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CHEM Year 1 Practical: Fundamentals of Practical Chemistry An introductory manual for the Year 1 Practical courses

1. COURSE OVERVIEW ........................................................................................................................................ 2

2 LEARNING OUTCOMES ................................................................................................................................... 3

3 ACADEMIC INTEGRITY .................................................................................................................................. 4

4 BREACHES OF ACADEMIC INTEGRITY ..................................................................................................... 4

5 COURSE ORGANISATION IN MORE DETAIL ............................................................................................ 5

6 WHAT DO WE EXPECT OF YOU? ................................................................................................................. 6

7 HOW WILL WE ASSESS YOU? ....................................................................................................................... 7

8 HOW DO WE SUPPORT YOU? ........................................................................................................................ 8

9 HEALTH AND SAFETY IN THE LABORATORY ENVIRONMENT ...................................................... 10

10 YOUR LABORATORY WORK ....................................................................................................................... 13

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1. Course overview This course overview is a short summary of the key features of the laboratory experience that you can expect in the first year of your degree. More detailed instructions for the experimental work that you need to undertake will be provided at the start of the laboratory course. 1.1 Where is it?

The practical courses in Chemistry are hosted in one of the teaching laboratories in B29.

Level 4 (B29:4005) is the teaching laboratory where you will undertake experiments to determine, and understand, the properties of inorganic and organic materials;

Level 5 (B29:5005) is the teaching laboratory where you will learn how to synthesise complex in-organic and organic compounds from simpler starting materials and use spectroscopic techniques to determine their structures

In addition to the main laboratories there are instrument rooms (B29:5013) and computer suites (B29:3012 and B29:4015) where you will spend some of your time during the courses.

1.2 When is it?

You will be allocated to a group which will have a practical session at the same time in each week of the semester. The first week of the semester will involve some introductory sessions. Laboratory sessions start in the second week and continue for a total of ten practical sessions.

First years will have practical sessions on a Monday or a Tuesday from 12:30 until 18:00.

1.3 Who runs it?

The following staff oversee the delivery of the practical courses in each of the teaching laboratories. During every laboratory session you will also be tutored by academic staff and post graduate teaching assistants.

Level 4 Colin Flowers

Laboratory Manager

C.M.Flowers@soton.ac.uk; room 29:4007

23327 or 023 8059 3327

Level 4 John Fosbraey

Technician

J.Fosbraey@soton.ac.uk, room 29:4009

24117 or 023 8059 4117

Level 5 Dr Thomas Logothetis

Laboratory Manager

thomas.logothetis@soton.ac.uk, room 29:5001

22193 or 023 8059 2193

Level 5 Diana Dias Fernandes

P-T Technician

D.C.Dias-Fernandes@soton.ac.uk

room 29:5007

23614 or 023 8059 3614

1.4 How does it work?

CHEM Year 1 practicals laboratory work

CHEM Year 1 practicals is the practical module associated with several core courses as per table below:

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Modulecodes Labmodule ORGANIC PHYSICAL INORGANIC

Year1Sem1

Y1-PracticalCHEM1031 CHEM1033 CHEM1035

Sem2 CHEM1032 CHEM1034 CHEM1036

Chemistry students will attend all courses and the associated practicals, whereas Natural Science students attend those practicals associated with their course choice(s).

Each week your laboratory session will require that you complete pre-laboratory exercises before you attend your session.

The practical part of the course commences at 12:30 and continues until 18:00. It is important that you manage your time to complete the work, allowing a period for clearing up as the laboratory will close promptly at 18:00.

The chemistry content of CHEM Year 1 practicals is organised in two broad areas.

One area consists of experiments that will illustrate techniques used in the synthesis of both or-ganic and inorganic materials. It will also introduce you to several spectroscopic methods that will allow you to work out their structure. These experiments will be carried out in the Level 5 teaching laboratory.

The second area relates to using experiments to understand the physical chemistry that under-pins the reactivity of matter (thermodynamics and kinetics) and which is the basis of the spec-troscopic and analytical methods used to determine molecular or material structure. These ex-periments will be carried out in the Level 4 teaching laboratory.

