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Measurement
Introduction
There are two types of data in chemistry: qualitative and quantitative. Quantitative data is the kind
of data that can be measured. It is important that these measurements are as accurate and precise
as possible, or the data will be corrupted and may lead to false conclusions to an experiment.
Being accurate and precise will lead to having a good experiment.
Precision
To obtain more precise measurements it is necessary to use equipment that has a high
resolution, like having a mass balance with more decimal places or a ruler with smaller divisions.
However, having more precise instruments does not mean that data obtained will be closer to the
true value.
Here are some examples of how to take more precise measurements:
● Always take burette readings to the nearest 0.05 cm3.
● When using a thermometer of 1ºC resolution, always take measurements to the nearest
0.5ºC.
● Use appropriate measuring instruments, for example do not use a meter rule to measure
the width of a pencil.
Accuracy
Accuracy is the closeness of the recorded data to the true value. To be more accurate
measurements should be repeated, so it may be necessary to repeat the same experiment several
times to get good data. A student must make a judgement to estimate how long an experiment will
take them, so that they can plan how many times they will repeat their experiment in the time they
are given. Accuracy of an experiment is affected by different types of errors, which all lead to
inaccuracy of the data. Being able to identify possible errors in the experiment and knowing
methods of correcting them is a key skill as a chemist and will definitely be assessed in the
practical part of your course. For example if you have a gas syringe setup in order to collect gas
from a conical flask, one possible error could be that some gas escapes the flask before the bung
is connected. One way to fix this would be to have one of the reagents inside a sample tube upside
down in the conical flask containing the other reagent. The two reagents can then be mixed by
shaking the flask so that the sample tube falls over.
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How to measure different quantities
Burette readings
A titre will be measured by recording the starting volume followed by the final volume, then using:
Titre = Start volume - End volume
Always measure the volume from the bottom of the meniscus, and measure with the level of the
liquid at eye level. This same technique applies to measuring liquids using a graduated cylinder.
Another thing to note about burette readings is that the reading indicates the volume of liquid
‘missing’ from the burette, not the volume of liquid in the burette itself.
Measuring mass
Solids are usually weighed on a weighing boat using a mass balance, this is to prevent
contamination of the pan on the mass balance and contamination of the solid used. Using this
method, however, consistently does not give an accurate value of the mass of solid you are using
in the experiment. This latter reason is why the ‘weighing-by-difference’ method is used: first
weigh the container with the solid in it, then add the solid to the reaction and reweigh the container,
the difference between these two values would be the mass of solid added.
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Once you have set up the apparatus as shown,
you may mix the reagents in the conical
flask and quickly close the conical flask using
the bung. The gas produced in the reaction will
then collect in the gas syringe or measuring
cylinder.
Measuring pH
A solution’s pH can be measured in two different ways: with a pH probe or using an indicator with
a pH scale. Using a pH probe is quite simple, you simply put the probe in the solution you are
testing, wait for a while until the reading is steady and record the pH shown on the digital display.
To get consistent results with a pH probe, the probe must be washed, then calibrated using buffer
solutions of known pH.
Using pH scales to find pH typically has a greater uncertainty and is less precise, but works when
a pH meter is not available or cannot be used. It is suitable for producing quick qualitative
results. To find pH using a scale, add an indicator to the solution (or add solution to paper
containing the indicator), then compare the colour that is produced to a suitable scale. The scale
for universal indicator is shown below. This method is not very accurate as the colour is subjective
and people often disagree about which value it matches on the scale.
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Phil Holliday, CC BY-SA 4.0
Measuring colour
Although colour is typically thought of as qualitative data, colour is a phenomenon that arises due
to the absorption of light, so it can be measured. The colour of a solution of a transition metal ion
typically gives us a good idea of its concentration. First, create a series of solutions of known
concentration with the transition metal ion. Then measure their absorptions using a suitable setup.
Create a ‘calibration curve’ which is a graph of the change in absorption with the concentration.
