GCE A2 CHEMISTRY Teachers' Guide 1 Contents GCE A2 CHEMISTRY Teachers' Guide Page 1. Introduction 1.1 - Overview of New Specification 1.2 - Rationale 1.3 - Changes for teaching from September 2008 4 5 6 2. Internal Assessment of practical skills, CH6 13 3. Contributors to the Teachers' Guide 21 GCE A2 CHEMISTRY Teachers' Guide 3 1. INTRODUCTION The WJEC A2 CHEMISTRY specification has been modified and updated for delivery from September 2009. The first AS awards will be made in Summer 2009 and the first A level awards in summer 2010. For the first availability of units, see page 2 of the specification. The specification can be delivered and assessed in centres throughout the UK. The revised QCA subject criteria for GCE CHEMISTRY require 3 units for A2, one of which will take the form of internal assessment of practical skills. This Guide is one of a number of ways in which the WJEC provides assistance to teachers delivering the new specification. Also essential to its introduction are the Specimen Assessment Materials (question papers and marking schemes) and professional development (CPD) conferences. Other useful provision: Examiners' reports on each examinations series Free access to past question papers via the WJEC secure website Easy access to specification and other key documents on main website On-line examination review Easy access to both the Subject Officer and to administrative sections Contact Points for GCE Chemistry are as follows: Jonathan Owen (Subject Officer) jonathan.owen@wjec.co.uk Matthew Roberts (Subject Support Officer) matthew.roberts@wjec.co.uk Subject page www.wjec.co.uk GCE A2 CHEMISTRY Teachers' Guide 4 1.1 Overview of the A2 Specification UNIT CH4 – Spectroscopy and Organic Chemistry (Analysing and building molecules) TOPIC 9 Spectroscopy TOPIC 10 Isomerism and aromaticity TOPIC 11 11.1 11.2 11.3 Organic compounds containing oxygen Alcohols and phenol Aldehydes and ketones Carboxylic acid and derivatives TOPIC 12 Organic compounds containing nitrogen TOPIC 13 Organic synthesis and analysis TOPIC 14 The process of how science works UNIT CH5 – Physical and Inorganic Chemistry TOPIC 15 15.1 15.2 15.3 Redox Redox and standard electrode potential Redox reactions Applications TOPIC 16 16.1 16.2 16.3 16.4 Chemistry of the p block General Group 3 (13) Group 4 (14) Group 7 (17) TOPIC 17 d Block transition elements TOPIC 18 Chemical kinetics TOPIC 19 19.1 19.2 Energy changes Enthalpy changes for solids and solutions Entropy and feasibility of reactions TOPIC 20 20.1 20.2 Equilibria General Equilibria Acid-Base Equilibria UNIT CH6 – Assessment of Practical Skills GCE A2 CHEMISTRY Teachers' Guide 5 1.2 Rationale The division of content in the A2 units has remained essentially the same as in the previous specification. The CH4 unit contains advanced level organic chemistry and associated spectroscopy. The CH5 unit contains advanced level inorganic and physical chemistry. The CH6 unit assesses practical skills acquired throughout the course via the completion of two exercises. One must be based on inorganic chemistry and its associated physical chemistry. The other must be based on organic chemistry and its associated physical chemistry. One must involve preparation and some analysis of a compound. The other may involve the identification of some unknowns through a planned procedure. Thus, students will be exposed to a wide range of meaningful practical techniques. A CH4 paper was set for the January series from 2010 to 2014 but this will not be the case for the remainder of the lifetime of this specification. From the academic year 2014-15 all A2 units will be available for summer entry only. GCE A2 CHEMISTRY Teachers' Guide 6 1.3 Changes to the specification for delivery in September 2009 Changes in Assessment Structure for A2 (a) Changes to Assessment Objectives The assessment objectives are listed on page 9 of the specification. A simplified interpretation of these is as follows: • • • (b) AO1 – k + u AO2 – applying k + u AO3 – prac skills (How Science Works) Changes to Assessment units There are 3 units for A2. Each assessment unit must now test all three AOs UNIT %of AS UM AO1 AO2 AO3 120 Raw mark 80 CH4 40 25 45 10 CH5 40 120 80 25 45 10 CH6 20 60 60 6 6 48 Note that AO2 forms a greater proportion of the total raw mark for the CH4 and CH5 papers compared to CH1 and CH2. No split units are allowed, so that the CH6a paper (the so-called synoptic paper) of the previous specification will cease to exist in the new specification. Changes in Content These have arisen in the following two ways: (a) 60% is specified by QCA criteria and this has resulted in • • • (b) some topics moving from AS to A2 some topics moving from A2 to AS some new topics The opportunity to delete unnecessary recall from