Many experiments will involve work at the interface between these two broad areas. Whichever area of chemistry you are covering in your laboratory work the learning outcomes specified at the beginning of the experiment will make it clear what you are expected to achieve.

Mathematics workshops

Year 1 also contains a maths component which is taught through workshops in both semesters 1 and 2. You will be allocated one workshop per week on your timetable. The maths component is examined at the end of each Semester, with the exam marks to the lab component of the Physical Chemistry part(s).

2 Learning outcomes Each experiment will have specified learning outcomes and your assessment will judge whether you have achieved them, and the degree of expertise you have demonstrated. In addition to these specific learning outcomes there are some general ones below that summarise the areas of com-petence that you will develop throughout your entire first year practical experience.

i. Understand the importance of experimental safety and risk assessments;

ii. Interpret experimental guidance (written, video, lectured) with care and at-tention to detail;

iii. Apply a variety of techniques and methodologies to the synthesis and anal-ysis of molecules and materials;

iv. Manage time effectively in the laboratory and in report writing to ensure that allocated tasks are completed on schedule;

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v. Describe experimental methods and outcomes in an appropriate laboratory record to a standard that would allow a skilled scientist to repeat your ex-perimental work;

vi. Organise experimental data clearly, logically and according to appropriate conventions;

vii. Analyse experimental data to provide an explanation for the observed ex-perimental outcome

viii. Apply appropriate formulae and conversions to generate quantitative infor-mation in preparation for experimental work and in the evaluation of the re-sults arising from it;

ix. Discuss experimental outcomes with respect to reliability of results in rela-tion to concepts such as accuracy, precision, ambiguity and levels of confi-dence;

x. Measure materials and properties with accuracy, precision and reproducibil-ity.

3 Academic integrity When you join our courses you sign up to a set of regulations which define what the University ex-pects of you with regard to your academic conduct. A fundamental aspect part of this is the con-cept of academic integrity. This requires that you conduct your academic life in the professional manner described via the SUSSED portal in the University Calendar, see http://www.calendar.soton.ac.uk/sectionIV/academic-integrity-statement.html.

The essence of this statement is captured in the following key points that involve you:

• Taking responsibility for your own work.

• Respecting the rights of other scholars.

• Behaving with respect and courtesy when debating with others even when you do not agree with them.

• Fully acknowledging the work of others wherever it has contributed to your own.

• Ensuring that your own work is reported honestly.

• Following accepted conventions, rules and laws when presenting your own work.

• Ensuring you follow the ethical conventions and requirements appropriate to your discipline.

• Supporting others in their own efforts to behave with academic integrity.

• Avoiding actions which seek to give you an unfair advantage over others.

4 Breaches of Academic Integrity If you are to work with academic integrity there are a number of practices you must avoid, including:

• Plagiarism - The reproduction or paraphrasing, without acknowledgement, from public or pri-vate (i.e. unpublished) material attributable to, or which is the intellectual property of another, including the work of students.

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• Cheating – Seeking to gain an unfair advantage before, during or after an assessment or as-sisting another student in doing so.

• Falsification – Any attempt to present fictitious or distorted evidence, data, references, experi-mental results and/or knowingly to make use of such material.

• Recycling – Where a piece of work which has already been used and assessed in one context is used again (without declaration) in a different context.

Please note that in cases where a person assists another in a breach of academic integrity, both parties will be penalized equally.

The University and the School regard breaches of academic integrity as reprehensible and an at-tempt to defraud other students and potential employers. Such breaches are taken very seriously and are dealt with according to the procedures noted in a related section in the University Calendar (http://www.calendar.soton.ac.uk/sectionIV/academic-integrity-procedures.html). Any breach of ac-ademic integrity that is confirmed will result in a note being placed on the student(s) file(s) and the following penalty will be imposed

(i) With ‘minor cases’, a mark of zero will be given for effected area of work, subject to the approval of the Academic Integrity Officer.

(ii) In more severe cases the Academic Integrity Officer can consider penalties from a mark of zero for a module up to termination of the course after appropriate investigation.

