solution as the
solubility decreases, and crystals will grow

 Crystals are collected by filtering the solution

 They are then washed with distilled water to remove any impurities and then allowed to dry

Diagram showing the process of crystallisation

Distillation: Simple & Fractional

Simple Distillation

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

 The solution is heated and pure water evaporates producing a vapour which rises through the
neck of the round-bottomed flask
  The vapour 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

Diagram showing the distillation of a mixture of salt and water

 Simple distillation can be used to separate the products of fermentation, such as alcohol and
water

 However, more effective separation is to use fractional distillation where the liquids are closer
to boiling point and a higher degree of purity is required

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)

 The solution is heated to the temperature of the substance with the lowest boiling point

 This substance will rise and evaporate first, and vapours will pass through a condenser, where
they cool and condense, turning into a liquid that will be collected in a beaker

 All of the substance is evaporated and collected, leaving behind the other components(s) of the
mixture

 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 beaker
  When the temperature starts to increase to 100 ºC heating should be stopped. Water and
ethanol are now separated

Fractional distillation of a mixture of ethanol and water

 An electric heater is safer to use when there are flammable liquids present

 The separation of the components in petroleum is achieved by fractional distillation on an

 Fractional distillation of crude oil is not carried out in school laboratories due to the toxic nature
of some of the components of the crude oil, but it can sometimes be simulated using a synthetic
crude oil made specially for the demonstration
Worked example

A student is given a mixture of calcium sulfate, magnesium chloride and water. The table below shows
some information about calcium sulfate and magnesium chloride.

substance solubility in water state at room temperature

calcium sulfate insoluble solid

magnesium chloride soluble solid

How does the student obtain magnesium chloride crystals from the mixture?

A crystallisation followed by distillation

Answer:

The correct answer is D because:

 The difference in solubility in water means the first step is to make a solution

 The magnesium chloride will dissolve, but the solid calcium sulfate will be left behind

 The mixture is filtered to remove the calcium sulfate and then evaporated and crystallised to
obtain magnesium chloride crystals

Exam Tip

You may be asked how to separate a mixture of gases. One method involves cooling the gaseous
mixture sufficiently to liquefy all of the gases. The liquified mixture is then separated by fractional
distillation. They can also be separated by diffusion, where the boiling points are very close or it is
impractical or expensive to use fractional distillation.

Assessing Purity

 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

 Mixtures have a range of melting and boiling points as they consist of different substances that
melt or boil at different temperatures

 Melting and boiling point data can therefore be used to distinguish pure substances from
mixtures

 An unknown pure substance can be identified by experimentally determining its melting point
and boiling point and comparing them to literature values / data tables

o Boiling points are commonly determined by distillation

 This is done using a melting point apparatus which allows you to slowly heat up a small amount
of the sample, making it easier to observe the exact melting point

Melting point test using an oil bath

 This is then compared to data tables

 The closer the measured value is to the actual melting or boiling point then the purer the
sample is

 If the sample contains impurities:

o The boiling point may appear higher than the sample's actual boiling point

o The melting point may appear lower than the sample's actual boiling point
 Identification of Anions

 The acidification with aqueous silver nitrate and aqueous barium nitrate / chloride is done to
remove ions that might give a false positive result

o The most common ion that is removed is the carbonate ion

o The choice of acid has to be considered so that it does not influence the results

o For example, aqueous silver nitrate solution should not be acidified with hydrochloric
acid as this will form a white precipitate due to the chloride ion in the acid

o For example, aqueous barium nitrate / chloride solution should not be acidified with
sulfuric acid as this will form a white precipitate due to the sulfate ion in the acid

Exam Tip

When it comes to qualitative inorganic analysis, always remember that there will be a test for the
metal cation part of the molecule and another test for the anion part.