the previous specification at the discretion of the examining team. GCE A2 CHEMISTRY Teachers' Guide 7 Details of changes in content The following indicates new learning outcomes and some deletions. UNIT CH4 – Spectroscopy and Organic Chemistry (Analysing and building molecules) TOPIC 9 Spectroscopy All statements referring to atomic emission spectra have been removed to AS. TOPIC 10 (b) Isomerism and aromaticity understand the term stereoisomerism as embracing both E–Z and optical isomerism; As stated in the AS Teacher Guidance booklet, E is from the German entgegen (opposite) and replaces trans; Z is from the German zusammen (together) and replaces cis. (g) describe and classify the nitration and halogenation reactions of benzene as electrophilic substitution, and recall the mechanism for these reactions †*; (The equation for the formation of NO2+ is not required.) Note that the equation for the formation of the NO2+ is not required. (h) describe the Friedel-Crafts alkylation of benzene †*; This is a new statement, introduced due to its continuing importance in organic synthesis. Note that several statements on halogenoalkane chemistry have been moved to AS. TOPIC 11 Organic compounds containing oxygen 11.1 Alcohols and phenol Simpler alcohol work – physical properties / social effects / use as a fuel – has been removed to AS. Alkaline hydrolysis of halogenoalkanes is now more generalised and not restricted to 1bromobutane 11.2 Aldehydes and ketones 11.3 Carboxylic acid and derivatives TOPIC 12 (g) Organic compounds containing nitrogen understand the formation of polypeptides and proteins and have an understanding of primary, secondary and tertiary protein structure; outline This statement has been modified to include simple ideas on primary, secondary and tertiary structure of proteins. GCE A2 CHEMISTRY Teachers' Guide 8 TOPIC 13 (b) Organic synthesis and analysis use given mass spectral data to elucidate the structure of simple organic molecules (up to and including C8 molecules, with one chlorine atom); The number of carbon atoms has increased from 5 to 8. (d) understand that n.m.r. spectra can give information regarding the environment and number of equivalent hydrogen atoms in organic molecules and use such supplied information in structure determination *; NMR will include spin-spin splitting or unsplit spectra at low resolution (l) outline the uses of thin layer chromatography (TLC), gas chromatography and highperformance liquid chromatography (HPLC) in analysis (details of the theory of chromatography and of the methods used are not required) and be able to find the composition of mixtures by use of retardation factor (Rf), retention time and peak area. The new criteria have necessitated the introduction of this statement. TOPIC 14 The process of how science works (a) understand and use the methods scientists employ in determining the accuracy, reliability and validity of their own and others' work; (b) appreciate the methods scientists employ in developing their own and others' work to produce new materials and applications, for example in natural product synthesis, using computational chemistry and in aspects of nanotechnology. Topic 14, the process of how science works, has been interpreted by some as largely the practical side of chemistry, and this is obviously an essential part of the subject. However, the way in which scientists work and how the ideas that they generate are further developed is an essential part of the scientific process. New ideas and procedures are subject to professional scrutiny as others try to replicate and assess the implications and possible developments from the initial work of both themselves and others. Questions will be asked, on a fairly basic level, that will attempt to explore this aspect of scientific thinking. The examiners will not expect detailed responses to questions but will be looking for answers that show that candidates have thought about modern developments in chemical science and how these might be further applied in a way to benefit mankind in general. Candidates will not be expected to have studied particular applications in any depth and indeed, questions may be phrased with the word 'suggest' so that candidates can have the opportunity to express their own thoughts in a meaningful way. GCE A2 CHEMISTRY Teachers' Guide 9 UNIT CH5 – Physical and Inorganic Chemistry The examiners have removed items regarded as unnecessary recall from this unit. TOPIC 15 Redox 15.1 Redox and standard electrode potential (d) recall and use the redox systems specified below, including the appropriate colour change and ion/electron half-equations Cu2+(aq)|Cu(s); Zn2+(aq)|Zn(s); H+(aq)|H2(g) Pt; Fe3+(aq), Fe2+(aq)|Pt; MnO4– (aq), Mn2+(aq)|Pt; X2(g)|2X (aq) (X = Cl , Br , I ); (e) use redox systems in addition to those in (d), for which all relevant information is supplied; Statement (e) gives examiners scope to use other redox systems provided all relevant information is supplied. 