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WIS Chemistry

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WELL DONE – YOU’VE CHOSEN
CHEMISTRY AS AN IB SUBJECT!
Now that you have shown extremely good taste in
selecting Chemistry for the next two years, there is an
introductory phase to the course that you will have to
go through. A sort of Boot Camp, if you will.

Please remember – material that was covered in the Chemistry part of your IGCSE
course is ASSUMED to be understood already. Important concepts that should
have remained in your cranium through the long summer months include:

• Basic periodic table arrangement


• Calculation of formula masses
• Calculation of moles based on masses of solids
• Writing and balancing chemical equations
• Calculation of the concentrations of solutions
• Expressing answers in standard form (from Mathematics)
• Significant figures (from Mathematics)

All of these will be reviewed during the course, but only


very briefly. It’s up to you to ensure that you feel
confident with all of the above i.e. through the novel
concept of SELF STUDY (get used to it – not just in
Chemistry but all your IB subjects).

A basic outline for the first 10 lessons of your


Chemistry course (SL or HL) is as follows:

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Lessons 1 & 2:

Practical X - An investigation into acid/base reactions and


indicators.

This will serve as an introduction to one of the most important techniques –


titrations - used in Years 12 and 13 which will help you to prepare for the practical
assessments you will face. This will also give your teacher an opportunity to assess
your current level of confidence and ability when doing experiments (don’t worry, it
doesn’t count for anything – yet). -

Lessons 3 & 4

Theory – Measurements and Uncertainties

This is actually one of the topics included in the IB course (topic 11). It is covered
at this early stage as understanding of error analysis, accuracy, precision etc. is
essential to perform any experiment at IB level to an acceptable standard.

Lessons 5 & 6

Practical Y – Identifying the formula of a compound

This activity allows you to find the formula of a compound from your own
experimental data – a technique that you may recall from year 10. It also prompts
you to think about the errors in your measurements and the concepts of precision
and accuracy. This experiment will really test your practical skills as a high
standard of accuracy is required during the heating process.

Lessons 7 & 8

Theory – Criteria used for internal assessment of experimental


work

Internal assessment of your experimental work will make up 24% (that’s almost one
quarter for those a bit slow on the uptake) of your final IB level. It is vital that you
understand how your work will be assessed in order for you to gain as high a mark
as possible. You will need your copy of the Chemistry Guide for these lessons.

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Lessons 9 & 10

Practical Z – An investigation into solubility

A Year 12 look at this relatively straightforward GCSE concept. You will need to
expand your use of terminology to an IB standard and develop further practical
skills. This will provide an opportunity to peer mark your work as per the IB
criteria.

The Appendices

In addition, there are several appendices of relevant information that will be of use
as you proceed with the experiments during your course. Much of the content of
the appendices is common sense, but this appears to be lacking in the average Year
12 student so a refresher is appropriate. You may work through these appendices
with your teacher in class, and refer to them during later experimental work.

Why study Chemistry? Well, take a look at the following Q & A


from a well-respected researcher with a doctorate in Chemistry:

Question: Is there really a chemistry of love?

Answer: I don't think there are any magic love potions that you can use to make
someone fall in love, but chemistry does play an important role in how a relationship
progresses. First, there's attraction. Nonverbal communication plays a big part in
initial attraction and some of this communication may involve pheromones, a form of
chemical communication. Did you know that lust is characterized by high levels of
testosterone? The sweaty palms and pounding heart of infatuation are caused by
higher than normal levels of norepinepherine. Meanwhile, the 'high' of being in love
is due to a rush of phenylethylamine and dopamine. All is not lost once the
honeymoon is over. Lasting love confers chemical benefits in the form of stabilized
production of serotonin and oxytocin. Can infidelity be blamed on chemistry?
Perhaps, in part. Researchers have found that suppression of vasopressin can cause
males (voles, anyway) to abandon their love nest and seek new mates. Hey, you gotta
have chemistry! (Anne Marie Helmenstine, PhD)

That’s right – love easily explained as a big bag of chemicals. What


did Physics ever give us? Gravity – woo hoo.

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Practical X - An investigation into acid / base reactions and
indicators.

In this investigation we find out why certain indicators work well for titrations in
some instances but not in others. You will titrate an acid with a soluble base (alkali)
and use an indicator to determine the equivalence point – when the acid has JUST
been neutralised. The two indicators most commonly used are methyl orange and
phenolphthalein. First we find out why universal indicator is not a good indicator for
titration work.

Indicator colour in acid colour in alkali


Methyl orange red orange
Phenolphthalein colourless pink

Instructions:

Part A

1. Rinse a clean burette with 10 cm3 of distilled water then with 10 cm3of the
solution of sodium hydroxide. Make sure the section of the burette below the
tap is rinsed then emptied into a labeled waste beaker.

2. Rinse a 25 cm3 pipette in the same way to prepare for use with the
hydrochloric acid solution.

3. Fill the burette with the sodium hydroxide solution and zero the liquid level,
making sure that the tap area is full and that there are no bubbles which would
compromise the accuracy of your work.

4. Pipette 25 cm3of the hydrochloric acid into a clean conical flask.


(We do not rinse the flask with the acid. Why not?)

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5. Add 2-3 drops of universal indicator to the flask and swirl. Make sure that the
colour is visible but not intense. Add a little more indicator if the colour
cannot be seen.

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6. Add the alkali from the burette into the acid in the flask a little at a time and
swirl after each addition. You should add about 1 cm3 at a time at the beginning
and systematically reduce the volume added as the equivalence point is
approached. We should never add a large volume of one reactant to another
without mixing thoroughly as in some cases this can result in inaccuracy.

7. Continue until you think that the equivalence point has been reached. Record
the volume of sodium hydroxide used in a result table. How confident can you
be of an accurate result using this indicator? Explain why.

8. Repeat the titration but using methyl orange as your indicator. Record the
amount of sodium hydroxide needed to neutralize 25 cm3 of the hydrochloric
acid and comment on the likely accuracy of your result.

9. Finally repeat once again but using phenolphthalein as your indicator.


Determine the difference in volume between your 3 results and comment on
which indicator(s) are acceptable for this acid/base pair.

Part B

1. Rinse your pipette with distilled water and then with the ethanoic acid
solution and pipette 25cm3 of this into a clean conical flask.