IMPORTANT: If you are missing or have collected poor data for a practical, you are not permitted to use another persons data (even if you acknowledge this in your write-up) UNLESS you have received permission to do so from the Lab Manager. Using another persons data without the Lab Managers permission will be treated as a breach of academic integrity by both yourself and the person who provided the data.

5 Course organisation in more detail 5.1 CHEM Year 1 Practicals Semester 1

1. Each of you will be allocated to a laboratory practical group early in the first week of the semes-ter. The correct information on your laboratory group will be posted on the Year 1 notice-boards in B29: level 2 (near the round tables) and you should check your on line timetable against this information. If there is a difference between the two you should contact Alison Tubb (timetabling@soton.ac.uk, 25506 or 023 8059 5506) for clarification.

2. Also contact Alison Tubb if you become aware of any timetable clashes. Do keep a check on your emails to see if there are any instructions regarding the practical courses.

3. Starting from Week 2 you will have one weekly practical session, always on the same day, which will start at 12:30 and will run until 18:00. It is permissible for you to take a short break during the practical session provided that (a) it is safe to do so (b) you do not miss any teach-ing and (c) you finish your work and leave the lab by 18:00.

4. Throughout the semester you will alternate between the two teaching laboratories. For example your group will spend Weeks 2, 4, 6, 8 and 10 in B29:4005 and Weeks 3, 5, 7, 9, and 11 in B29:5005 or the other way around.

5. In your allocated laboratory you will do the experiments in each laboratory in the same order as everyone else. You will undertake one experiment per week and most of the glassware you

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need will be provided (usually in trays) in the area of the laboratory where you work. More spe-cialist equipment will be provided separately.

6. You will perform the work with help from written guidance and from the tutors who will be in the laboratory with you. Careful use of both will ensure that you know what to do in the lab and what to do for your report.

7. You will be helped to organize your time to ensure that you complete your work and can leave before 18:00. No work can be carried out after this time.

8. Before you can leave the laboratory you will need to clean any equipment that you have used and return it to its starting location. This, and the tidiness of your workspace, will be checked by a tutor who will not allow you to leave until these tasks have been completed properly. A pro-portion of your assessment is related to this process.

5.2 CHEM Year 1 practicals Semester 2

The second semester has the same organization as the first with the following exceptions:

a. The experiments in each laboratory will be conducted in a ‘circus’ format. Every week all five of the experiments will be active with a group of between 5 and 8 students attending each. By the end of the course you will all have done the same experiments but in a different order.

b. Each experiment will have a specific location in the laboratory and the equipment for each will be provided at this location.

c. In addition to the laboratory experiments there will also be a (CHEM1034) Computational prac-tical. ALL students will be timetabled to perform this during Week 1 of Semester 2. There is no lab report associated with this practical – Instead, throughout the semester, groups of students will be timetabled to present their work/analysis and the assessment of the presentation will re-place the report mark. More details of about this can be found on the Level 4 Lab Website (www.l4labs.soton.ac.uk).

6 What do we expect of you? CHEM Year 1 practicals is a core module which means that it must be completed successfully be-fore you can progress to the next academic year. You are expected to:

• Attend 100% of the laboratory sessions that are allocated to you*.

• Complete a laboratory notebook throughout the practical sessions as instructed by your tutors.

• Submit laboratory reports by the deadlines specified, as directed in this course manual **.

• Attend the maths workshops and complete the maths assessments.

• Achieve a minimum of 40% for the lab component of each core module.

• Participate fully in the learning experience offered in your laboratory classes.

• Provide us with your thoughts on the course by completing a course question-naire at the end of the course.

PLEASE NOTE THAT IT IS NOT POSSIBLE TO PASS THE LAB COMPONENT OF THE MOD-ULE IF YOU HAVE ANY UNVALIDATED ABSENCES OR YOUR FINAL AVERAGE MARK IS BE-LOW 40%.

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* Absence from the course

If for any reason you miss one of your laboratory sessions, you must inform the relevant staff (us-ing inform-chem@lists.soton.ac.uk) as soon as possible.

As soon as you return you must contact the relevant Lab Manager to obtain a Laboratory Absence Form.