15.2 Redox reactions 15.3 Applications (m) explain the principles underlying the operation of the hydrogen fuel cell in terms of the electrode half reactions 2H+ + 2e– H2 and O2 + 4H+ + 4e– 2H2O in the presence of a platinum catalyst, its potential use for storing energy and generating electricity and heat, and the benefits and drawbacks of its use (details of cell construction not required). The hydrogen fuel cell is essentially an electrochemical cell. Overall reaction 2H2 + O2 → 2H2O EMF + 1.23V Forward (exothermic) reaction used to release energy. A fuel cell works like a battery but does not run down or need recharging. it will produce electricity and heat as long as fuel (hydrogen) is supplied. Reverse (endothermic) reaction used to store energy. Examples of advantages: "Clean" technology with water as only product; Convenient method of storing energy; More efficient than internal combustion energy at releasing energy from fuel. Examples of disadvantages: Energy is lost as storage cycle not 100% reversible; Problems of storing gases; Run at relatively low temperatures (~ 80 °C) so an expensive catalyst needed. GCE A2 CHEMISTRY Teachers' Guide 10 TOPIC 16 Chemistry of the p – block 16.1 General 16.2 Group 3 (13) (e) understand the electron deficient nature of Group 3 systems such as BF3, BCl3 and monomeric AlCl3 and their electron acceptor properties; (f) explain the ready formation of the Al2Cl6 dimer, its structure and its bonding; The statements are modifications and one is an extension of the previous specification (g) understand the formation of donor-acceptor compounds such as NH3.BF3; (h) recall that the affinity of AlCl3 for chlorine species results in industrially important catalysts such as (i) (halogen carriers in) the chlorination of benzene and (ii) low melting temperature ionic liquids, containing the chloroaluminate(III) ion, AlCl4–, which are being developed as "clean technology" solvents and catalysts for processes such as the polymerisation of alkenes; Ionic liquids are organic salts that generally have melting points below 100 °C, unlike conventional salts; and the melts are liquid over a wide temperature range. Ionic liquids with melting points below or near room temperature (RTILs) are especially interesting. For example, reactions and extractions may be performed under mild conditions, promoting lower likelihood of product thermal degradation and reducing energy costs. The organic products are immiscible in the ionic liquids, separate out and can be tapped off. The ionic liquid is recyclable. The archetypal ionic liquids are the N butylpyridinium chloride-aluminium(III) chloride, [N Bupy]Cl-AlCl3, and 1-ethyl-3-methylimidazolium chloride-aluminium(III) chloride, [emim]Cl-AlCl3, systems. In each case, the organic Cl dative bonds to AlCl3 followed by ionisation. There are approximately one trillion (1018) accessible room temperature ionic liquids. Room temperature ionic liquids have developed, in less than 20 years, from an adjunct to the US 'Star Wars' research on battery electrolytes, into an industrial reality as media for catalytic chemical processes. As an example, a wide range of acidic chloroaluminate(III) and alkylchloroaluminate(III) ionic liquids catalyse the dimerisation and oligomerisation of olefins. In what is an exceptionally simple system, the olefinic feedstock may be mixed with, or simply bubbled through, the ionic liquid catalyst to produce oligomeric products which have low solubility in the ionic liquid catalyst and separate as a less dense organic phase which is readily removed by tapping off. GCE A2 CHEMISTRY Teachers' Guide 11 (i) explain how boron nitride, BN, forms hexagonal and cubic structures corresponding to graphite and diamond respectively and, because of its hardness, chemical inertness, high melting temperature and semiconductor properties, is finding increasing use as lubricant, as wear-resistant coating and as nanotubes for wire sleeving, catalyst support and semiconduction; Boron nitride is isoelectronic to the elemental forms of carbon and isomorphism occurs between the two species. That is boron nitride possesses three polymorphic forms; one analogous to diamond, one analogous to graphite and ones analogous to the fullerenes. Graphite-type Boron Nitride B B B B B N N N N N B B B B B N N N N N B B B B N N N B B N B N N These sheets (unlike those in graphite) are in register. This means that layers are placed directly upon one another. The polar B-N bonds interfere with electron transfer so that boron nitride in this form is not an