2. Add methyl orange as indicator and then titrate to an end point. Comment on
your result and the confidence you have in your value.

3. Repeat the operation using phenolphthalein as indicator and compare your


results. Can both indicators be confidently used for this acid base pair?

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Results table

Conclusions drawn:
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Theory – Measurements and Uncertainties

If a reported measurement is to be useful, it must include some indication of its


uncertainty. The complete expression of a measured quantity must include the
number value and the unit and also show how reliable the number is. This section
discusses how measurements are reported and used so that the reliability of the
numbers is understood by everyone.

Accuracy and Precision

The quality of a measurement depends on the measuring instrument and the skill of
the person making the measurement. Uncertainty in measurements can result from
limitations in accuracy or limitations in precision. The limitations may be those of
the instrument or the experimenter, or both.

Accuracy refers to the closeness of a measurement to the true or


accepted value of the quantity measured. An electronic balance that is often
calibrated with a standard mass is likely to be more accurate than an old,
mechanical balance that has been dropped many times.

Precision refers to the agreement among the numerical values of a set of


measurements of the same quantity made in the same way. A chemist who
frequently carries out a complex experiment is likely to have more precise
results than someone just learning the experiment.

Suppose it is necessary to determine the density of a sample of chloroform (CHCI3)


at 20oC. One chemist obtained values of 1.495g/ml, 1.476g/ml, and 1.485g/ml for
the density of the sample. These measurements vary widely; the precision is poor.
Another chemist repeated the measurements three times using the same
equipment as the first chemist and found densities of 1.487g/ml, 1.490g/ml, and
1.488g/ml. This group of measurements has good precision. Comparing these values
with the accepted value of 1.489g/ml for chloroform at 20 oC shows that this group
of measurements also has good accuracy.

If a measurement can be compared to the correct value, its accuracy can be judged
using percent error. Percent error is calculated as follows:

Value accepted – Value experimental

Percent Error = x100%


Value accepted

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Errors associated with apparatus:

Whenever it is available manufacturer's information (labels) should be reported


according to the specifications for the particular class of instrument e.g. on
pipettes, burettes and measuring cylinders if obvious.

If no error is stated on the apparatus, the following guidelines should be followed:

a) For most of the scale divisions (analogue equipment), the reading uncertainty is
equal to ± half scale division. Thermometers, measuring cylinders and burettes
are examples of such apparatus

For example, if a thermometer goes up in increments of 0.1oC then the error will
be ± 0.05oC (NB: readings and errors must be given to the same number of
decimal places, so a reading of 24.1oC should be recorded as 24.10 ± 0.05oC ).

b) For a digital readout, the absolute uncertainty is equal to the least count (not
one half the least count) or more specifically, the absolute uncertainty is equal
to the unit of the last place of the readout. Balances and pH meters are
examples of apparatus where this is appropriate.

For example, if a digital balance displays 63.24 grams for the mass of an object,
then the error = 0.01 grams. So the measured mass of the body would be:
(63.24 ± 0.01) grams.

Find as many different pieces of apparatus as possible in the laboratory and state
the errors associated with them, classified as Manufacturer’s, Digital or Analogue:

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The following pages cover material that is stated in the actual IB Chemistry
syllabus for topic 11 – this could be discussed in class or set as self study.

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Topic 11 Measurement and Data Processing

Pages 75 – 77 of the Chemistry for the IB Diploma IB Study guide (Neuss)


should also be referred to.

11.1 Uncertainty and Error

Precision and accuracy:

Precision: A measure of the amount of human error in taking a reading or a


measurement.

Accuracy: The equipment used will have a limit to the accuracy with which
measurements or readings can be taken. Most lab equipment has a standard level of
accuracy.

Therefore measurements can be precise but may not be accurate.

E.g. the volume of solution in a pipette may be recorded precisely using the
meniscus of the liquid, however it will still be inaccurate due to the limitations of
the accuracy of the pipette itself.

Random Uncertainties:

By combining together the precision of the measurement with the accuracy of the
equipment the total random uncertainty can be calculated for each reading taken.

This is given as a + and – as it could be above or below the actual reading.

E.g. Standard accuracy of 25cm3 pipette = ± 0.05 cm3

Estimation of precision with which readings are taken = ± 0.1 cm3

As opposed to estimating precision, the usual practice is to take a sufficient


number of repeats and obtain a RANGE of values for any specific reading. Other
random errors may arise from difficulty in determining colour changes etc.

Total random uncertainty = ± 0.15 cm3

(Random uncertainties are estimated and presented during DATA


COLLECTION)

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11.2 Uncertainties in Calculated Results

Processing Random Uncertainties

Random uncertainties can be presented as % uncertainty.

E.g. In a simple titration:

Uncertainty due to 25cm3 pipette = ± 0.15 cm3


Uncertainty due to burette = ± 0.05 cm3 for a titre reading of 14.25 cm3
% Uncertainty due to pipette = (0.15 / 25) x 100 = ± 0.6 %
% Uncertainty due to burette = (0.05 / 14.25) x 100 = ± 0.4%

Total random uncertainties = 0.6 + 0.4 = ± 1.0%

Note: Round up % uncertainties to 1 or 2 sig figs depending on circumstances.

Use of Significant Figures

When an answer is calculated, awareness must be displayed that it has an


uncertainty.

This can be done by choosing an appropriate number of significant figures.

E.g. Calculated concentration of acid by titration = 1.3245 mol dm-3 ± 1.3%

Since 1.3% of 1.3245 = ± 0.017 mol dm-3

Therefore the concentration could be: 1.3245 + 0.017 = 1.3415 mol dm-3
or: 1.3245 – 0.017 = 1.3245 mol dm-3

Clearly there is uncertainty in third significant figure of the answer.

The concentration should therefore be expressed as: 1.32 ± 0.02 mol dm-3

Or as a range: 1.342 – 1.325 mol dm-3.

(Random uncertainties are processed during DATA PROCESSING)

Systematic Errors

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Systematic errors are qualitative explanations describing why the answer given by
experiment differs from the actual literature/theoretical value.

