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Guidance on the internal assessment

Design

For example, a suitable research


question could be: How will
changing the concentration of
X affect the value of Y in the
reaction...? Where a particular
chemical reaction is being studied,
you should give an equation for
that reaction, e.g.: In the reaction
A(s) + B(aq) C(aq) + D(g), how
does changing the concentration
of B affect the rate at which D is
produced?

This involves formulating a research question that you will investigate.


As part of this criterion you must also identify the variables in the
experiment.

Aspect 1

Define your research question. This must be clearly stated and not
vague.
List all possible variables. Decide which are the key variables, i.e.
the ones that are most important in determining the outcome of
the experiment. Decide which variable is to be investigated. Which
variables are to be controlled?
You should classify your variables as independent, dependent
and controlled.

For instance, Table 1 shows the independent, dependent and controlled


variables if you are investigating the effect of changing the concentration
of hydrochloric acid on the rate at which hydrogen is given off in the
following reaction:

A variable is any factor that


could affect the outcome of the
experiment.

Mg + 2HCl MgCl2 + H2
Independent variable concentration of HCl

the variable that you change in order to see what


effect it has

Dependent variable

volume of hydrogen given off in a certain time

what you measure

Controlled variables

temperature, surface area of magnesium, volume


of acid, atmospheric pressure

the things you keep the same

Table 1 The independent, dependent and controlled variables in an experiment to investigate the effect of changing the concentration
of hydrochloric acid on the rate of hydrogen production.

It is also worth mentioning here that you must keep all apparatus and
the procedure constant between different runs of the same experiment.

Aspect 2

List the apparatus to be used. The list of apparatus should include


absolutely everything that you will need in order to carry out the
experiment. For example, will you use a measuring cylinder or a
pipette to measure out 25 cm3 of a solution? If you use a measuring
cylinder, what size will you take? Dont forget the electronic balance!
List all the chemicals that you will require.You should state masses of
solids that you will use and concentrations and volumes of solutions
required.
You should give a step-by-step method detailing how you will
carry out the experiment.Your method should be such that someone
reading it could recreate your experiment exactly. For example, in an

CHEMISTRY FOR THE IB DIPLOMA CAMBRIDGE UNIVERSITY PRESS 2011

A diagram is required only if it


helps to explain how the apparatus
is set up. There is no point in
drawing a diagram in, for example,
a titration experiment. Any
diagram should be clearly labelled.
You do not have to do this all
theoretically, as you can use
preliminary experiments to
work out suitable amounts/
concentrations.

GUIDANCE ON THE INTERNAL ASSESSMENT

Example of apparatus list for the


reaction between Mg and HCl:
boiling tubes (2)
gas burette (50 cm3)
measuring cylinder (10 cm3)
measuring cylinder (100 cm3)
delivery tube and bung
plastic trough (2)
electronic balance
stopwatch
magnesium ribbon (approx.
0.5 g)
hydrochloric acid (1 mol dm3)
(approx. 500 cm3)
distilled water (approx. 500 cm3)
tap water

Your method should contain an


explanation of how you are going
to control the variables that
you need to control and how you
will vary the others. For example,
the temperature is controlled
by placing the boiling tube in a
trough of water; the volume is
controlled by always using 10 cm3
of hydrochloric acid; the surface
area of the magnesium is controlled
by always using one single strip of
magnesium, etc.

investigation of the effect of concentration on the reaction between


magnesium and hydrochloric acid:

I will set up the apparatus as in the diagram

I will fill the gas burette to the top with tap water

I will place the boiling tube in the water in the plastic trough
(control of variables temperature) and measure the temperature of
the water

I will weigh out accurately 0.06 g of magnesium ribbon on the


electronic balance

I will put the magnesium ribbon into the boiling tube

I will use the following concentrations of hydrochloric acid:


0.20 mol dm3, 0.40 mol dm3, 0.60 mol dm3, 0.80 mol dm3,
1.0 mol dm3

I will make up the various concentration of HCl as follows:


0.80 mol dm3 could be prepared by putting 80 cm3 of the acid into
a 100 cm3 measuring cylinder and making it up to the 100 cm3 mark
by adding distilled water, whereas 0.60 mol dm3 would require
60 cm3 of the acid and 40 cm3 of water

I will measure out 10 cm3 of 1 mol dm3 acid using the 10 cm3
measuring cylinder and measure the temperature of the acid

I will pour the acid as quickly as possible into the boiling tube, place
the bung on the tube and start the stopwatch (these three actions
should be done as close to simultaneously as possible)

I will record the level of water in the gas burette every 15 s until
the gas burette is filled with gas or there appears to be no further
reaction

I will repeat the experiment with the same concentration of


hydrochloric acid and mass of magnesium; in order to make the
repeated experiment as close to the original as possible the boiling
tube must be washed out thoroughly and dried and the water in the
trough into which the boiling tube is placed should be replaced in
case the temperature has changed

I will then carry out the experiment using the other concentrations
of hydrochloric acid

I will repeat all experiments until consistent results are obtained


If you have some variables that are going to prove very difficult to
control (e.g. atmospheric pressure), then you should not simply ignore
them and, wherever possible, you should at least monitor these variables
to determine to what extent they do remain constant
If you use a method that is adapted from another source, you must
reference the original source; however, you must change this method in
some way, as the whole point of this section is not that you simply use
a method from a book or the internet but that you design a method
yourself.

Aspect 3
You should plan to collect sufficient relevant data. For instance, if you are
investigating the trend in a particular continuous variable, with the aim of
plotting a line graph, you should plan to change your independent variable
at least five times this will give you sufficient points to plot a graph.
If you are investigating a discrete variable (e.g. how the different
isomers of C3H8O affect their enthalpy change of combustion), you will
2

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CHEMISTRY FOR THE IB DIPLOMA CAMBRIDGE UNIVERSITY PRESS 2011

not be required to change the variable five times (there are only three
possible isomers!), but you should change the variable as many times as
possible.You would not use this data to plot a line graph a bar chart
would be more appropriate.
You should plan to use as large a range of the independent variable as
possible. For example, if you are investigating the effect of temperature on
the rate of a particular reaction, investigating five temperatures between
20 C and 30 C is unlikely to produce experimental data that will give a
true picture of the effect of this variable.You should carry out preliminary
work to determine the maximum and minimum values for the range that
you can investigate. For example, you could try your rates experiment at
90 C and find that the reaction is over in less than 3 s, so this temperature
is impractical. The reaction at 80 C, however, takes about 10 s, and the rate
can be measured reasonably precisely at this temperature. The maximum
temperature you will investigate will therefore be 80 C. In the same
way you should investigate the minimum temperature that you can use.
You should explain in your experimental report how you have used
preliminary work to determine the values of the independent variable that
you will investigate.
In most experiments you should plan to take repeat readings of a
particular property. This will allow you to take an average (mean), which
should improve the reliability of your data.You should generally plan to
take repeat readings until consistent results are obtained.
A trial run of an experiment is often a good idea, as this will give
you an idea as to whether the quantities you are using give sensible and
reliable results.

Data collection and processing


Aspect 1: data collection
Recording data.You must record all raw data that you measure. Best
practice is to record data neatly as you go along and not to scribble data
onto a piece of paper and then try and make sense of it later when you
come to write up the experiment.

Raw data are measurements that


you actually make.

Raw data
It is important that you do actually record raw data. For example, when
carrying out an experiment that involves a rise or fall in temperature,
the initial and final temperatures must be recorded not the
temperature change, as temperature change is a derived quantity worked
out from the initial and final temperatures.

Recording data

Record all data in a neat table so that it is easy for anyone looking
at it to understand them. Make sure that you have written accurate
and complete headings in the table and, if necessary, write sufficient
explanation to make it clear exactly what the table is showing.
All quantitative data must be accompanied by a unit where appropriate.
All data must be recorded to the degree of precision appropriate to
the apparatus, e.g. a mass recorded on a two decimal place electronic
balance must be recorded as 23.00 g and not 23 g.