electrical conductor (in contrast to graphite). N N B B N Boron nitride nanotubes can also be constructed by "bending over the layer" and joining the two meeting edges. Due to its excellent dielectric and insulating properties, BN is used in electronics e.g. as a substrate for semiconductors, microwave-transparent windows, structural material for seals, electrodes and catalyst carriers in fuel cells and batteries. It can be prepared in the form of fibres, structurally similar to carbon fibres, sometimes called white carbon fibre. The diamond-like allotrope of boron nitride is widely used as an abrasive for industrial tools. (j) recognise that in none of the cases (f) to (i) above is the compound electron deficient. This new statement is self explanatory. 16.3 16.4 Group 4 (14) Group 7 (17) TOPIC 17 d block transition elements TOPIC 18 Chemical kinetics GCE A2 CHEMISTRY Teachers' Guide 12 TOPIC 19 Energy changes 19.1 Enthalpy changes for solids and solutions 19.2 Entropy and feasibility of reactions (f) appreciate that the entropy, S, of a chemical system is to a large degree determined by the freedom possessed by the molecules or atoms within the system, and that for all natural changes, entropy increases towards a maximum (definitions not required); (g) recognise that molecules or atoms in a solid have much more restricted freedom than in a gas and that, other factors being equal, entropy increases in the sequence S(solid) < S(liquid) < S(gas); (h) apply the equation relating free energy change, ΔG, to the entropy change, ΔS, ΔG = ΔH - TΔS and understand that, for a reaction: if ΔG is negative, the reaction occurs spontaneously; if ΔG is positive, the reaction does not occur spontaneously; (i) understand that, because of the entropy change, endothermic processes such as the boiling of liquids, the solution of some salts and the thermal decomposition of oxysalts may still occur spontaneously. The new QCA criteria have necessitated the introduction of this topic. The topic is treated in such a way as to keep recall to a minimum. There is a useful analogy with enthalpy which will help to explain the examiners' intentions here. Students may not be able to offer a definition of enthalpy or fully grasp its meaning. However, they may still be able to use the concept of enthalpy change and Hess' law to calculate enthalpy changes. In a similar way, it is intended that students should understand and be able to use and apply the above statements. TOPIC 20 Equilibria 20.1 General Equilibria (e) recognise that for a reaction with ΔG negative (see 19.2 (h)) Kp and Kc will have large values as the products predominate and that for a reaction with ΔG positive Kp and Kc will have small values as the reactants predominate; This is a new statement. 20.2 Acid-Base Equilibria GCE A2 CHEMISTRY Teachers' Guide 13 2. INTERNAL ASSESSMENT OF PRACTICAL SKILLS CH6 INTRODUCTION The AS work in Unit Three was concerned with developing basic practical skills in general and physical chemistry, especially in the fields of analysis, thermochemistry and kinetics, and relating these to the associated theory units. In A2 the focus shifts to inorganic and organic chemistry and the standard of practical skill required is increased to match the maturing skills of the candidates. As before, the ability to relate the practical work to the theory to their mutual benefit is an important aim of the unit. In this connection, although the assessment is based mainly on Assessment Objective Three - How Science Works (essentially the experimental aspect) marks are also allocated for Assessment Objective One (knowledge and understanding) and Assessment Objective Two (application of knowledge). To ensure full coverage, one experiment will be in the field of inorganic chemistry and one organic, each selected from a choice of four. Additionally there is a need to balance the type of experiment chosen: some involve a substantial planning element while others involve the preparation and quantitative analysis of a compound and there should therefore be no more than one experiment of the planning type. To be specific, if 6.I2 is chosen 6.O2 cannot also be used and vice versa. All candidates must carry out their practical work independently. Pairing up candidates, e.g. because of limited availability of equipment, is not permitted. The same applies of course to the written elements of the task and candidates are required to sign a declaration stating that all work is their own. Each of these exercises is designed to be carried out in an ‘open-book’ examination situation. Candidates should have free access throughout to their own notebooks, textbooks and any other resources normally available to them in the laboratory, including the internet. The work must however be