Advice on the practical exam

The basis on which Paper 5 is set is very clearly defined. Although this might make it predictable, recent experience has shown that questions can still be difficult. Since the restructuring of the examinations in 2006, Paper 5 has been set in order to provide students with a significant challenge. Additionally, since there is no actual practical work by the candidate, this means that questions can be set based on situations which would not normally be examined.
Methods

M1

A summary of a typical mark scheme for Paper 5

Skill Planning Breakdown of marks 15 marks Defining the 5 marks problem Methods 10 marks Analysis, 15 marks Dealing with 8 marks conclusions data and Evaluation 4 marks valuation e Conclusion 3 marks

describe the method to be used to vary the independent variable, and the means that will ensure that its value is measured accurately M2 describe how the dependent variable is to be measured M3 describe how each of the other key variables is to be controlled M4 explain how any control experiments will be used to verify that it is the independent variable that is affecting the dependent variable, and not some other factor M5 describe the arrangement of apparatus and the steps in the procedure to be followed M6 suggest appropriate volumes and concentrations of reagents M7 assess the risks in their proposed methods M8 describe precautions that should be taken to keep risks to a minimum M9 draw up tables for data that they might wish to record M10 describe how the data might be used in order to reach a conclusion

Statement Bank
Planning
Defining the problem

Analysis, conclusions and evaluation

Dealing with data
D1 identify the calculations and means of presentation of data that are necessary to be able to draw conclusions from provided data use calculations to enable simplification or explanation of data use tables and graphs to draw attention to the key points in quantitative data, including the variability of data

P1 P2 P3

P4

identify the independent variable in the experiment or investigation identify the dependent variable in the experiment or investigation express the aim in terms of a prediction or hypothesis, and express this in words or in the form of a predicted graph identify the variables that are to be controlled

D2 D3

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Advice on the practical exam

Evaluation
E1 identify anomalous values in provided data and suggest appropriate means of dealing with such anomalies within familiar contexts within familiar contexts, suggest possible explanations for anomalous readings identify the extent to which provided readings have been adequately replicated, and describe the adequacy of the range of data provided use provided information to assess the extent to which selected variables have been effectively controlled use these evaluations and provided information to make informed judgements on the confidence with which conclusions may be drawn

E2 E3

E4

rate and concentration. Here, the supporting explanation would need to be given in terms of the frequency of particle collisions as a result of greater concentration. A further request for a supporting graph may be given. Candidates will have to specify the independent and the dependent variables. They might also have to consider the need to control other variables. In a rate exercise, the independent variable might be a particular concentration or temperature while the subsequent rate of the reaction is the dependent variable. Alternatives to the rate such as the elapsed time would also be acceptable.

E5

Methods
When creating a method, the aim for a student should be to produce a method which can be followed by another, similar, student without the need to ask any supplementary questions. This means of course that fine detail is required and nothing should be omitted on the basis that it is obvious. The student may be provided with further information that builds on the stem, but the student is expected to have the experience of basic laboratory apparatus. A good way to ensure this is for the students to follow a programme of experimental work. This would also have the advantage of promoting the understanding of relevant theory. Basic techniques, such titrations, standard solution production and rate measurement, should be thoroughly understood in detail. Students also need to be aware of the various methods of volume and mass measurement available in a laboratory. For example, an experiment involving the production and collection of a gas, such as the effect of heat on nitrates, would require the student to be aware that gas syringes tend to have a capacity of 100cm3 and that the alternative use of a burette would allow for the collection of only 50cm3. This example shows how important it is for students to perform meaningful practical work in order to prepare them for Paper 5. There is no substitute for familiarity in handling the apparatus. On occasion, a diagram of the apparatus to be used is requested and the student needs to be able to represent the apparatus in a simple and understandable format. The diagram does not need to be of a text-book standard, but it is essential for the examiner to be able to recognise
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Conclusions
C1 draw conclusions from an investigation, p roviding a detailed description of the key features of the data and analyses, and considering whether experimental data supports a given hypothesis make detailed scientific explanations of the data, analysis and conclusions that they have described make further predictions, ask informed and relevant questions and suggest improvements

C2 C3

Planning
As the criteria show, all plans contain two distinct sections: defining the problem this is worth 5 marks the actual method this carries a further 10 marks.