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GUIDANCE ON THE INTERNAL ASSESSMENT

All data recorded with the same piece of apparatus must be recorded to
the same degree of precision.
All quantitative data must be accompanied by an uncertainty.You
should estimate the degree of precision to which your measuring
apparatus can measure.

Uncertainties
Uncertainties are discussed in
more detail in Chapter 11 of the
Coursebook.

If you think that the uncertainty in


a particular quantity is negligible,
so that it can be ignored, you must
state this.

The concentration of HCl is stated


without an uncertainty, as this was
supplied and the uncertainty is
unknown.

The number of decimal places


recorded for the initial data
corresponds to the uncertainty.
So, 25.0 0.1 and 0.12 0.01 are
correct, but e.g. 25 0.1, 0.12 0.1
and 0.12 0.10 would all be
incorrect.

In general, the uncertainty of a measurement made on a digital instrument


should be quoted as the smallest division. Therefore, a reading on an
electronic balance measuring to two decimal places should be quoted as
23.00 0.01 g.
As a general rule of thumb, for analogue instruments, the uncertainty
on a measurement is half the smallest division to which you take a
reading. This may be the division on the piece of apparatus used, or it
may be an estimate if the divisions are sufficiently far apart to be able to
estimate between them.
For a ruler measuring in mm, a value could be recorded as
23.0 0.5 mm. For a ruler on which the smallest division is 1 cm, you can
usually estimate a value for a length more accurately than to the nearest
cm. If you think that you can estimate a value to the nearest 0.2 cm, i.e.
values of 23.0, 23.2, 23.4 cm, etc. could be recorded, then you should take
the uncertainty as half the division to which you are measuring, in this
case 0.2 cm, and the values can be recorded as 23.2 0.1 cm.
In some cases, for example when using a stopwatch, you may need to
estimate an uncertainty due to reaction times.
An example of the recording of quantitative data for an experiment to
measure the rate of reaction between magnesium and hydrochloric acid
could be:
Initial data
mass of magnesium ribbon / g

0.12 0.01
3

volume of hydrochloric acid / cm


concentration of HCl / mol dm

25.0 0.1
0.20

initial temperature of HCl / C

18.0 0.5

nal temperature of HCl / C

20.0 0.5
Reading on gas burette 0.1 / cm3

Time 0.2 / s
0.0

0.0

30.0

10.5

60.0

18.3

90.0

25.6

etc.

Using a burette
It is usual to read a burette to two decimal places, with the second decimal
place being estimated as 0 (on, or very close to the line) or 5 (between the
lines).

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Initial reading / cm
3

Final reading / cm
3

Titre / cm

Trial

Run 2

Run 3

0.00 0.03

10.05 0.03

5.20 0.03

23.30 0.03

33.15 0.03

28.25 0.03

23.30 0.06

23.10 0.06

23.05 0.06

Initial and final readings on the


burette must be recorded (these
are the raw data), as the titre is
a derived quantity, obtained by
calculation from the raw data.

Note: all readings have been recorded to the same degree of


precision, i.e. same number of decimal places.

Note: you are reading the burette


to the nearest 0.05 cm3, and so
your uncertainty is half of this, i.e.
0.03 cm3 (rounded up).

The uncertainty on the titre is 0.06, as this is the sum of the


uncertainties on the initial and final readings when adding or
subtracting quantities, the uncertainties must be added together.

Data logging
If you are using data-logging equipment, you must state the sensitivity
of the instrument and make sure that the precision of your data does not
exceed the sensitivity of the instrument used. For example, if you are using
a pH probe with a sensitivity of 0.02, you cannot quote a pH of 2.378.