Once the form has been satisfactorily completed (i.e. the absence has been validated) it must be returned to the Lab Manager in person, where:

• If it is possible the missed session will be rescheduled.

• Where rescheduling is impractical, an alternative assignment will be issued to you. This must be completed/submitted within one week. The work will be assessed and this as-sessment will count towards your final mark (in place of the missed lab report).

IMPORTANT: The paperwork validating your absence must be submitted within two of your return from the absence.

** Late submission of coursework

Reports that are submitted late will have a deduction in marks applied with the size of the reduction rising in proportion to the time beyond the submission deadline. This procedure is described in the University Late Submission policy (http://www.soton.ac.uk/quality/docs/Extensions_and_Late_Submission_Penalties.doc).

IMPORTANT NOTE: Reports submitted more than five working days late will not be accepted (i.e.

will receive a mark of zero) and other assessed work (i.e. pre-labs, lab-books and interim reports)

will not be accepted after the specified deadline.

Note: More details on attendance, absence and the procedures to follow in the event of an ab-sence (or known future absence) can be found at http://www.l4labs.soton.ac.uk/policies/absence.htm

7 How will we assess you? CHEM Year 1 practicals is a core module which means that it must be completed successfully be-fore you can progress to the next academic year. This means that you have to complete the tasks that are set and do so to a standard that we judge meets the pass mark (35%) or better. Each of the tasks will be related to the learning outcomes described in Section 2 (and also the ones related to each specific experiment) and the assessments will allow your tutors to be sure that you will have achieved these learning outcomes by the end of the course.

The experiments in the two different teaching laboratories have slightly different assessment re-quirements which will be described in more detail in subsequent sections. However, the following will always be important:

• Completion of the associated Prelab exercises by midnight on the day before your lab ses-sion;

• Attendance at the laboratory sessions – mandatory and a prerequisite for all else!

• Maintaining a laboratory notebook throughout your laboratory sessions;

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• Submission and assessment of a short interim assessment completed during the laboratory session (not all experiments);

• Quality and quantity of chemical products produced in experiments;

• Quality of the measurements/ data/ spectroscopic results collected during experiments;

• Safe, efficient and well organised laboratory work and appropriate cleaning and clearance of work area and equipment before leaving the laboratory;

• Organisation and analysis of measurements/ data/ spectra collected during experiments;

• Written report of the experimental outcomes completed after the laboratory session;

• Submission of your work before the deadline specified.

For the Level 4 Laboratory, the breakdown of the assessments that will contribute toward your practical mark are detailed in the practical lab scripts.

For the Level 5 Laboratory, the various assessments will contribute towards your final mark as fol-lows: Pre-Lab: 10%

Lab (e.g. notes, tidiness, safety): 30% *

Main Report: 60% *

*Quality of results will be assessed as part of the lab notes and the report. Overall, theory aspects and practical aspects will contribute roughly equally to the grade of a practical

8 How do we support you? Your learning experience will be supported with resources to help you complete your experimental work, and to understand what you have done, why you have done it and how it works. It is also im-portant that we help you understand what you have to do to succeed on the course. There are three main points of delivery of this support: in advance, during and post assessment.

8.1 Advance support - The Blackboard portal

There is a major Blackboard (www.blackboard.soton.ac.uk) resource you will use during your prac-tical course – identified by the course code CHEM Year 1 practicals. This will contain all resources for your learning and also the Prelab materials.

8.2 Teaching and learning during laboratory sessions

When you are in the laboratory your learning will be supported by a combination of academic staff, teaching fellows and trained teaching assistants. All of them will teach you throughout your time in the laboratory with a combination of group sessions and one-to-one tuition.

In addition, you will each have extensive written guidance for each experiment and web access to the resources mentioned above.

An important aspect of any learning process is giving each student feedback on performance. This is a continuous process during your laboratory sessions. Informal discussion between students and/ or between staff and students is of incredible value in increasing understanding. You should make sure that you take full advantage of the feedback opportunities available throughout your sessions by getting involved in discussion about chemistry with your colleagues and tutors. Re-member that effective feedback starts with an effective input from you!