Defining the problem

The question generally begins with a stem, which will contain information relevant to the plan and the aim of the plan. The area to be covered may or may not be familiar to students but the stem will contain all the detail required. Almost invariably, a prediction is required with a subsequent simple explanation of the basis of the prediction. For example, in a question about rate of reaction, a student may predict direct proportionality between
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Advice on the practical exam

each piece of equipment in the diagram. Practice drawing sessions are a very good idea. Relevant calculations are an almost routine requirement and these must be logically presented. The preparation of a standard solution of a solid acid such as ethanedioic acid requires the calculation of the mass to be dissolved in a chosen volumetric flask in order to produce the required concentration. The described procedure should indicate that the solid needs to be dissolved completely in distilled water prior to adding the solution to the volumetric flask. The student should make clear how they would ensure that all of this solution is transferred successfully to the volumetric flask. Once in the flask the solution is made up to the required mark, and must then be thoroughly mixed. Students are expected to calculate the amounts of substance used to suit the volume or size of the apparatus that they specify. For example, if the plan involves collecting a gas from the decomposition of a carbonate in a 100cm3 gas syringe the calculated mass of the solid should be such as to produce slightly less than 100cm3 of the gas. An integral part of any plan is the collection and presentation of results. Any processing of the results must be specified, and the figures obtained should also be presented as the derived results. The derived results may then be processed in order to confirm or deny the original prediction. This processing may be graphical or by some other means. The recorded results are those of the various steps taken in carrying out the procedure. For example, in an exercise to find the enthalpies of solution of Group I hydroxides the necessary results columns to be recorded are: the name or nature of the hydroxide the mass of a weighing bottle the mass of the weighing bottle and a sample of the hydroxide the initial temperature of the water and the final temperature of the solution. Each column should have the correct units, represented as either /g or (g) for any mass, for example. The next stage is to process the results: a to calculate the mass of hydroxide used b to calculate the number of moles of hydroxide used c  to calculate the number of joules of energy released into the solution d  to use the results to parts b and c to deduce the standard enthalpy change per mole of hydroxide.
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All plans have to be assessed for risk; examination questions can ask for: an assessment of the risks involved in a particular experiment how to deal with the risks both of these. In an exercise to determine the enthalpy of neutralisation with hydrochloric acid (students are told that this is harmful) and sodium hydroxide (students are told that this is corrosive), a student could be asked about a suitable precaution. Alternatively, an experiment on solubility may have hot water as a possible hazard.

Analysis, conclusions and evaluation

The three remaining skill areas (Data handling, Evaluation and Conclusions) are often dealt with in one question, but on occasion two smaller questions might be set to cover these areas.

Data handling
Typically the student will be presented with some data, usually tabulated, derived from an experiment. The details of the experiment are given to the student, who will then be asked to process the data and produce a system which incorporates all the results and allows not only correct patterns to become apparent but also detects anomalous results. The tabulated results will be the measured quantities of the processes carried out in a laboratory. For example, in an experiment to confirm the formula of zinc iodide by reacting excess zinc with iodine, the measurements would be: mass of an empty test tube mass of the test tube and zinc powder mass of the test tube, zinc powder and iodine mass of the test tube and excess of zinc. From these the student would calculate: the mass of zinc used the mass of iodine that reacted with that mass of zinc. These results would be tabulated, possibly alongside the original data, with each column showing the appropriate units and an expression to show how the values were calculated. All calculations should be correct and recorded to an appropriate number of significant figures and/or decimal places. The student will on occasion be told the degree
Advice on the practical exam

of accuracy required, but often the student will need to decide. Many balances weigh to the nearest 0.01g and hence masses should be recorded to 2 decimal places, remembering that whole number masses should be recorded to the same accuracy, e.g. 4.00g. In other circumstances, derived data should be recorded to the same number of significant figures as the least accurate item of supplied data. Where students are in doubt, it is reasonable to suggest 3 significant figures as appropriate for most calculations. Having processed the raw data, the next step involves either a series of calculations to be averaged or some form of graphical plot. In the zinc iodide experiment on the previous page, the ratio of the number of moles of iodine with the number of moles of zinc can be used to produce a series of ratios. These ratios can either then be averaged, excluding any anomalies to produce an appropriate result, or a graph could be plotted of the two molar values. In this case the appropriate slope would indicate the formula of zinc iodide. For example, if moles of zinc is plotted on the x-axis, and moles of iodine is plotted on the y-axis, the slope of the graph should be 2. This shows that the formula of zinc iodide is ZnI2. The first step in plotting a graph is an appropriate choice of scales for the two axes, with the independent variable along the x-axis. Suitable scales will allow the plotted points to use the graph paper as fully as possible. When choosing a scale it is useful to remember that the plotted points should be spread over at least half of each axis. Students must ask themselves whether or not the origin is a point on their graph. Whether or not to include the origin will usually be clear from the nature of the results, although generally the origin can provide a further useful point to be plotted. Chosen scales should be easily readable by the student, as they are plotting the graph. Many errors have been seen where students have chosen unhelpful scales. For example, the division of each of the two centimetre squares into three makes accurate plotting very difficult. Plotted points are best shown as small crosses, made with a hard, sharp, pencil. Most plotted points will show a clear trend, indicating whether the graph should be a straight line or a curve; a straight line is the more usual. The plotted points must first be assessed to identify any anomalous points. If any anomalous points are identified, they should be clearly
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Advice on the practical exam