carried out in the centre and under careful supervision. Candidates must not be permitted to take the pro forma or the questions within them outside of that environment. Centres must inform WJEC when their candidates will be undertaking their practical assessments so that random spot checks may take place. Completed work and relevant teacher results sheets must be securely stored by the Exams Officer before it is submitted to WJEC by the May 15 deadline. All candidates work will be marked by WJEC. GCE A2 CHEMISTRY Teachers' Guide 14 STRUCTURE OF THE UNIT The internal assessment unit in A2 makes up 20% of the A2 mark and thus 10% of the total A level mark. Each of the two pieces of work has a maximum of 30 marks, giving a total of 60 marks. Of these 30 marks, 24 are allocated to the overall practical exercise (called Assessment Objective 3 - How Science Works), 3 to questions testing knowledge and understanding (Assessment Objective 1) and three to questions on applying that knowledge (Assessment Objective 2). The 30 marks are divided into the four sections of Planning, Implementing, Analysing and Evaluating with the actual mark distribution being dependent on the type of exercise. The following describes the general nature of these sections and full details for each experiment are given when these are described. Planning In experiments having a significant planning component. I2 and O2, nine marks are allocated comprising six marks for the plan and three for AO1 and AO2 questions. In the remainder of the experiments five marks are allocated, including three for AO1 and AO2. Implementing In I2 and O2 implementing is a relatively minor component and is awarded up to six marks but comprises around fifteen marks in the other experiments where the actual conduct of the exercise is of major importance. Analysis Analysing the observations made is clearly important in I2 and O2 and is allocated twelve marks while being given around five marks in the other experiments. Evaluation This is given between three and five marks in all the exercises including three marks for AO1 and AO2 questions. GCE A2 CHEMISTRY Teachers' Guide 15 PRESENTATION OF WORK Normally a pro forma will be used and any additional sheets must be labelled with the candidate's name and securely attached to the pro forma at the correct place in the work and not all at the end. The two pieces of work must be connected together along with the Candidate Cover Sheet. The cover sheet must contain full details of the candidate and the experiments chosen. The declaration by the candidate that this is their own work and confirmation by the teacher must both be signed. All the work, additional sheets and cover sheet must be bound together by using a treasury tag in the top left-hand corner; paper clips should not be used, since they become detached in the packets. The work from the centre must be arranged in the candidate number order on the invoice. In the case of large centres having several practical groups it is sufficient for the scripts to be in invoice order within each group. No rough work or instruction sheets should be included with the work. Teacher Result Sheets are a vitally important part of most of the experiments since many of the Implementation marks are allocated by comparing the candidate’s results with those of the teacher. All relevant sections of these must be completed without ambiguity and it must be very clear if different candidates or sets of candidates have different solutions or materials and which candidate has which. All work should be in ink and any temporary pencil work written over in ink. GENERAL POINTS 1. Theory. For each experiment the section headed Theory (presented on a separate page) gives full details of how any required answers may be deduced. So long as candidates obtain these answers somehow, they are at liberty to use either the approach outlined or to follow any alternative method which they may prefer. The Theory Sections are not intended to be prescriptive but are meant simply to assist candidates in understanding the experiment in question. 2. Consequential marking. Any error on one section will not affect the mark given in a subsequent section. In particular, a candidate's plan should be checked by the teacher, deficiencies noted on the work, and the candidate given a correct plan to work with. 3. Equipment variations across centres have to be taken into account in mark schemes and teachers should report any features such as thermometer precision, availability of data logging and interfacing equipment and, especially, limitation in the type of balance available. Note that experiments 6.I1, 6.I3 and 6.I4 need at least a threeplace balance. 