You can expect to have discussion about the techniques that you are using, the theory based on them and the quality of the reporting that you accomplish in your laboratory notebook.

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In some experiments there will be a requirement to complete an interim report which will be part of the assessment and which offers another opportunity for feedback before you complete a final re-port.

Finally, you will have your laboratory notebooks checked at the end of every laboratory session where comments will be provided on the standard you are achieving. At the same time you will have your work area checked to ensure that your space is clean and tidy – an important part of Health and Safety in the laboratory environment.

8.3 Feedback after each laboratory session

Once you have completed an experiment and report has been submitted it will be assessed. The purpose of the assessment is to arrive at a mark that will contribute to your module grade. In addi-tion, the assessment will identify your strengths and weaknesses and comments on these will be provided – another example of useful feedback.

There are three routes by which post laboratory feedback is provided to you which are noted below:

• Once a grader has assessed the report feedback is available on the submitted report in Turnitin. To access the information you need to navigate yourself to the link where you submitted the report and “view” the outcome. Further details how to submit reports and ac-cess feedback will be provided separately on Blackboard. Electronic feedback (comprising the assessor’s report describing the strengths and weaknesses of your work) will normally be available one week after the submission deadline of your report (provided the report was submitted by the deadline); however note the official policy that it will be made available within 10 working days of submission.

• If, having read the online feedback, you wish to clarify or discuss in greater depth the feed-back you have received you are welcome to make an appointment with the laboratory manager to do so. Please refer to http://www.l4labs.soton.ac.uk/policies/fb.htm for infor-mation of the procedure used to request clarification. Please note that this is an opportunity for clarification of clearly defined queries. The grade will not be discussed on such occa-sions.

• Provisional marks will also be posted either on the feedback site or via Grade-center on Blackboard. Seeing how your own performance develops against the benchmark of the rest of your colleagues is a useful resource when used sensibly. This information will typically be made available within 10 working days of feedback submission.

To make the best use of your online feedback you should read it in conjunction with a copy of your report, so you can identify exactly what it was you did well and what could be improved. In order to facilitate this process, and to have a record for your own development, we recommend to keep a feedback diary, where critical points are recorded for your perusal – reflection on feedback helps.

Your work will be assessed by academic staff or teaching assistants with the whole assessment being overseen and moderated by the appropriate laboratory manager. If you have anything you wish to discuss about your work you should contact the laboratory manager. Should the lab man-ager arrange for you to have an appointment with a member of the assessment team please make sure you stick to the time agreed. If you do wish to raise issues with grading or feedback, please do so in a timely fashion. Missing an agreed appointment without prior notification and without valid reason will forfeit your right to further additional feedback.

Note: Further information on online feedback (e.g. how to interpret/apply it, procedure to request clarification) can be found on http://www.l4labs.soton.ac.uk/policies/fb.htm.

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Your chance to give essential feedback to us

During your final week questionnaires will be issued. After that week’s work has been completed please take the time to anonymously fill in and submit the questionnaire – this feedback is valued and is used to refine the course, to make it a more relevant, productive and enjoyable experience for future students.

9 Health and safety in the laboratory environment 9.1 Emergency procedures

Fire alarm Turn off any naked flame and leave the laboratory by the nearest exit. Follow the teaching staff to the muster area outside the building without delay

Fire in work ar-ea

Immediately notify teaching staff and do not take any action that puts yourself or others at risk

First aid If you have any need for first aid, or see someone else in the laboratory who needs it, call one of the teaching staff in the laboratory.

Minor chemical contamination or burn

Go to the nearest sink and rinse effected area with plenty of cold water while asking someone to get a member of staff to assist you

Major chemical contamination

Remove effected clothing and rinse effected area in cold water. In extreme cases utilise the drench showers present near the exits if each teaching lab.

Please note that misuse of any safety equipment is considered to be a serious disciplinary matter.

9.2 Personal protective equipment (PPE) and appropriate clothing

You will be provided with a laboratory coat and a pair of safety glasses as part of your laboratory equipment. Any replacement of either item will be at your own expense. Please note the following laboratory rules with regard to the use of PPE, your own clothing and your belongings.