Qualitative data
As part of this criterion, you should also record qualitative data, in
the form of observations, in each experiment. For example, in the
experiment to determine the effect of the concentration of HCl(aq) on
the rate of reaction with magnesium, observations could include:
the magnesium was pale grey
the hydrochloric acid was a colourless solution
the reaction mixture fizzed, with the evolution of a colourless gas
the magnesium dissolved
the rate of effervescence and the speed with which the magnesium
dissolved increased as the concentration of the hydrochloric acid
increased
the final mixture was a colourless solution
the reaction mixture became hotter
it was difficult to take readings at higher concentrations, because the gas
was being produced so quickly.
Of these, the most important observations are the last two, as these are
critical to the experiment and probably a source of error. These should be
referred to in the evaluation section.
Even in a titration experiment, you will be expected to record
observations, and these could include the observed colour change and the
intensity of the indicator colour in each run:
Run 1

When using measuring


instruments such as a pH meter
or a colorimeter, you could make
observations such as:
the reading on the pH meter
was not stable
the needle on the colorimeter
took a long time to reach the
final value.

Run 2

Run 3

10.05 0.03

5.20 0.03

23.30 0.03

33.15 0.03

28.25 0.03

Titre / cm

23.30 0.06

23.10 0.06

23.05 0.06

Observations

rough titration; colour change of indicator from


colourless to pink; nal colour was bright pink

nal solution pale pink very pale pink; one drop


caused colour change

Initial reading / cm3 0.00 0.03


3

Final reading / cm
3

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GUIDANCE ON THE INTERNAL ASSESSMENT

When the experiment involves solely qualitative data, it is essential that


all observations are as detailed as possible. The initial colour and physical
state of the starting material should be recorded. For example, consider
the addition of ammonia solution to copper sulfate solution:
Initial appearance of
substances

Observations made during the reaction

Final appearance
of substances

copper sulfate was a royal


blue solution; the ammonia
solution was colourless with
a pungent odour

upon addition of a few drops of ammonia, a pale blue gelatinous


precipitate was formed, which oated upon the blue solution; as the
mixture was shaken, the precipitate was distributed throughout the
mixture; addition of excess ammonia caused the precipitate to dissolve to
give a dark blue solution

dark blue solution

Aspect 2: data processing

You should set out your calculation


clearly, showing all the steps.

Data processing involves the processing of raw data into a form from
which conclusions can be drawn:
if repeat readings are made, these should be averaged
calculations, using the averaged value, should be carried out to work
out the required quantity
processing will often involve drawing a graph and a line of best fit (see
below)
wherever possible, the gradient (with units) of the graph should be
calculated.

Aspect 3: data presentation


A graph must have a title.

Axes must be correctly labelled.

It is important to consider whether


the graph should go through the
origin or not.
When a straight-line graph is
drawn, it is usual to work out the
gradient (with units) of the line of
best fit.

When two values containing an


uncertainty are added or subtracted,
the absolute uncertainties are
added, so the uncertainty in the
temperature difference is the sum
of the uncertainties for the original
readings, i.e. 0.2 + 0.2 = 0.4.

GUIDANCE ON THE INTERNAL ASSESSMENT

Drawing graphs
Data should be presented in a way that allows for easy interpretation. This
means that, wherever possible, a graph should be drawn.
One way of labelling axes on a graph is:
volume
of gas / cm3

pressure / 104 N m2.


The second form allows you to plot values such as 2.0 104 N m2 as 2.0.
The points on the graph should not be joined up, but instead a line of
best fit (either a straight line or a curve) should be drawn.
When you are plotting continuous data e.g. volume of gas produced
against time, then you should plot a line graph (scatter graph) and
draw a line of best fit. If you are plotting discrete data, e.g. enthalpy of
combustion values for a series of alcohols, a bar chart is more appropriate.

Error analysis
The examples below illustrate the level of error analysis that must be
carried out. Consider a calorimetry (measuring heat changes) experiment:
Initial temperature / C

21.5 0.2

Initial mass / g

23.57 0.01

Final temperature / C

24.2 0.2

Final mass / g

23.23 0.01

Temperature difference / C 2.7 0.4

Mass difference / g 0.34 0.02

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A percentage error can then be worked out for each quantity.