This curve can then be used to identify concentrations of transition metal solutions by their
absorptions.
A way to qualitatively measure colour more effectively is to put a white tile under the container you
are measuring the colour in, this technique can be used in titrations to better see the endpoint of a
reaction.
Observation
Qualitative data is the type that is observed. Things like colour changes or the type of chemical
present cannot be described with a number. In an experiment it is important to write down every
change seen, even if it seems insignificant, it may come into play when you make your conclusions
and analysis. It is also important that everything you do is written down: the changes made to the
experiment should be recorded exactly so that observations and measurements can be repeated.
Anomalous data
A chemistry student should be able to recognise anomalous data, any data that does not fit the
current trend is anomalous. If a student is performing a rates of reaction experiment and they
decrease the concentration of a first order reactant by a small amount, we would expect the rate of
reaction to slightly decrease, if instead the rate of reaction recorded shows a large increase the
student should suspect that an error has been made. This data point should be marked as
anomalous.
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CIE Chemistry A-Level
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Presentation of data and observations
Data Tables
Tables of data are the most common form of recording observations in chemistry. This type of data
is referred to as qualitative data. A table should be set up before the experiment starts, and
should have the correct rows so that there is enough space to record all of your observations. A
student must therefore have a good idea of how many observations they will make as well as what
they will be observing. Tables can contain quantitative or qualitative data or both, they help to
organise the data so conclusions can more easily be made. The table below is an example of a
table containing qualitative data.
Using the above table, we can conclude that solution A contains CuSO4, solution B contains MnCl2,
and solution C contains FeI2. Always bring a ruler and pencil to the exam in order to draw these
tables.
Graphs
Introduction
A table is a good way of recording results and observations during the experiment and for
qualitative data it is also a good way of presenting the data. However, for quantitative data, a
graph is generally best used to present the data, as it clearly shows patterns and trends and how
the dependent variable varies with the independent variable.
Drawing graphs
You will not only need to be able to read and interpret graphs given to you in the exam, you may
also be expected to draw a graph from a set of data given. Here are some important tips for
drawing graphs:
● Always use a sharpened pencil and ruler to draw the axis and line of best fit.
● Label the axis with its variable and its units.
● Draw your graph a sensible size.
○ Use up at least half of the graph paper given.
● Use a sensible scale.
● The dependent variable goes on the vertical y axis.
● The independent variable goes on the horizontal x axis.
● Determine the ranges of the axis so you can include all the data points collected.
● Give the graph an appropriate title .
● Indicate any anomalies but identify them as anomalous.
○ Ignore these when drawing your line of best fit.
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● Draw a line of best fit if possible.
○ The ‘line’ could be straight or curved. If the line of best fit is not a straight line, a
freehand continuous curve must be drawn.
○ Never just connect the points like a dot-to-dot.
○ Bring a long, clear ruler to the exam so you can see the data points when drawing a
straight line of best fit.
A helpful way to remember which axis the independent and dependent variables go on is to
imagine the letters ‘I’ and ‘D’ sat on their respective axis as shown:
Shown below is an example graph drawn for the following table of results:
Notice that the units of measurements are only included in the title of each column. Each
measurement of the same type must be given to the same degree of accuracy - e.g. in the table
below, each weight value is given to three significant figures. The graph to represent this data:
Length Weight
(cm) (g)
10 35.0
15 38.5
25 50.0
33 58.0
40 65.0
45 100
58 88.0
59 85.0
70 96.0
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An example conclusion:
The data collected shows that as the length of oak leaves increases, the weight of them also
increases linearly. For instance, a leaf which measured 10 cm weighed only 35.0 g whereas a leaf
which measured 59 cm weighed 85.0 g. The explanation for this is that longer leaves have a larger
surface area and, therefore, a greater mass. If I were to repeat this experiment I would measure
longer leaves to investigate whether the trend remains the same and if it remains linear for lengths
past 80 cm.