• Laboratory coats* and safety glasses are to be worn in the laboratory at all times;

• Safety gloves will be provided and must be worn as instructed;

• Long hair (including fringes) must be tied/ held back. If you use a hat for this purpose it must not reduce vision or hearing or be offensive to others;

• Legs, ankles and feet must be fully covered while in laboratory. Shorts, skirts and open toed footwear are not allowed;

• Phones, mp3 players and similar devices must not be used in the laboratory at any time.

* Please note that we only allow laboratory coats to be labelled with your name (front and back). Anyone with anything else on their coats will be required to replace it at their own cost.

9.3 Other safe laboratory practices (including fume cupboards)

Working safely is mostly about applying your common sense and knowledge to your work. While Most of the statements below are common sense always remember that if you understand what you are doing you will have a better chance of doing it safely and effectively. Be prepared when you come to the laboratory and think while you are doing you work.

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• Do not eat or drink or use mobile phones in the laboratory;

• Do not undertake practical work unless a member of staff is present;

• If you have an accident of any sort you must immediately inform the laboratory staff regardless of how minor the incident might have been;

• Never leave naked flames unattended and only leave apparatus that is under vacuum unat-tended with the approval of your supervisors;

• Make sure that you keep all communal areas clean and tidy, e.g. balances, instrument rooms, melting point apparatus, computer workstations;

• All waste chemicals and solutions must be disposed of according to the guidance provided;

• When the practical work has been completed make sure all apparatus that has been used has been cleaned and that your work area is clean and tidy.

Fume cupboards (f/c) are used to minimise a chemist’s exposure to harmful vapours. You will of-ten be using them during the practical course particularly when synthesising inorganic or organic materials. Some general guidelines for their proper use are outlined below.

• When not using the f/c make sure that the sash front is pulled down to its lowest point.

• When using the f/c work with the sash front as low as possible without compromising your mo-bility.

• If the air flow alarm on your f/c goes off, stop working, lower the sash front and make sure a member of staff knows of the problem.

• Do not allow too much clutter to build up in your f/c – it interferes with the airflow through it and increases the risk of vapours escaping through the front of the f/c.

9.4 Disposal of waste materials

From the environmental, financial and Health and Safety perspective waste disposal should be kept to a minimum. Where disposal is essential in the laboratory environment it is crucial that dif-ferent classes of materials are disposed of in away that is considerate of the risk to the person dis-posing of them and the person who will be dealing with the disposed item.

Paper and cardboard There will be a labelled location to collect this material for recycling

Uncontaminated combustible waste

Gloves, tissues, scraps of paper etc. should go in the bins under the sinks

Solid waste Dispose of with care using the methods described in the manual

Organic solvents All non-aqueous solvents must be disposed of into the appropriate sol-vent waste container, not down the sink.

Aqueous waste Unless otherwise specified in your experimental details this may be dis-posed of down the sink with dilution using tap water.

Broken glassware Must be decontaminated (if necessary) and disposed of in the appropri-ately labelled containers. Glassware for disposal must not go into any other container.

TLC plates and capil-laries

There will be dedicated, labelled containers for the disposal of these ma-terials.

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Careless disposal of waste from experimental work is dangerous to you and those around you. If such practice is noted it will impact on the assessment of your laboratory skills and, if sufficiently serious, lead to a formal warning regarding hazardous practice that would be recorded in your stu-dent record.

9.5 Segregation of ‘clean’ and ‘dirty’ work areas

In a laboratory environment ‘clean’ means an area where chemicals are not in use and ‘dirty’ means an area where the experimental work is being carried out. There are strict rules that must be observed to ensure that contamination of a ‘clean’ area does not arise from work done in a ‘dirty’ area.

You must not carry chemicals into, or wear laboratory coats in, a clean area. All computer suites in the School of Chemistry are clean areas and the main stairwell and access corridors in the School are ‘clean’. You will be shown how to get from the teaching laboratories to other work spaces via ‘dirty’ corridors when the need arises.