The percentage error in the temperature difference is given by:
uncertainty

0.4
100 = 14.8%
2.7

measured quantity
The percentage uncertainty in the mass difference is:

These are random uncertainties


due to the limitations of reading
the measuring apparatus.
When quantities containing
uncertainties are multiplied
or divided, the percentage
uncertainties must be added.

0.02
100 = 5.9%
0.34
If the calculation to work out the final quantity involves, among other
things, dividing the temperature change by a mass change, then we must
add the percentage uncertainties in each of these quantities to get the
final, overall, percentage uncertainty.
The total percentage uncertainty is 14.8 + 5.9 = 20.7%, i.e. 21%.
If the final value for the enthalpy change comes out as
35.137 45 kJ mol1, we must use the overall percentage uncertainty to
work out to how many significant figures the final value should be
quoted.

The number of significant figures in


the final answer is usually the same
as that of the piece of raw data with
the fewest significant figures.

The absolute uncertainty in the final value can then be worked out:
% uncertainty
absolute uncertainty

21
35.137 45 = 7.4, i.e. 7 (quote final uncertainty to one
100
significant figure)

final value
Thus we have: 35.137 45 7. The final value can, therefore be
quoted as 35 7 kJ mol1.

Quoting values to the correct number of signicant gures


If the result of your calculation gave you a value of 157.4 kJ mol1, then
with a percentage uncertainty of 21% the absolute uncertainty becomes:
21
157.4 = 33, i.e. 30
100
You should quote your final answer as 160 30 kJ mol1.
The significance of the percentage uncertainty will be considered
further in the section on evaluation.

Mean (average) values


There are various more or less complicated ways of quoting the
uncertainty in a mean (average) value. For practical work, it is usually
sufficient to quote the uncertainty of the mean as being the same as that

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Figures are not usually quoted


beyond the uncertainty position.

The absolute uncertainty should


be quoted to one significant figure,
and no figures in your final answer
should be quoted beyond the
uncertainty see Chapter 11,
page 507 of the Coursebook.

The uncertainty is in the second


significant figure (tens) of your
value, and no figures should be
quoted after this.

GUIDANCE ON THE INTERNAL ASSESSMENT

of the original quantity. Thus, if we need to find the mean of 21.0 0.2,
21.3 0.2, 21.5 0.2, we can take it as 21.3 0.2.

Conclusion and evaluation


In this section you must draw and explain conclusions and evaluate the
experiment.

Aspect 1
Your conclusion should be
quantitative where possible.

You should quote a full reference


for the literature value.

You must use the results you have obtained to draw some sort of
conclusion. Where you have designed the experiment, your conclusion
should, of course, relate back to the research question. It is important that
the conclusion is based on your results and not on what you think the
results should have been. For instance, you cannot draw a straight-line
graph that does not pass through the origin then draw the conclusion that
a proportional relationship exists, if that is not what your data are showing.
You must explain how your processed data have led you to a particular
conclusion. For example: Owing to the fact that the graph of reaction
rate against concentration is a straight line passing through the origin, it
can be concluded that in the reaction between Mg and HCl a directly
proportional relationship exists between the concentration of HCl and the
rate of reaction.
The values you have worked out should be compared with literature
values and, where possible, a percentage error calculated.
% error =

literature value experimental value


100
literature value

For instance, if you have worked out a value of 35.7 kJ mol1 for a
particular quantity, and the accepted literature value is 39.5 kJ mol1, the
percentage error is:
% error =

39.5 35.7
100 = 9.6%
39.5

This value should be compared with the total percentage random


uncertainty in your experiment.
If the percentage error, when compared with the literature value, is
smaller than that due to random uncertainties, you can be fairly confident
that the experiment has worked well as a way of obtaining a value for this
particular quantity. If the random uncertainties are, however, quite large,
the experiment can be further refined by using more precise measuring
apparatus and/or taking more repeat measurements.You should comment
on this.
If your percentage error is larger than the percentage uncertainty due to
random uncertainties, then this suggests that there are systematic errors in
your experimental procedure, and these must be eliminated as far as possible
to obtain a more accurate value for the measured quantity. In the case of
systematic errors, redesign of the experiment must be considered. Systematic
errors will have resulted in your value being either larger or smaller than the
accepted value explain which.You must comment on this.

