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 cm 3

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 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

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 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

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 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

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  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

Solutions
 You need to know all the following terms used when describing solutions:

Terminology About Solutions Table

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Acid-Base Titrations
 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,
the concentration or volume required to neutralise an acid or a base
 Titrations can also be used to prepare salts

Describing how to carry out a titration

 The typical materials needed are:

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 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

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Topics: Experimental Techniques Short Notes for Quick Revision Compiled by Mr. Faisal Mehmood Janjowa 8
 The steps in performing a titration

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

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

Common Acid-Base Indicators

Paper Chromatography
 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

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Topics: Experimental Techniques Short Notes for Quick Revision Compiled by Mr. Faisal Mehmood Janjowa 11
 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.

Locating Agents
 For chromatography to be useful the chemist needs to be able to see the components move up the
paper, which is not the case for colourless substances such as amino acids or sugars
 Locating agents are substances which react with the sample and produce a coloured product which
is then visible
 The chromatogram is treated with the agent after the chromatography run has been carried out,
making the sample runs visible to the naked eye

Retention Factor (Rf) Values

 These values are used to identify the components of mixtures
 The Rf value of a particular compound is always the same
 Calculating the Rf value allows chemists to identify unknown substances because it can be compared
with Rf values of known substances under the same conditions

Calculation

 The formula to calculate the retention factor is:

The Rf value is a ratio and therefore has no units

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 Using Rf values to identify components of a mixture

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

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 Filtration of a mixture of sand and water

Crystallisation

 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

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 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

 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

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 Diagram showing the distillation of a mixture of salt and water

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

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 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 industrial
scale
 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?

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A crystallisation followed by distillation
B crystallisation followed by filtration
C distillation followed by crystallisation
D filtration followed by crystallisation

Answer

The correct answer is D because:


o The difference in solubility in water means the first step is to make a solution
o The magnesium chloride will dissolve, but the solid calcium sulfate will be left behind
o 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
 Melting point analysis is routinely used to assess the purity of drugs for example
 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

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 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

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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.

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If you are an extended level student you may be asked to write balanced ionic equations for cation and
anions tests, so make sure you know the formulae of all the ions and precipitates formed.

Identification of Cations
 Metal cations in aqueous solution can be identified by the colour of the precipitate they form on
addition of sodium hydroxide and ammonia
 If only a small amount of NaOH is used then normally the resulting metal hydroxide precipitates out
of solution
 In excess NaOH some of the precipitates may re-dissolve
 A few drops of NaOH is added at first and any colour changes or precipitates formed are noted
 Then the NaOH is added in excess and the reaction is observed again
 The steps are then repeated for the test using ammonia solution

Analysing results

 The table below contains the results for each of the cations included in the syllabus
 If a precipitate is formed from either NaOH or aqueous ammonia then it means that the hydroxide is
insoluble in water
 Zinc chloride, for example, reacts as such:

ZnCl2 (aq) + 2NaOH (aq) → Zn(OH)2 (s) + 2NaCl (aq)

 Ca2+ ions can be distinguished from Zn2+ and Al3+ as calcium hydroxide precipitate does not dissolve in
excess NaOH but both zinc hydroxide and aluminium hydroxide do
 Zn2+ ions can be distinguished from Al3+ ions as Zn(OH)2 dissolves in excess aqueous ammonia but
Al(OH)3 does not
 Most transition metals produce hydroxides with distinctive colours

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Exam Tip
The ammonia or sodium hydroxide solution must be added very slowly. If it is added too quickly and the
precipitate is soluble in excess, then you run the risk of missing the formation of the initial precipitate, which
dissolves as quickly as it forms if excess solution is added.

Be sure to distinguish between the term “colourless” and “clear”. A solution that loses its colour has become
colourless. A clear solution is one that you can see through such as water. Solutions can be clear and have
colour eg. dilute copper sulphate.

 The flame test is used to identify the metal cations by the colour of the flame they produce
o Ions from different metals produce different colours
 Dip the loop of an unreactive metal wire such as nichrome or platinum in concentrated acid and then
hold it in the blue flame of a Bunsen burner until there is no colour change
o This is an important step as the test will only work if there is just one type of ion present
 Two or more ions means the colours will mix, making identification erroneous

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  This cleans the wire loop and avoids contamination
 A small sample of the compound is placed on an unreactive metal wire loop such as nichrome or
platinum
 Dip the loop into the solid sample / solution and place it in the edge of the blue Bunsen flame
o Avoid letting the wire get so hot that it glows red otherwise this can be confused with a flame
colour

Diagram showing the technique for carrying out a flame test

 The colour of the flame is observed and used to identify the metal ion present:

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 Diagram showing the colours formed in the flame test for metal ions

Exam Tip
The sample needs to be heated strongly, so the Bunsen burner flame should be on a blue flame.

Identification of Gases
 Several tests for anions and cations produce gases which then need to be tested
 The table below indicates the tests for the gases included in the syllabus

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Exam Tip
It is easy to confuse the tests for hydrogen and oxygen. Try to remember that a ligHted splint has
a H for Hydrogen, while a glOwing splint has an O for Oxygen.

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