4. When experiments lead to results which differ significantly from those expected, this should be reported, together with any appropriate comment. In such circumstances it would be reasonable for the candidates to be marked on the basis of the teacher's results, so long as this is to their benefit. It should be appreciated, that if the teacher's result is not reported, it is not possible for the Board to take any remedial action should the candidate score badly by virtue of poor agreement with literature values. GCE A2 CHEMISTRY Teachers' Guide 16 5. Choice of experiments. Centres are required each year to choose from the given list of experiments one inorganic and one organic experiment. Not more than one planning type of experiment (i.e. 6.I2 and 6.O2) is allowed. This is to ensure an appropriate spread of experimental skills in the assessment. Centres are encouraged to vary their choices from year to year so that the exercises do not become repetitively stereotyped to the students. 6. Specimen pro formas are included to be used by the candidates if the centre wishes. If additional space is needed for any section then additional sheets should be attached to the pro formas in the appropriate position. Pro formas may be modified to suit individual centre needs. 7. Format of the Experiments The mark allocation described above (following the QCA/DECWL rules) has been designed to test all the skills previously examined for the A2 Work. The nature of the exercises, requiring the integration of skills within AO3 as well as the AO1 and AO2 question components, means that the work is intrinsically synoptic in character and thus needs no additional element of synoptic questions as in the previous specification. 10% of the marks are awarded for AO1 and for AO2 questions and these questions are very largely directed towards reinforcing the linkage between practical work and theory and helping to ensure that students carry their theoretical knowledge into the laboratory and their practical knowledge and experience into the examination room. It is, however, recognised that, for most teachers, laboratory time is both limited and precious. It is therefore advised that only the actual execution of the experimental work has necessarily to be carried out during laboratory periods. The great bulk of the listed questions can be answered either before or after the experimental work is undertaken but in Experiment 6.I2 and 6.O2 the required plans must obviously be formulated first. Teachers are therefore free to arrange the timing of the candidates' responses to the questions posed as they think most appropriate so long as they ensure that this is done under controlled conditions. GCE A2 CHEMISTRY Teachers' Guide 17 Inorganic Experiments Two types of experiment are offered here. Thus experiment 6.I2 is an identification exercise and the marks awarded will mostly relate to correct planning, identities and explanations and rationalisations thereof. By contrast, experiments 6.I1, 6.I3 and 6.I4 contain sections which involve accurate analysis by volumetric techniques. For the straightforward titrations, such as Part 1 of 6.I1 and Part 2 of 6.I3, an accuracy of about ± 0.8-1.0% will be expected for full marks, tapering off to zero for deviations exceeding about ± 2.5-4.0 %, depending on the difficulty of the titration involved. For titres of the order of 25 cm3 these limits correspond approximately to deviations of ± 0.20-0.25 cm3 and ± 0.60-1.00 cm3 respectively. For the somewhat more demanding mass aliquot titrations in I1, I3 and I4 the titre deviations will be more generously assessed. Note that accuracy will here be assessed on the titres, the primary experimental quantity, rather than on derived values such as percentage compositions in which apparently small deviations from theoretical values may conceal significant experimental errors. Where several aliquots of a solution are to be titrated the mutual consistency (or otherwise) of titres used in deriving an average value will also be taken into account, since titres deviating significantly in opposite directions from the correct result could otherwise lead to average values showing a spurious closeness to the theoretical quantity. Note that here it is especially important that supervising teachers should report fully their own results on the forms provided. Normally volumetric results will be marked on the basis of the theoretical results since the compounds prepared are stable and of well-defined composition but where this will clearly benefit the candidates the teacher's values may be used. In exceptional circumstances the centre average result may also be taken into account. As detailed in the AS guide the sensible use of significant figures in the avoidance of excessive truncation of calculator outputs of final results and the recording of