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If you have worked out a trend for which there is no literature value,
you should consider how any conclusion you draw would fit in with
accepted theory. For instance, if you are doing a rates experiment and
accepted theory would have predicted a graph that passed through the
origin, whereas you have obtained a good straight line that does not pass
through the origin, you could explain this as probably due to systematic
errors in the experiment.
If you have drawn a line of best fit you should comment on whether all
your points lie on or very close to the line, as an indication of the quality
of your data.

Aspect 2
The limitations of the procedure must be considered.

Systematic error
Possible sources of systematic error in an experiment could include:
heat loss to the surroundings
solutions not being exactly the stated concentrations
poor technique (there are many aspects to this, such as not stopping a
stopclock at the correct moment, contamination of apparatus, etc.).
You should consider each factor and in which direction it will cause an
error for example, will heat loss to the surroundings cause your final
value to be too small or too large? You must be careful here, because if
your final value for an enthalpy change experiment was more exothermic
than the literature value, you cannot explain the difference in terms of
heat loss to the surroundings, as this would cause the value to be less
exothermic.
You should then consider the relative size of these flaws in your
procedure is one factor a lot more significant than the others? This
should be identified as the major source of systematic error.

You should analyse the apparatus


you used and the techniques
involved in order to identify as
many sources of error as possible.

Random error
You should consider the nature of random errors in your experiment
as shown by percentage uncertainties that have already been calculated.
Is one source of random uncertainty much larger than the others? For
instance, if you are measuring a temperature difference with a random
uncertainty of 5% and a mass with an electronic balance with a random
uncertainty of 0.1%, then the precision of the experiment can be
much more significantly improved by using a more precise thermometer
compared with using a more precise balance.

Questions to consider
For instance, when calculating an enthalpy change involving a solution,
did you assume that the specific heat capacity of the solution was the same
as that of water?
You should consider whether the variables that were identified as
controlled variables were actually controlled. For instance, you may have
stated that temperature was a controlled variable in a rates experiment, but
was this actively controlled or did you just rely on the temperature not
changing very much?
Was the range of value you used for your independent variable too
small for you to be certain about a conclusion for instance, if you were
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Note: only random errors, and not


systematic errors, can be reduced
by taking more repeat readings.

You should consider whether


any approximations used in the
calculations could affect your
overall result.

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investigating the effect of concentration on rate and only changed the


concentration from 1.0 to 1.5 mol dm3?

Aspect 3
Suggest improvements to the experiment to eliminate as far as possible
the flaws you have identified.You should consider improvements to
reduce both random and systematic errors.

Reducing/eliminating systematic errors


Start with the most significant error and suggest improvements, which
should be as specific as possible, e.g. use a beaker made of expanded
polystyrene (styrofoam) is better than stop heat loss to the surroundings.
Your improvements should be realistic and possible to carry out in a
school laboratory.
Consider how controlled variables may be more actively controlled. For
instance, do you need to do a rates experiment in a water bath or insulate
the reaction vessel better?

Reducing random errors

Remember, be specific!

10

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It is important to realise that random errors can never be completely


eliminated, only reduced. This can be done by taking more repeat
readings or using more precise apparatus.You must, again, be
specific about the more precise apparatus and must, for example, suggest
the use of a burette instead of a measuring cylinder to measure the
volumes of liquids, rather than just saying, use more precise apparatus.
Finally, you could suggest what further measurements might need to
be taken to improve your data. For instance, if the range of values was
too small, what other readings should be taken? Again, be specific. For
example, the following concentrations should also be investigated to
provide a better range of results from which a more reliable conclusion
may be drawn.

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