Exam questions
As well as drawing graphs you will need to be able to interpret and read graphs given to you in
the exam. Possible skills you could be tested on include:
● Reading data points off a graph
● Drawing an appropriate line of best fit
○ Remember it may not be straight!
● Suggesting the type of graph you would use for a given set of data
○ General rule of thumb - if quantitative use a scatter graph, if qualitative use a bar
chart.
● Identifying patterns and trends
● Drawing conclusions from the graph which must include referencing data points
● Comparing 2 similar graphs
○ For instance, comparing 2 graphs which have the same dependent and independent
variables but a different subject of study (e.g. for the example above, comparing that
graph to another graph which shows the lengths and weights for a different species
of leaf).
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CIE Chemistry A-Level
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Analysis
Intro
It is necessary to perform analysis of the data after an experiment has been completed so that
conclusions may be drawn from the experiment. We must analyse many aspects of the
experiment, not just the obviously conclusive ones. Some important analyses may include
determining the percentage uncertainty in some of our conclusive values, percentage purity of a
solid, atom economy of a reaction and percentage yield. These latter calculations will not get us
our main conclusive value, but will help us to confirm the validity and efficiency of our experiment.
Calculations
Some general calculations you may need to complete to evaluate an experimental procedure:
Example 1:
A 250 cm3 volumetric flask has an error of ±0.10cm3. What is the maximum percentage error of the
volumetric flask?
Example 2:
A burette has a percentage error of ± 0.05 cm3. A titre was calculated to be 28.40 cm3. What is the
total percentage error of this measurement?
For this calculation the 0.05 uncertainty has to be doubled as two measurements are taken when a
burette reading is calculated - the volume at the start and the volume at the end.
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Percentage yield
The expected yield can be determined from the initial masses of the reactants and the overall
equation of the reaction. The actual yield is measured by weighing of the final product produced.
Atom economy
To work out the efficiency at which our reaction produces the desired product of the experiment,
we must calculate the atom economy of the reaction, there may be other routes to produce the
desired product that are more efficient.
Example:
Hydrogen can be produced from methane in the following reaction.
CH4 + H2O → 3H2 + CO
What is the atom economy for the production of hydrogen?
The gradient of a straight line may need to be found in order to determine the constant of a rate
equation, for example the gradient of a concentration-rate graph would give this value.
Percentage purity
It might be the object of an experiment to find the percentage purity of a given impure mixture, like
an iron tablet, this is normally done by titration to find the actual mass of the desired substance
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present in the impure mixture. Finding the purity of reactants can be done on the side of the main
experiment in order to better estimate the expected yield of the main experiment.
Conclusion
An experiment is concluded, at A-Level, by comparing against known observations/values or by
making judgements based on calculated results like percentage purity or the equation of a straight
line. A calculated Rf value of an organic product from a synthesis would be compared to known Rf
values of the expected product to assess if the correct product was made, this would then lead to
the conclusion that the correct product was made, or that it was not.
Significant figures
It is also important that conclusive values are written to the correct number of significant figures.
This is done by looking at the number that you have used in the calculation that has the least
number of significant figures, this is the maximum number of significant figures you may use when
presenting your conclusive value. Use the following calculation as an example:
n = 0.709 mol
p = 101400 pa
T = 278.9 K
V=?
pV=nRT
101400V = 0.709 × 8.314 × 278.9
V = 0.0162 m3
Although most of the values used in the equation are to 4 significant figures, the number of moles,
n, is only to 3 significant figures, we must therefore present our final value to 3 significant figures.
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Evaluation
Now it is time to assess our experiment, we must look at the whole of our experiment and identify
any possible errors that have occurred, this may be to fix a particular issue like a very low
percentage yield when synthesising organic solids. One example of an error is the false positive
that may be obtained in ion tests from testing for sulphate ions first, where chloride ions could
create a white precipitate and falsely indicate the presence of sulphate ions.
To fix a low percentage yield we must also balance how pure we would like our sample to be.