If the experimental answer is below the literature value, the systematic errors
attempt to explain why this may be. These explanations may be in the form of:

• Human errors (e.g. misinterpretation of a colour change at end point)


• Equipment errors (e.g. the solid didn’t filter successfully, instrument was
calibrated incorrectly)
• Chemical errors (e.g. there were small amounts of other substances in the
solution that the acid may have reacted with, incomplete combustion)

There does not need to be any quantitative estimation of such errors.

(Systematic errors are explained and presented in the EVALUATION).

11.3 Graphical Techniques

• Construct a variety of types of graph to represent experimental data.

• Choose appropriate scales for graphs. This can affect the accuracy of any
calculations (e.g. gradients) using the graph.

• Use lines of best fit that can either be straight or smooth curves. Try to get
the same number of points on each side of the line.

• Interpret the shape of a graph and use to show proportional or inversely


proportional relationships.

• Although uncertainty bars are not specifically required in IB chemistry, HL


students are encouraged to show some appreciation of the uncertainty in
graphs.

• HL students are encouraged to use simple uncertainty bars and if a gradient is


calculated, appreciate the uncertainty in the gradient (max/min).

For further clarification, please read through the following extract from the IB
teacher’s guide (even they need help, sometimes).

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Errors and uncertainties in chemistry internal assessment
The consideration and appreciation of the significance of the concepts of errors and uncertainties
helps to develop skills of inquiry and thinking that are not only relevant to the group 4
experimental sciences. The evaluation of the reliability of the data upon which conclusions can
be drawn is at the heart of a wider scientific method that IB students consider in other areas such
as group 3 individuals and societies, and theory of knowledge. They then may apply this in their
subsequent educational, professional and personal lives.

Errors and uncertainties are addressed in “Topic 11: Measurement and data processing” of the
subject guide and this topic can be very effectively treated through the practical scheme of work.

The treatment of errors and uncertainties is directly relevant in the internal assessment criteria of:

• data collection and processing, aspects 1 and 3 (recording raw data and presenting
processed data)
• conclusion and evaluation, aspects 1, 2 and 3 (concluding, evaluating procedure(s), and
improving the investigation).

Expectations at standard level and higher level

The expectations with respect to errors and uncertainties in internal assessment are the same for
both standard and higher level students and are supported by topic 11 of the subject guide.

Within internal assessment students should be able to do the following:

• make a quantitative record of uncertainty range (±) (data collection and processing:
aspect 1)
• state the results of calculations to the appropriate number of significant figures. The
number of significant figures in any answer should reflect the number of significant
figures in the given data (data collection and processing: aspect 3).
• propagate uncertainties through a calculation so as to determine the uncertainties in
calculated results and to state them as absolute and/or percentage uncertainties (this
applies to both higher and standard level students). Only a simple treatment is required.
For functions such as addition and subtraction absolute uncertainties can be added. For
multiplication, division and powers, percentage uncertainties can be added. If one
uncertainty is much larger than others, the approximate uncertainty in the calculated result
can be taken as due to that quantity alone (data collection and processing: aspect 3).
• determine from graphs physical quantities (with units) by measuring and interpreting a
slope (gradient) or intercept. When constructing graphs from experimental data, students
should make an appropriate choice of axes and scale, and the plotting of points should be
clear and accurate. (Millimetre square graph paper or software is appropriate. Quantitative
measurements should not be made from sketch graphs.) The uncertainty requirement can
be satisfied by drawing best-fit curves or straight lines through data points on the graph
(data collection and processing: aspect 3). (Note: Chemistry students at SL and HL are
not expected to construct uncertainty bars on their graphs and may achieve “complete” for
aspect 3 of data collection and processing without them. However, students, probably
those who also study IB physics, often construct error bars and there is no requirement to
discourage them from doing so.)

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• justify their conclusion by discussing whether systematic errors or further random errors
were encountered. The direction of any systematic errors should be appreciated. The
percentage error should be compared with the total estimated random error as derived
from the propagation of uncertainties (conclusion and evaluation: aspect 1).
• comment about the precision and accuracy of the measurements when evaluating their
procedure (conclusion and evaluation: aspect 2)
• suggest how the effects of random uncertainties may be reduced and systematic errors be
eliminated. Students should be aware that random, but not systematic, errors are reduced
by repeating readings (conclusion and evaluation: aspect 3).

Explaining terms and concepts


(a) Random and systematic error

Systematic errors arise from a problem in the experimental set-up that results in the measured
values always deviating from the “true” value in the same direction, that is, always higher or
always lower. Examples of causes of systematic error are miscalibration of a measuring device or
poor insulation in calorimetry experiments.

Random errors arise from the imprecision of measurements and can lead to readings being
above or below the “true” value. Random errors can be reduced with the use of more precise
measuring equipment or its effect minimized through repeat measurements so that the random
errors cancel out.

(b) Accuracy and precision

Accuracy is how close a measured value is to the correct value, whereas precision indicates how
many significant figures there are in a measurement. For example, a mercury thermometer could
measure the normal boiling temperature of water as 99.5° C (±0.5° C) whereas a data probe
recorded it as 98.15° C (±0.05° C). In this case the mercury thermometer is more accurate
whereas the data probe is more precise. Students should appreciate the difference between the
two concepts (topic 11.1.2).

(c) Uncertainties in raw data

When numerical data is collected, values cannot be determined exactly, regardless of the nature
of the scale or the instrument. If the mass of an object is determined with a digital balance
reading to 0.1 g, the actual value lies in a range above and below the reading. This range is the
uncertainty of the measurement. If the same object is measured on a balance reading to 0.001 g,
the uncertainty is reduced, but it can never be completely eliminated. When recording raw data,
estimated uncertainties should be indicated for all measurements.

There are different conventions for recording uncertainties in raw data.

• The simplest is the least count, which simply reflects the smallest division of the scale, for
example ±0.01 g on a top pan balance.
• The instrument limit of error: this is usually no greater than the least count and is often a
fraction of the least count value. For example, a burette is often read to half of the least
count division. This would mean that a burette value of 34.1 cm3 becomes 34.10 cm3
(±0.05 cm3). Note that the volume value is now cited to one extra decimal place so as to
be consistent with the uncertainty.