Within a working laboratory you must also be considerate to avoid contamination. Most particularly you must not use a keyboard interface (or other instrument controls) with gloves on.

9.6 Risk assessment during the laboratory courses

It is a legal requirement that all experimental work is assessed to determine the risk associated with it. The purpose of the assessment is to ensure that risks are minimised to a level where they are judged to be acceptable.

The experiments that you are doing have had an overall risk assessment completed by your labor-atory manager. However, as the person doing the work you will need to undertake your own as-sessment too. Clearly this has to happen before you start the experimental work. You have more time for the actual experiment is, if this is done before coming the laboratory class.

Some of the key terms (and some useful weblinks) involved in risk assessment are described be-low:

Hazard The way in which a material or a process could cause harm to a user, their colleagues or their environment.

Risk The likelihood that the potential hazard associated with a material or a pro-cess would become reality.

Control measure The method(s) applied to ensure that the risks associated with using a mate-rial or a process are minimised to an acceptable level.

Risk factors Any factor that might impact on risk: for example the work environment, the skill of the operator, equipment, substance, and scale characteristics.

Risk assessment An assessment which identifies control measures that minimise the risk as-sociated with the collective hazards of materials and processes.

Risk and Safety phrases

These can still be found in outdated documentation. Since 2014 these have been replaced by Hazard statements, Precautionary statements and signal words. A table is available in the labs and on Blackboard. H and P numbers on MSDS and in scripts refer to these statements.

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Material Safety Data Sheets (MSDS)

A summary of the physical properties and hazards associated with the named chemical, including all hazard and precautionary statements. Copies are available in the laboratory.

Workplace Expo-sure Limit (WEL)

WELs define limits which are legally binding describing the maximum amount of a specific chemical acceptable in the environment of any workplace.

10 Your laboratory work Completing laboratory work is only one part of the overall experimental process. Before you do any experimental work there is a planning and preparatory stage. This includes learning about the the-ory underlying the experiment that you are doing, planning how you are going to use your time in the laboratory and learning about how to control the hazardous nature of your work (see Section 9). Over the duration of your practical courses you will develop skills in all these areas.

You also need to be able to communicate effectively what you have done during your experiment, both verbally and in writing. This course concentrates on helping you record and communicate your results in writing, although talking about your work will be an informal part of every lab session.

10.1 Pre-labs

Each experiment will have a set of resources including readings, videos, exercises and quizzes that you must complete before attending the associated laboratory session. Some of these activi-ties will be assessed and this assessment will count towards your final mark for this course.

The deadline for the completion of the assessed prelab elements is midnight on the day before your experiment starts. Access to the resources will be maintained throughout the course.

A summary of the pre-lab requirements and assessment criteria for the two labs is given below:

LEVEL 4 LABORATORY LEVEL 5 LABORATORY

Semester 1 Practical 1

Read the script; watch the associated videos and record rele-vant notes from them.

A copy of the notes you have made must be submitted before the end of the day of the practical session. The utility of these notes will be assessed and will count as your pre-lab mark.

Read the script; watch the asso-ciated videos; complete the associated quiz.

Assessment will be based on the quiz result.

Semester 1 Practical 2

Read the script; watch the associated videos; perform the preparation exercises as detailed in the lab script.

Pre-lab will not be assessed.

Semester 1 Practicals 3-5

Read the script; watch the associated videos; complete the associated quiz.

Assessment will be based on the quiz result.

Semester 2 All Practicals

Read the script; watch the associated videos; complete the associated quiz.

Assessment will be based on the quiz result.

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10.2 Your laboratory notebook

One of the most useful skills to acquire in the laboratory is the proper use of a laboratory notebook. Notebooks, or other formally kept records, are an essential tool in many careers and the effort in-vested in developing good habits of notebook use will be amply repaid for those who pursue a fu-ture in any basic or applied sciences.

A laboratory notebook should be legible, and data in it should be readily accessible, clearly labelled with units, and grouped in a logical way. The ultimate goal of a laboratory notebook is to provide a permanent record of all the information necessary for another person (who is an experienced sci-entist) to reproduce your experiment and replicate your results.