Every time a solid is recrystallised it’s purity increases, but some product is lost. The same is true
for washing an organic liquid with water in a separating funnel. Other factors that could affect the
yield would be that not all of the reactants reacted (incomplete reaction) or some product was lost
when transferring between containers. Often, the yield is increased by using a different method
which may involve changing the chemicals used in the reaction.
We must also identify all numerical errors in the experiment, like the error in each burette or
thermometer reading. This value is normally half of the resolution of the instrument, for example a
thermometer of resolution 1ºC would have an uncertainty of ±0.5ºC, or a burette with a resolution
of 0.1 cm3 would have an uncertainty ±0.05 cm3. The percentage uncertainty of each measurement
could therefore be reduced by increasing the value measured, like using a larger volume in a
titration, or a larger mass in an enthalpy change experiment.
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CIE Chemistry A-Level
Practicals for Papers 3 and 5
Titrations
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Example Method for an acid-base titration
Method Accuracy Explanation
1. Pour approximately ● Use a clean, dry beaker.
100cm3 of the standard
solution of known
concentration into a
beaker.
2. Fill the burette with the ● Rinse the burette before If the jet space is not filled it will
standard solution of using a small volume of the lead to errors if it then fills
known concentration. solution. during the titration, leading to a
● Make sure the jet space in larger than expected titre
the burette is filled and reading.
doesn’t contain air bubbles.
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8. Repeat, calculate and ● You should normally carry
record the volume of out at least three titrations.
solution used in the
titration in a table (titre
volume). Repeat until two
concordant results are
obtained. Record all of
the results that you
obtain.
Conical flask/burette:
● If solution A is titrated against solution B, it means that solution A is in the conical flask and
solution B is in the burette.
● The alkali usually in conical flask.
● lf 2 or 3 values are within 0.10cm3 and are therefore concordant, then the results are
accurate and reproducible and the titration technique is good or consistent.
● Results should be clearly recorded in a table.
● Rows on the table should be: initial burette reading, final burette reading and titre, all in cm3.
● Columns on the table should be the different trials labelled numerically.
● Tick the two concordant titres.
● Record titre volumes to 2dp (0.05 cm3).
● Only make an average titre volume using the concordant titre results.
Safety precautions:
● Acids and alkalis are corrosive (at low concentrations acids are irritants).
● Wear eye protection and gloves.
● If spilled immediately wash affected parts after spillage.
● If a substance is unknown, treat it as potentially toxic and wear gloves.
Titrating mixtures:
Testing batches:
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● In quality control it will be necessary to do titrations or testing on several samples as the
concentration and amount of the chemical being tested may vary between samples.
Uncertainties:
● Replacing measuring cylinders with pipettes or burettes which have lower apparatus
uncertainty will lower the overall error.
● To reduce the uncertainty in a burette reading the titre volume needs to be made larger.
This could be done by: increasing the volume and concentration of the substance in the
conical flask or by decreasing the concentration of the substance in the burette.
● Leaving NaOH in the burette will cause damage to the apparatus which could lead to
errors.
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CIE Chemistry A-Level
Practicals for Papers 3 and 5
Enthalpy Change & Measuring Temperature
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Measuring Temperature
Enthalpy Change
Before the practical begins, use the method for measuring mass, to calculate a mass of solid
used. Then calculate the moles from (n = Mr X m). The energy change is from Q=mc ΔT) where: Q
is energy in J (divide by 1000 to convert to kJ), m is mass of water in grams, c is specific heat
capacity (4.186 for water) and ΔT is temperature change (from graph). To work out enthalpy
change divides the energy (kJ) by moles. If exothermic add a minus, if endothermic add a plus.
Standard units are kJ mol-1.
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Method (example: enthalpy change of hydration of CuSO4)
Method Accuracy Explanation
1. Weigh out between 3.90-4.10 g of ● Wash the containers
anhydrous copper (II) sulfate in a dry, with the solution to be
stoppered weighing bottle. Keep the used.
stock of solid in a closed container ● Dry the cup after
during weighing. The precise mass washing.
should be recorded.