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• The estimated uncertainty takes into account the concepts of least count and instrument
limit of error but also, where relevant, higher levels of uncertainty as indicated by an
instrument manufacturer, or qualitative considerations such as parallax problems in
reading a burette scale, reaction time in starting and stopping a timer, random fluctuation
in a voltmeter read-out, or difficulties in knowing just when a colour change has been
completed in a rate experiment or titration. Students should do their best to quantify these
observations into the estimated uncertainty.

In chemistry internal assessment it is not specified which protocol is preferred and a moderator
will support a teacher when it is clear that recording uncertainties has been required and the
uncertainties recorded are of a sensible and consistent magnitude.

(d) Propagating errors

Random errors (uncertainties) in raw data feed through a calculation to give an error in the final
calculated result. There is a range of protocols for propagating errors. A simple protocol is as
follows:

1. When adding or subtracting quantities, then the absolute uncertainties are added.

For example, if the initial and final burette readings in a titration each have an uncertainty of
±0.05 cm3 then the propagated uncertainty for the total volume is (±0.05 cm3) + (±0.05 cm3) =
(±0.10 cm3).

2. When multiplying or dividing quantities, then the percent (or fractional)


uncertainties are added.

For example,

molarity of NaOH(aq) = 1.00 M (±0.05 M) percent uncertainty = [0.05/1.00]×100 = 5%


3 3
volume of NaOH(aq) = 10.00 cm (±0.10 cm ) percent uncertainty = [0.10/10.00]×100 = 1%

Therefore, calculated moles of NaOH in solution = 1.00×[10.00/1000] = 0.0100 moles (±6%)

The student may convert the calculated total percent uncertainty back into an absolute error or
leave it as a percentage.

Note: A common protocol is that the final total percent uncertainty should be cited to no more
than one significant figure if it is greater than or equal to 2% and to no more than two significant
figures if it is less than 2%.

There are other protocols for combining uncertainties such as “root sum of square” calculations.
These are not required in IB chemistry but are acceptable if presented by a student.

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(e) Repeated measurements

Repeated measurements can lead to an average value for a calculated quantity. The final answer
could be given to the propagated error of the component values in the average.

For example,

Δ Hmean = 102 kJ mol–1 (±10%)

Δ Hmean = [+100 kJ mol–1 (±10%) + 110 kJ mol–1 (±10%) + 108 kJ mol–1 (±10%)] / 3

This is more appropriate than adding the percent errors to generate 30%, since that would be
completely contrary to the purpose of repeating measurements. A more rigorous method for
treating repeated measurements is to calculate standard deviations and standard errors (the
standard deviation divided by the square root of the number of trials). These statistical techniques
are more appropriate to large-scale studies with many calculated results to average. This is not
common in IB chemistry and is therefore not a requirement in chemistry internal assessment.

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Practical Y - Identifying the formula of a compound

This activity allows you to find the formula of a compound from your own
experimental data. It also helps you to think about the uncertainties in your
measurements and it gives you practice at converting mass to amount of substance.

Requirements

• copper strip (approximately 15 cm x 1 cm)


• emery paper
• dry filter paper
• access to a balance
• iodine crystals (0.3 g)
• boiling tube
• Bunsen burner

Introduction

You know for a fact that the formula of water is H 2O. But did you know that, like
every fact in chemistry, it has been experimentally determined; it has come from
observation and measurement?

One way to determine the formula of water is to break it down into its elements _
hydrogen and oxygen - in an electrolysis experiment:

water hydrogen + oxygen

The hydrogen and oxygen formed can be collected and the volume of each gas
measured. The mass of each gas produced can be calculated from the volumes and
then converted to the amount in moles. The simplest ratio of moles of atoms can be
found and thus the empirical formula of water.

Experiment Mass of Mass of


Hydrogen (g) Oxygen (g)
1 0.020 0.168
2 0.017 0.139
3 0.021 0.157

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The Table on the previous page gives the results of three experiments. Use these
data to find the empirical formula of water. The relative atomic masses of
hydrogen and oxygen are 1 and 16 respectively (Ar: H, 1; 0,16). The rest of this
activity will help you to find experimentally the formula of another compound - a
yellow compound formed when copper reacts directly with iodine vapour. In the
water example above the compound was broken down into its elements. In this
example, you will make a compound from its elements.

The exact masses which react together (reacting masses) can be measured and
then used to find the empirical formula of the compound.

What you do

1. Clean a strip of copper with emery paper and wipe it with a piece of dry filter
paper. Weigh the copper strip.

2. You need to use about 0.3g of iodine crystals so first weigh a dry boiling tube.
(You may find it helpful to stand the boiling tube in a beaker so that it does not
roll.) Add a small quantity of iodine to the boiling tube and reweigh it. (CARE Iodine
is harmful. Avoid skin contact and do not inhale the vapour.) Keep adding iodine
crystals until you have about 0.3g in the tube. It is not necessary to know the exact
mass of iodine in the tube, so you do not need to record the mass of the tube or
the iodine.

3. Bend one end of the copper strip so that it fits over the lip of the boiling tube
and the other end of the copper is about 2cm above the iodine crystals (Figure 1).

Boiling tube

Copper strip

HEAT

Figure 1

4. Gently heat the copper nearest to the iodine. This should be done in a fume
cupboard.

5. Continue heating until no more iodine vapour is seen but do not heat so strongly
that iodine vapour escapes from the tube. Keep moving the tube in and out of the
flame to avoid overheating it.

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6. Allow the tube to cool. Carefully remove the copper strip and reweigh it.

7. Remove the. yellow coating of copper iodide from the surface of the copper by
scraping gently with a spatula onto a piece of scrap paper and reweigh the copper
strip.

Record your results

Initial mass of copper strip = g


Mass of copper strip + copper iodide = g
Final mass of copper strip = g

Using your results

8. What mass of copper has reacted with the iodine?

9. What mass of iodine did it react with?

10. How many moles of copper atoms reacted? (Ar: Cu, 63.5)

11. How many moles of iodine atoms reacted? (Ar: I, 127)

12. How many moles of iodine atoms combine with one mole of copper atoms?

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13. What formula does this indicate for the copper iodide?

Evaluating your results and procedures

As a matter of routine, on completing an experiment you should review and evaluate


the procedures you used so that you can identify any that could have been sources
of error. Where your experiment involves measurements, you should consider
whether the sources of error in your procedure would tend to make your values
larger or smaller. For example, if it was difficult to remove all of the copper iodide
then the final mass of copper would be too high.