labelled as such. The line of best fit is then drawn, either as a curve or straight line. This line may not pass through all or indeed any of the plotted points. As a rough guide, an equal number of points should lie on the left of the line and on the right of the line. An appropriate plot for the zinc iodide experiment would be a straight line passing through the origin. Alternatively, an experiment looking at how the rate of effusion of a gas depends on its molar mass should produce a curve if the effusion time is plotted against the molar mass.

Evaluation
The evaluation of a set of results can be approached in a number of ways. The aim of any experiment is to draw an appropriate conclusion, either to verify a relationship or to establish a new relationship. This is accomplished by looking at the nature of the results and the quality of the experiment itself. When anomalous results are identified, they should be clearly labelled as such. The source of the anomaly will often need to be identified and will usually fall into one of two categories, either as a positive or a negative deviation from the general trend. In a reaction involving the reduction of a metal oxide the anomaly might arise because the reduction was incomplete, leading to a larger than expected mass of metal. The excess mass of course is the unreacted oxide. If the reaction involves the thermal decomposition of hydrated iron(II) sulfate two, opposite, errors are possible: insufficient heating this will cause the residual mass to be too great over heating this will cause the residual mass to be too small. The former result corresponds to the incomplete removal of the water of crystallisation while the latter relates to the decomposition of the iron(II) sulfate into iron oxide. A student may be called upon to consider whether the actual experiment under consideration is of highenough quality to produce reliable results and appropriate improvements may be requested. If the results provide poor support for a conclusion it may well be that further repeats are needed, or that the range of results needs to be extended. Apparatus may need to considered from two viewpoints: is it appropriate? is it accurate?
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In the measurement of volume, burettes and pipettes are intrinsically more accurate than measuring cylinders but if for example the volume to be measured is large, a measuring cylinder could well be quite adequate. An experiment measuring a small temperature change in an enthalpy exercise often involves volumes of the order of 25cm3 to 50cm3 and a typical temperature change of the order of 5C to 10C, using a thermometer accurate to the nearest degree. In this case, the volumes could safely be measured with a measuring cylinder since the percentage error of the temperature change will be greater than that of the measuring cylinder. The volumes measured during titrations are about as accurate as simple exercises can be. If these are involved in an experiment the source of any error is likely to be elsewhere. Measuring small volumes or masses generally produces high percentage errors, whichever item of simple laboratory apparatus is used. As an example, an experiment to investigate the rate of reaction between hydrochloric acid and magnesium by measuring the volume of hydrogen produced requires less than 0.10g of magnesium if the gas produced is to be collected in a 100cm3 syringe. This is a very small mass of magnesium. Using a typical balance accurate to 0.01g would give a 10% error and consequently the accuracy of the syringe is of negligible significance. The error in measuring the mass of the magnesium will be the greatest percentage error.

Conclusions
The conclusion of an exercise draws upon the key features of data collected and the subsequent analyses. Usually the data will support a given hypothesis. However, it must be clearly understood that data which does not support an initial suggestion might also have to be considered. In the magnesium/acid reaction, processing could involve plotting a graph of rate against the relative concentration of the acid. Inspection of the graph would allow a deduction to be made about the order with respect to [H+] in the rate equation. This conclusion would then be considered in the light of an original hypothesis. This, in turn, could lead to further predictions and experiments. If the experiment is considered to be too approximate, suggested improvements to the exercise might be requested.

Summary
Paper 5 will continue to involve: the planning of experiments the processing and presentation of results the evaluation of results a decision as to whether the results do, or dont, support the original hypothesis. The use of supplied results, rather than the students own results, will allow these skills to be examined more fairly and more reliably.

AS and A Level Chemistry Cambridge University Press

Advice on the practical exam