2. Construct a suitable table of results to
allow you to record temperatures at
minute intervals up to 15 minutes.
3. Using a measuring cylinder, place 25 ● Allow the water to stand This ensures they all
cm3 of deionised (or distilled) water into for some time. reach room
a polystyrene cup and record its initial ● Stir the liquid temperature, allowing
temperature (t=0). Start the timer and continuously. a better average
then continue to record the ● Place the polystyrene temperature to be
temperature each minute, for three cup in a beaker for extra obtained.
minutes. insulation and support. Polystyrene beakers
● Clamp thermometer into make good
place ensuring that the calorimeters because
bulb is immersed in they are good
liquid. (see diagram) insulators and have
● If the two reactants are high specific heat
solutions then the capacities.
temperature of both
solutions need to be
measured before
addition and an average
temperature is used.
4. At the fourth minute, add the powdered ● Add the powdered
anhydrous copper (II) sulfate to the anhydrous copper (II)
water in the polystyrene cup and but sulfate rapidly.
do not record the temperature. At the ● Using a lid on the
fifth minute continue the temperature polystyrene cup can
readings at minute intervals, up to help to minimise heat
fifteen minutes. Stir the solution in the loss and maximise
polystyrene cup as this is done. change in temperature.
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CIE Chemistry A-Level
Practicals for Papers 3 and 5
Gases Evolved
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Qualitative test for a gas
Take these data into account when testing gases. For example, less dense gases will rise so must
be sealed in a bun upside down or they’re lost and denser gases will sink. Also gases like
ammonia are unlikely to be evolved from a liquid under standard conditions because it’s very
soluble.
A lit wooden splint makes a squeaky popping sound in a test tube of hydrogen.
To test the effervescence for carbon dioxide, pass the gas through calcium hydroxide solution
(limewater). Carbon dioxide turns limewater cloudy white as solid calcium carbonate precipitates.
Ammonia has a characteristic strong, choking smell. It also makes damp red litmus paper turn
blue. Ammonia forms a white smoke of ammonium chloride when hydrogen chloride gas, from
concentrated hydrochloric acid, is held near it.
Experimental advice:
● Ensure the litmus paper is damp and not dry, by adding a bit of distilled water to it.
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● Don’t let the litmus paper touch the test tube as alkali on the sides may cause the colour
change to blue, which is a false positive for ammonia gas.
● Keep litmus paper 1cm away from test tube
● State that red litmus paper is being used not just litmus, as blue litmus paper also exists.
Chlorine has a characteristic strong, choking smell. It also makes damp blue litmus paper turn
red, and then bleaches it white. Chlorine makes damp starch-iodide paper turn blue-black.
A qualitative test is the smell of rotten eggs. Other tests include paper dipped in potassium
dichromate will go from orange to green and damp blue litmus paper will turn red.
NO2
If you place a bung on a reaction of acid and nitrate ions test tube, a build-up of NO2 will cause the
sides of the test tube to go a pale brown. When the bung is released, a visible (on a white
background) pale brown gas is released.
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CIE Chemistry A-Level
Practicals for Papers 3 and 5
Evaporation & Crystallisation
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What is evaporation and crystallisation?
It is simply heating a hydrous salt and until all the water evaporates and then calculating the mass
of water that has evaporated.
Experiment Advice:
● Heat using an electric heater gently. This is to ensure that the crystals do not decompose
under heating. (You can use Bunsen burner but adjust heating to ensure boiling isn’t too
vigorous.). For example, compounds such as nitrates will decompose on heating to for a
pale brown gas of nitrogen dioxide. Gentle heating ensures the percentage yield remains
high.
● Heat and weigh mass of solid crystals at intervals. When the weighed mass becomes
constant you can finish. Mass becomes constant because all the water has evaporated.
● Use before and after weighing method - see measuring mass document.
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