As well as evaluating your procedures it is also important to bear in mind that when
any physical measurement is made there is always some kind of uncertainty
associated with the value obtained. This is sometimes referred to as experimental
error, although it is not a mistake.

A source of uncertainty is the precision of the instrument being used. Every


measuring instrument is designed to measure to a certain level of precision. For
example, the copper iodide activity involves several weighings using a balance. The
commonest balance you will use reads to 2 decimal places but there is an
uncertainty associated with the second place. Remember – balances give DIGITAL
readings.

For example, a reading of 11.46g means that the mass is between 11.45g and 11.47g.
This can be written as 11.46 ± 0.01g .

± 0.01g is the precision error of the balance.

To compare the importance of the precision errors for different measurements


they are usually expressed as percentage errors.

error x 100
Percentage error = reading

In this case, the percentage error = 0.01g x 100 = 0.08%


11.46 g

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QUESTIONS

a. What was the percentage error for each of the three weighings that you did?

b. How is the percentage error related to the value of the mass recorded?

c. If you wanted to reduce the percentage error for the initial mass of copper,
would you use a smaller or larger piece of copper?

d. Identify stages in your procedure which could have led to errors. How would
these errors have influenced the answer you obtained for I2?

e. Look at all the sources of error associated with weighing and with carrying out
your experiment. Which one(s) do you think had the greatest effect on your final
result? If you were to repeat the experiment, write down any changes you would
make to how you would carry it out or with which parts of the procedure you would
take extra care.

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Theory - Criteria used for internal assessment of experimental
work

As stated previously, internal assessment of your experimental work will constitute


24% of your overall IB level. The criteria for marking that is followed may appear
confusing at first, but you will have plenty of opportunities to gain marks in each of
the respective disciplines – do not be discouraged if your initial few marks are a
little low! As you become more familiar with the criteria, so your marks will improve
(Year 13 is when you expect to gain most of the marks that will be used in your final
level).

In the next two lessons, you will take a look at the marking criteria as well as some
examples of past students’ work – along with the marks allocated.

For these lessons you will need the following:

• IB Diploma Chemistry Guide


• Practical Scheme of Work Record (PSOW)
• A manila folder

If you do not have these three items, ask your teacher nicely for them (manners
cost nothing, you know).

The following extract gives some clearly set out examples of students’ work, along
with the allocated marks as explained by the IB Diploma assessors. Note carefully
the layout of results, the decimal places, the significant figures, the errors
associated, etc. It is attention to detail and GLP (Good Laboratory Practice) that
will lead to level 6s being obtained.

REMEMBER – always refer to the marking criteria in your


Chemistry guide when writing up practical work.

23
Interpreting the relevant assessment criteria
Data collection and processing: Aspect 1 (recording raw data)

Sample extracts of typical student work from an experiment on volumetric analysis in acid-base
titration are shown in tables 1–3.

Table 1: DCP aspect 1 = “partial”

Table 1

a. Titration of standard NaOH against vinegar

Final volume / cm3 42.5 41.5


3
Initial volume / cm 2.5 1
3
Volume of base required / cm 40.0 40.5
Colour of solution at end point light pink dark pink

Some appropriate raw data is recorded but there are no uncertainties and the number of decimal
places is inconsistent. Either of these factors reduces the level of achievement for aspect 1 of data
collection and processing to partial/1.

Table 2: DCP aspect 1 = “partial”

Table 2

b. Titration of standard HCl against NaOH

Run 1 Run 2 Run 3


3 3
Initial volume / cm (±0.1 cm ) 0.0 2.7 1.0
Final volume / cm3(±0.1 cm3) 42.2 42.7 41.5
Volume of base required / cm3(±0.2 cm3) 42.2 40.0 40.5

Some appropriate raw data is recorded with units and uncertainties. However, relevant qualitative
observations were not recorded and the level of achievement for aspect 1 of data collection and
processing is partial/1.

Table 3: DCP aspect 1 = “complete”

Table 3

c. Titration of 5.00 cm3 vinegar against the standardized NaOH

Trial 1 Trial 2 Trial 3


3 3
Initial volume / cm (±0.05 cm ) 1.00 2.55 0.00
3 3
Final volume / cm (±0.05 cm ) 42.50 43.25 40.50
3 3
Total volume of base required / cm (±0.1 cm ) 41.5 40.7 40.5

24
Colours of solutions: acid, base and phenolphthalein indicator were all colourless. At the end
point, the rough trial was dark pink. The other two trials were only slightly pink at the end point.

The student records appropriate qualitative and quantitative raw data, including units and
uncertainties. The level of achievement for aspect 1 of data collection and processing is
complete/2.

The following examples of data collection and processing (see tables 4–6) are from a gas law
experiment.

Table 4: DCP aspect 1 = “complete”

Table 4

Temperature T / °C ± 0.2° C Height of column h / mm ± 0.5 mm


10.5 58.0
20.3 60.5
30.0 61.0
39.9 64.0
50.1 64.5
60.2 67.5
70.7 68.0
80.8 71.0
90.0 71.5

In table 4, the student designed the data table and correctly recorded the raw data, including units
and uncertainties. The level of achievement for aspect 1 of data collection and processing is
complete/2.

Table 5: DCP aspect 1 = “partial”

Table 5

Temperature (T) Height of column (h)


10.5 58.0
20.3 60.5
30.0 61.0
39.9 64.0
50.1 64.5
60.2 67.5
70.7 68.0
80.8 71.0
90.0 71.5

In table 5, units and uncertainties are not included. The level of achievement for aspect 1 of data
collection and processing is partial/1.

25
Table 6: DCP aspect 1 = “partial”

Table 6

Temperature Height of column


10.5 58
20.3 60.5
30 61
39.9 64
50 64.5
60.2 67.5
70.7 68
80.8 71
90 71.5

In table 6, units and uncertainties are not included, and the data is recorded in an inconsistent
manner. Significant digits are not appreciated. The level of achievement for aspect 1 of data
collection and processing is partial/1.

Note: In investigations where a very large amount of data is recorded (probably by a data logger),
it may be more appropriate to present the data as a graph. The uncertainties should be recorded
on the axis labels and any qualitative observations recorded as annotations on or below the graph.