measured data to the full precision of the apparatus (burette readings to 0.05 cm3 including initial 0.00 cm3 and weighings – 0.200g and not 0.2 g - ) is important. For the marking of yields (in experiment 6.I4) see under the same topic in the Organic Experiments. For all the experiments, both Organic and Inorganic, there are various questions, given on the pro formas, to be answered so as to explore the various areas listed above and the students' understanding of them (see Structure of the UNIT section above). GCE A2 CHEMISTRY Teachers' Guide 18 Organic Experiments Again two types of experiment are offered: here experiment 6.O2 is essentially an identification exercise and will be assessed in a fashion similar to that used for experiment 6.I2. The remaining experiments involve preparation and characterisation and, apart from the questions posed on the pro formas, will be marked largely on the basis of yields obtained and melting temperatures reported. In general, even for preparations which in theory give yields close to quantitative, it is quite easy for less experienced operators to lose product in the process of purification. See the next section. For that reason the experiments involve solid products (rather than liquids which are significantly more difficult to manipulate) and full marks are usually to be awarded for yields of 70 % or more. (Note, however, that penalties will be applied for products which are so wet that they lead to yields in excess of 100 %!) The marks given will taper off as the yield decreases but will only fall to zero if no product is obtained. Similarly the melting temperatures of the products obtained are also marked on a sliding scale. In most cases full marks will be awarded for melting temperature values within ± 2 °C (usually –2 °C!) of the literature value tapering off to zero where the deviation exceeds about ± 10°C. Again it is most important that supervising teachers should report their own yield and melting temperature value (together with any range over which melting occurs) on the forms provided since, where appropriate, these will also be taken into account in the marking. As for the Inorganic Experiments, the pro formas contain various AO1 and AO2-based questions, relating to the experiment, to be answered, which are intended to strengthen the theory-practical linkage. Obtaining good yields The main reason for poor yields is not so much a failure to carry out the reaction properly but rather a failure to remove all the product from solution usually during recrystallisation. In general the crude product contains the required product and impurities that are more and/or less soluble than this in the solvent to be used. Normally low yields are caused by adding excessive amounts of hot solvent in an attempt to dissolve the less soluble impurities under the impression that these are required product. Consequently on cooling much of the required product remains in solution. Clearly some judgement is needed but the best procedure is to add the minimum of hot solvent needed to dissolve what appears to be almost all of the product, filtering to remove insoluble impurities and cooling. Any solid then crystallising in the filter can be removed with a minimum of hot solvent. The lower the temperature to which the filtered solution is cooled the greater the yield of product since many organic compounds have large temperature coefficients of solubility. The solubility of benzenecarboxylic acid, for example, is about 0.2 g/100 cm3 of water at room temperature and 5.8g at 90o. Reluctant products can sometimes be induced to crystallise by scratching the inside of the vessel with a glass rod to provide nucleation centres. Some solutions are prone to supersaturation, a non-equilibrium phenomenon in which, although solid and solution should co-exist under the conditions prevailing, the rate of crystal growth is less than that of re-solution so that no crystal forms. The effect of scratching above or of the presence of dust particles, etc, is to provide a nucleus on which the rate of growth is increased. GCE A2 CHEMISTRY Teachers' Guide 19 Scale of experiments The scale of organic preparations may be adjusted either upwards or downwards, as teachers feel is necessary or expedient. It is, of course, their responsibility to ensure that such preparations, so modified, do in fact proceed satisfactorily, and any such changes must be made clear on the results sheets of both teachers and candidates. The inorganic exercises (6.I1, 6.I3 and 6.I4) however present a rather more difficult situation as regards the analyses which they contain. In these experiments the requirement to weigh accurately samples of about either 0.1 or 0.2 g clearly necessitates access to balances weighing to three decimal