26
Data collection and processing: Aspect 3 (presenting processed data)

Figures 1 and 2 show graphs of the gas law data from table 4.

Figures 1 and 2: DCP aspect 3 = “complete”

Figure 1

Figure 2

27
Figure 1 is a graph of the gas law data showing the significant uncertainty. The computer drew
the uncertainty bars based on the student entering the correct information, which in this case was
0.5 mm for each value. Figure 2 does not show the uncertainty bars. In chemistry, students are
not expected to construct uncertainty bars. In both graphs the title is given (although it should be
more explicit), and the student has labelled the axes and included units. The level of achievement
for aspect 3 of data collection and processing for both graphs is complete/2.

Figure 3: DCP aspect 3 = “partial”

Figure 3

In figure 3, the student does not include a title for the graph, and the units are missing. The level
of achievement for aspect 3 of data collection and processing is partial/1.

Figure 4: DCP aspect 3 = “not at all”

Figure 4

28
In the examples shown in figure 4, the first student has failed to draw a best-fit line graph and the
second has drawn no line at all. The units and the titles of the graphs are missing. In the second
graph, poor use is made of the x-axis scale/ The level of achievement for aspect 3 of data
collection and processing for both graphs is not at all/0.

Conclusion and evaluation: Aspects 1, 2 and 3 (concluding, evaluating


procedure and improving the investigation)

When attempting to measure an already known and accepted value of a physical quantity, such as
the charge of an electron, the melting point of a substance, or the value of the ideal gas constant,
students can make two types of comments:

1. The error in the measurement can be expressed by comparing the experimental


value with the textbook or literature value.
Perhaps a student measured the value of the ideal gas constant R = 8.11 kPa dm3 mol–1 K–
1
, and the accepted value is 8.314 kPa dm3 mol–1 K–1. The error (a measure of accuracy,
not precision) is 2.45% of the accepted value. This sounds good, but if, in fact, the
experimental uncertainty is only 2%, random errors alone cannot explain the difference,
and some systematic error(s) must be present.
2. The experimental results fail to meet the accepted value (a more relevant comment).
The experimental range does not include the accepted value. The experimental value has
an uncertainty of only 2%. A critical student would appreciate that they must have missed
something here. There must be more uncertainty and/or errors than acknowledged.

In addition to the above two types of comment, students may also comment on errors in
the assumptions of the theory being tested, and errors in the method and equipment being
used. Two typical examples of student work are given in figures 5 and 6.

Figure 5: CE aspect 1 = “partial”, aspect 2 = “not at all”

Figure 5

29
Conclusion and evaluation: Intermolecular bonds are being broken and formed which consumes
energy. There is a definite correlation between the melting point and the freezing point of a
substance. If good data is collected, the melting point should be the same as the freezing point. A
substance should melt, go from solid to liquid, at the same temperature that it freezes, goes from
liquid to solid. Our experiment proved this is true because, while freezing, the freezing point was
found to be 55 °C, and when melting, the melting point was also found to be 55 °C (see graph).

The student states a conclusion that has some validity. No comparison is made with the literature
value. There is no evaluation of the procedure and results. The level of achievement for aspect 1
of conclusion and evaluation is partial/1. The level of achievement for aspect 2 is not at all/0.

Figure 6: CE aspects 1, 2 and 3 = “complete”

Figure 6

Melting point = freezing point = 55.0 ± 0.5 °C

Conclusion and evaluation: Literature value of melting point of para-dichlorobenzene = 53.1° C


(Handbook of Chemistry and Physics).

The fact that % difference > % uncertainty means random errors alone cannot explain the
difference and some systematic error(s) must be present.

Melting point (or freezing point) is the temperature at which the solid and the liquid are in
equilibrium with each other: (s) ⇌ (l). This is the temperature at which there is no change in

30
kinetic energy (no change in temperature), but a change in potential energy. The value suggests a
small degree of systematic error in comparison with the literature value as random errors alone
are unable to explain the percentage difference.

Evaluation of procedure and modifications:

1.Duplicate readings were not taken. Other groups of students had % uncertainty > % difference,
that is, in their case random errors could explain the % difference, so repeating the investigation
is important.

2.How accurate was the thermometer? It should have been calibrated. In order to eliminate any
systematic errors due to the use of a particular thermometer, calibration against the boiling point
of water (at 1 atmosphere) or better still against a solid of known melting point (close to the
melting point of the sample) should be done.

3.The sample in the test tube was not as large as in other groups. Thus the temperature rises/falls
were much faster than for other groups. A greater quantity of solid, plus use of a more accurate
thermometer (not 0.5°C divisions, but the longer one used by some groups) would have provided
more accurate results.

The level of achievement for aspects 1, 2 and 3 of conclusion and evaluation is complete/2.

31
Practical Z – An investigation into solubility

You are going to investigate the way that the solubility of a salt changes when we
change the temperature, and to graph your results. Marks will be awarded for the
way in which you carry out the experiment. This means CONTROLLED heating,
CAREFUL measurement of masses and volumes and GOOD OBSERVATION as well
as the ability to calculate the solubility and draw a graph.

1. Weigh out exactly 5g of potassium CHLORATE on to a square of paper, and make


sure that all of the crystals go in to a dry boiling tube.

2. Clamp the tube and contents onto a stand, and arrange it so that it can be
lowered easily in and out of a 250 ml beaker half full of tap water. Marks will be
awarded for how well you can operate these pieces of equipment.

3. Add 10 ml. (10g) of PURE water using the measuring cylinder or syringe provided.
The salt will not dissolve in 10g of water at this temperature no matter how much it
is stirred, but will dissolve if heated to a higher temperature.

4. Raise the temperature of the tube gradually by placing it into the beaker of
water and heating the beaker of water. Watch carefully until the solid completely
dissolves, then IMMEDIATELY turn off your Bunsen and raise the tube from the
hot water by raising the clamp. [MAKE SURE YOU PRACTICE DOING THIS A
COUPLE OF TIMES BEFORE STARTING THE EXPERIMENT!] There is no need to
try to record the temperature at which the solid just dissolved; it is much more
accurate to record the temperature at which precipitation occurs because the
temperature has cooled.

5. As the tube cools watch out for the appearance of small crystals. This occurs
when the solution is just saturated. It is a good idea to CAREFULLY stir the
solution as it cools with the thermometer, and be ready to record the EXACT
temperature at which this 'snowing' occurs. If you are not paying full attention you
will miss this!

6. When you have read the temperature record it in the appropriate place in the

results table.

7. Now add a further 5ml (5g) of pure water using the syringe. Stir with the
thermometer CAREFULLY and check that the salt does not dissolve. Now place the
tube and warm the solution again until the salt just dissolves. This should be at a
lower temperature than before, because you now have more water present to
dissolve the salt.

32
8. Repeat operations 5 and 6 to find out the new temperature at which the solution
becomes saturated.

9. Add a further 5ml of pure water and repeat operations 4, 5, and 6 to obtain a
new temperature for the saturation of 5g of your salt in 20ml (20g) of water.

10. Repeat until you have a total of 30ml of water in your solution, or until the
solute remains dissolved even at room temperature. You should have 6
temperatures written down. Now try to do the calculations set out below.

RESULTS TABLE – Recorded as per IB Marking Criteria, with all associated


errors detailed

33
Calculations

WORK OUT the solubility of your solute in g per l00g of water at each of the
temperatures recorded. Propagate errors as appropriate.

Graph your results by hand (line of best fit) or using a software programme like
Excel (if using EXCEL then graph must be an X-Y scatter with a trend line).

Plot solubility of KClO3 per 100g. water against temperature.

e.g. at 78 °C 5g of KClO3 dissolved in 10g of water

therefore the solubility of KClO3 at 78°C is 5g x l00g/l0 g

= 50g per l00g water.

Question: What factors affect the solubility’s of the ions shown in your results?

34
Appendix 1: Questions on Techniques & Safety

Section A: Identify the following pieces of equipment.

Section B: Answer the following questions in complete sentences.

1. As soon as you enter the lab, what safety equipment should you put on
immediately?

2. Before doing an experiment, what should you read and discuss with your
teacher?

3. Before you light a burner, what safety precautions should always be


followed?

4. What type of flame is preferred for laboratory work and why?

35
5. Why are broken glassware, chemicals, matches, etc. never thrown into a
wastepaper basket?

6. Why should you never touch chemicals with your hands?

7. What precaution can you take against chemical contamination in reagent


bottles?

8. Why are chemicals and hot objects never placed directly on a balance pan?

9. List three instruments used in the laboratory for measuring small quantities
of liquids. What precautions should be taken when filling a burette with
liquid?

10. How can a liquid be transferred from a beaker to a funnel without spattering
and without running down the outside wall of the beaker?

11. What procedure is used to dilute a concentrated acid?

12. How would you dispose of a spillage of concentrated sulphuric acid?

Section C: Hazard Symbols

Identify each of these hazard symbols:

Appendix 2: Techniques and Safety

36
Decanting and Transferring Liquids

1. The safest way of transferring a liquid from one test


tube to another is shown in Figure S-1. The liquid is
transferred at arm's length with the elbows slightly bent.
This position enables you to see what you are doing and still
maintain steady control.
Figure S-1.

2. Sometimes liquids contain particles of insoluble solids


that sink to the bottom of a test tube or beaker. Use one of
the methods shown below to separate a supernatant (the
clear fluid) from insoluble solids.

(a) Figure S-2 shows the proper method of decanting a


supernatant liquid in a test tube.

Figure S – 2

(b) Figure S-3 shows the proper method of decanting a supernatant liquid in a
beaker by using a stirring rod.

The rod should touch the wall of the receiving vessel. Hold
the stirring rod against the lip of the beaker containing the
supernatant liquid. As you pour, the liquid will run down the
rod and drop off into the beaker resting below. In this way
the liquid will not run down the side of the beaker from
which you are pouring.

37
Heating Substances and Evaporating Solutions

1. Use care in selecting glassware for high-temperature heating. The glassware


should be Pyrex or a similar heat-resistant type.

2. When heating substances in glassware by means of a gas


flame, use a ceramic-centered wire gauze to protect
glassware from direct contact with the flame. These
wire gauzes can withstand extremely high temperatures
and will help prevent glassware from breaking.

Figure S-4 shows the proper setup for evaporating a


solution over a water bath.

Figure S-4

3. In some experiments you are required to heat a substance to high temperatures


in a porcelain crucible. Figure S-5 shows the proper apparatus setup used to
accomplish this task
.
4. Figure S-6 shows the proper setup for evaporating a solution in a porcelain
evaporating dish with a watch glass cover that prevents spattering.

5. Heated glassware, porcelain, and iron rings look cool several seconds after they
are removed from a heat source, but can still burn your skin for several minutes.
Use heat-safety items such as safety tongs, heat-resistant mittens and pads,
aprons, rubber gloves, and safety goggles whenever you handle this apparatus.

Figure S-5

38
6. You can test the temperature of questionable beakers, ring stands, wire gauzes,
or other pieces of apparatus that have been heated by holding the back of your
hand close to their surfaces before grasping them. Any heat generated from
the hot surfaces will be felt - DO NOT TOUCH. Allow plenty of time for the
apparatus to cool before handling.

Note:
You will more likely use a
tripod, rather than an iron ring
on a clamp stand, but otherwise the set-up is the
same.

How to Pour Liquid from a Reagent Bottle

1. Read the label at least three times before using the contents
of a reagent bottle.

2. Never lay the stopper of a reagent bottle on the lab table.


Remove the stopper by grasping the stopper between two
fingers.

3. Pick up the reagent bottle making sure the label is toward the
palm of your hand. Note that the stopper is still between the
fingers.

4. When pouring a caustic or corrosive liquid into a beaker, use a


stirring rod to avoid drips and spills. Hold the stirring rod against
the lip of the reagent bottle. Estimate the amount of liquid you
need and pour this along the rod into the beaker.

5. Extra precaution should be taken when handling a bottle of acid.


Remember these two important rules: (a) Never add water to any
concentrated acid, particularly sulphuric acid, because of splashing
and heat generation, (b) To dilute any acid, add the acid to water in
small quantities, stirring slowly and constantly.

Remember the "triple A's"—Always Add Acid to water.