places. It is recognised that shortage of such equipment may present difficulties for some centres, especially where large numbers of candidates are involved, but here any change in the quantities stipulated would require corresponding changes in the concentrations of the solutions used in the analyses. Consequently, for any changes of scale in these cases, the onus must lie upon the centre concerned to ensure that the modified procedure would then actually work satisfactorily and to advise the WJEC in advance of their intentions, giving appropriate details. GCE A2 CHEMISTRY Teachers' Guide 20 General Safety Considerations The purpose of these general instructions is to acquaint students with many aspects of safety practice which are common to much of the A2 laboratory work and need not therefore be separately rehearsed in the Instruction Sheets for each Experiment. Specific dangers and hazards will, however, be noted individually where they occur. As a general approach, while students should not regard practical work with undue timidity, they must always treat both apparatus and reagents with care and respect and take full note of any hazardous properties which are indicated. Attention is drawn to the following: Eye protection This is of paramount importance in the laboratory. Centres are required to provide safety goggles for all experiments for this purpose. These should be 'chemical' grade goggles complying with the EN166 3 standard (formerly BS 2092 C). For students who normally need to wear glasses suitably strengthened personal safety spectacles may be a satisfactory alternative. Students should be warned of the possible hazards when goggles mist up. Inorganic Experiments Volumetric work A safety pipette filler should always be used here: never pipette any solutions by mouth, especially alkali since this is very caustic if it is swallowed. (Similarly solutions containing copper(II) ions or ethanedioate ions, for example, are toxic and should on no account be pipetted by mouth.) Spillages For solutions of dilute acids add excess water before mopping up. For solutions of dilute sodium (or potassium) hydroxide stand clear of any spillage since these can be very slippery as well as caustic: again dilute with water before mopping up. At the concentrations involved, other reagent solutions present only minimal hazards (e.g. potassium iodide, sodium thiosulfate, starch and iodine). No special precautions are necessary for the spillage of solids but if large amounts are involved they may be mixed with sand before sweeping up. GCE A2 CHEMISTRY Teachers' Guide 21 Contact with skin Where appropriate plastic gloves should be worn to prevent adsorption of harmful reagents by the skin. Remember though, that wet gloves are slippery and should not be used for handling apparatus or reagent bottles. If you splash any of the reagents (solutions or solids) onto your skin, notify your supervisor and wash the affected area with a large amount of water. Mercury thermometers Should one be broken, try to retain the liquid mercury. The vapour is a cumulative poison. If necessary droplets of mercury can be sucked up using a small aspirator pump. If mercury is spilled into floor cracks the volatility can be reduced by brushing in sulphur or zinc dust. Disposal of surplus material Unless otherwise instructed, small quantities of the chemicals may be disposed of by adding to running water in the sink and then discharging to waste. Organic Experiments The great bulk of organic compounds are to a greater or lesser extent flammable and should not therefore be exposed to naked flames or sparks. (This is especially true, for example, of fairly low boiling solvents such as propanone and ethanol.) In general, direct heating will only be necessary where heating under reflux is specified and for all other purposes the temperature attainable on a water bath (100 ºC) should be sufficient. Other hazards The procedures to be followed for spillages and contact with the skin are in general the same as for the Inorganic Experiments. Special care should be taken when working with concentrated acids. Note that water should never be added to concentrated sulfuric acid: if this is to be disposed of it should be added to an excess of water (not vice-versa). Specific hazards are indicated for individual experiments as appropriate. Teachers should note that they are responsible for ensuring safe working practice and that all practical work fulfils the requirements of the COSHH regulations and the Health and Safety at Work Act. GCE A2 CHEMISTRY Teachers' Guide 22 Contributors to the Teachers' Guide CH4 Dr David Ballard CH5 Dr Martin Anthoney Internal Assessment of Practical Skills, CH6 GCE Chemistry (A2) - Teacher Guidance/ED 19 September 2013 Dr Peter Blake