6. Replace the stopper on the reagent bottle after you are finished
pouring.

39
7. Examine the outside of the reagent bottle for any liquid that
has dripped down the bottle or spilled on the counter top.
Your teacher will show you the proper procedures for
cleaning up a chemical spill.

8. Never pour reagents back into stock bottles. At the end of


the experiment, any excess chemicals should be properly
discarded under the direction of your teacher.

How to Heat Material in a Test Tube

1. Check to see that the test tube is PYREX or a similar heat-


resistant type.

2. Always use a test tube holder or clamp when heating the


test tube.

3. Never point a heated test tube at anyone, because the


liquid may splash out of the test tube.

4. Never look down into the test tube while heating it.

5. Do not heat any one spot on the test tube. Heat the test tube from the upper
portions of the tube downward and continuously move the test tube. Otherwise
pressure from a vapour meeting a layer of liquid above it m may cause the bottom
of the tube to blow out.

How to Use a Mortar and Pestle


Figure S-11

1. A mortar and pestle should be used for grinding only one substance at a time.

2. Never use a mortar and pestle for simultaneously mixing different


substances.

3. Place the substance to be broken up into the mortar.

3. Pound the substance with the pestle and grind to pulverize.

5. Remove the powdered substance with a spatula.

40
CAUTION Do not blow into the mortar to remove any remaining powder, since
dust may get into eyes and nasal passages.

Testing an Odour Safely

1. Test for the odour of gases by wafting your hand over


the test tube and cautiously sniffing the fumes.

2. Do not inhale any fumes directly.

3. Use a fume cupboard whenever poisonous or irritating


fumes are evolved.

DO NOT waft and sniff poisonous or irritating fumes.

41
Liquid Measurements – Measuring Cylinders,
Pipettes & Burettes. Measuring
cylinder

1. For approximate measurements of liquids, a measuring


Pipette
cylinder such as the one shown to the right is generally
used. These cylinders are usually graduated in millilitres
(ml). Such a measuring cylinder may read from 0 to 10 ml,
0 to 25 ml, or more, from bottom to top.

2. A pipette or a burette is used for more accurate measurements. Burette

Pipettes are made in many sizes and are used to deliver measured
volumes of liquids. A pipette is fitted with a suction bulb (pipette
filler) which is used to withdraw air from the pipette while drawing up the liquid to
be measured. Always use the suction bulb.

3. Burettes, fitted with a tap, are used for delivering any desired quantity of liquid
up to the capacity of the burette. Many burettes are graduated in tenths of
millilitres. When using a burette, follow these steps:

a) Clamp the burette in position on a clamp stand. See Figure 1-10.

b) While filling the burette, place it on a stool, so that it


is below eye-level.

c) Place a beaker, 250-ml, at the bottom of the burette.


The beaker serves to catch any liquid that will be
drawn off.

d) Pour into a 100-ml beaker a quantity of the liquid you


want to measure from the liquid's reagent bottle.
Remember to carefully check the label of the reagent
bottle before removing any liquid.

e) Fill the burette with the liquid and then draw off
enough liquid to fill the tip below the tap and bring the
level of the liquid down to the zero. The height at
which the liquid stands is then read accurately. (You
may need to flick the tap with your fingers to remove
air bubbles.)

42
4. Observe that the surface of a liquid in the burette is slightly curved. Such a
curved surface is called a meniscus. You read to the bottom of the meniscus, as
shown in Figure 1-11. This is the line AB. If you read the markings at the top of
the meniscus, CD, you will get an incorrect reading.

5. After you have taken your first burette reading, as


directed, open the tap and draw off as many millilitres of
the liquid as you wish. The exact amount drawn off is equal
to the difference between your first and final burette
readings.

Notes:
All the glassware used here may be graduated in
cubic centimetres (cm3) instead of millilitres (ml).
1ml = 1cm3
Glassware should be read to an accuracy of half
of one division e.g. if a measuring cylinder is
graduated in 1cm3 steps, give the reading to the
nearest 0.5 cm3. i.e. read 14.0 cm3 or 17.5 cm3

43
Appendix 3: Table of Ion valencies.

+1 (I) +2 (II) +3 (III) +4 (IV) -3 -2 -1


H+ Mg2+ Al3+ Sn4+ (tin(IV) N3- (nitride) O2- F-
Li+ Ca2+ Fe3+ Pb4+ (lead(IV)) P3- S2- (sulphide) Cl-
(iron(III)) (phosphide)
Na+ Sr2+ Mn4+ SO32- Br-
Cr 3+
(manganese(IV) PO4 3-
(sulphate(IV) –
K+ Ba2+ (chromium(III)) ) (phosphate(V) sulphite) I-
)
Rb+ Cu2+ V3+ SO42- NO2-
(copper(II)) (vanadium(III)) (sulphate(VI) – (nitrate(III) -
Cs+ sulphate) nitrite)
Fe2+ (iron(II))
NH 4
+
CO32- NO3-
(ammonium) Mn 2+
(carbonate) (nitrate(V) –
(manganese(II)) nitrate)
Cu+ Cr2O72-
(copper(I)) Ni2+ (dichromate(VI)) MnO4-
(nickel(II)) (manganate(VII))

Zn 2+
ClO-
(chlorate(I) -
Sn2+ (tin(II))
hypochlorite)
Pb2+ (lead(II)) ClO3-
(chlorate(V))

IO3- (iodate(V))

Notes:
Some d-block metals, and group 4 elements have more than one possible oxidation
state. When writing the name the oxidation state is indicated using Roman
numerals e.g. tin(II) chloride, iron(III) sulphate

Names in italics are old-fashioned, but are still commonly used. The old convention
was to use –ite to indicate the lower oxidation state and –ate to indicate the
higher oxidation state. So nitrate(III) was nitrite, and nitrate(V) was simply
nitrate. If nitrate, sulphate etc appear without a Roman numeral, assume the
higher oxidation state.

44
Appendix 4: Organic Functional Groups

Many important organic chemistry molecules contain oxygen or nitrogen. It's


essential to memorise the names and structures of these functional groups

Other functional groups that you will become familiar with include:

• Alkanes
• Alkenes
• Alkynes
• Haloalkanes (Halogenoalkanes)
• Aromatic Compounds that include a Benzene ring

45
46

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