Key features of laboratory notes are as follows:

1. It must be kept up to date throughout your practical sessions, written in ink and any mis-takes must be ruled out clearly (do not use correction fluid or scribble things out illegibly).

2. Each new practical must start on a new page and begin with your name, the date and an in-formative title.

3. The record should be in the 3rd person past tense.

4. A short description of the experiment – this might be a reaction scheme or a short state-ment of the aim.

5. The procedure, which outlines how the experiment was done, should include key observa-tions made during the experiment, and cite the exact quantities that you used. This must be written as you perform the work, i.e. it is a record of what was actually performed.

6. For instruments or in-house built apparatus record the settings used but not the operating instructions. When data is saved electronically, the filename and location must be listed and it should be clear what data is contained in the file.

7. Ensure that data includes units and is quoted to an appropriate number of significant fig-ures. When required to assess errors (this will be specified in the lab script) they should be estimated whilst the lab work is being performed and recorded next to the associated data.

8. All data that you collect during the experiment needs to be recorded in a legible format – (never record data on scraps of paper to be included later!).

Note: Further details on keeping a lab book will be covered in the morning sessions for your first practical in each lab. You must submit your Lab-book on the day of the practical – Failure to do so will result in you receiving a mark of zero for it.

10.3 Interim Reports – Level 4 Lab Only These are a requirement for some of the Level 4 experiments only. The experiments for this lab are designed so that the practical element will be finished before 18.00. The remaining time is allo-cated for completion of part of the analysis and generation of an Interim Report.

The specifics of what needs to be included in the interim report are detailed in the script for each practical. Note that if you are not explicitly asked to supply an error estimate for a value, you do not need to cite it in your interim report.

Interim reports can be written on loose paper or on a computer – They must not be recorded in your lab book. You can also ask for them to be assessed multiple times (only the final assessment

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will count towards your mark). Interim Reports need to be submitted before 18.00 of the day you performed the practical – Failure to do so will result in you receiving a mark of zero for it.

10.4 Laboratory notebook assessment – Level 5 Lab & Some Level 4 experiments Laboratory notes, recorded only in a lab notebook, are an actual record of your risk assessment(s), chemistry details, executed procedures, observations and results. For any acquired data you must record the source/name and location of the original file. Spectra must carry your name and indic-tate which compound/sample they represent. You must present your notes for assessment to an academic staff member during the laboratory opening times. Manage your time in the laboratory such that you can present the notebook in good time, allowing for some waiting time/queueing and the actual assessment. It is your responsibility to present your book early enough for assessment to finish by 18:00. Assessment will stop at this time and notes not assessed will receive a mark of zero.

10.5 Laboratory reports Most of your experiments will require that you complete a report on your work that is in a distinct from. These reports will often require that you apply some of your theoretical knowledge to the practical results. Each individual experiment will have specific requirements for the laboratory re-port and these will be described separately. However, ALL reports should be considerate of the following:

• Your report must be submitted in advance of any submission deadline. Penalties will be applied if it is not.

• Laboratory reports must be submitted via Turnitin on Blackboard – only a single file in PDF format will be accepted.

• Laboratory reports must be typed using word processing software. Handwritten accounts are not accepted.

• During the course of this practical you will reproduce graphs, equations and chemical struc-tures. Over time there is an expectation that relevant software is used. However, a neat scan of well presented data imported to the main text document is acceptable.

• The file size must not exceed the limits of Turnitin – currently 10MB, but this may change at the discretion of Turnitin.

• Reports must have been submitted by 23:59 on the day before your next practical, or by 23:50 one week after your last practical. Example: Practical day is Monday, then the report is due latest the following Sunday 23:59.

• Laboratory reports must be written in the third person past tense.

• Reports should be word processed, with the proviso that reaction mechanisms, drawings, equations and calculations can be neatly written by hand.

• Reports must be concise – short without omitting relevant details.

• The presentation of the report will contribute towards its grade.

The body of a laboratory report should be as follows:

• The header has to be an informative title and has to include your name, university username AND full student ID number.

1. AIM This should be a single sentence stating the primary goal of the practical.

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2. INTRODUCTION a) For L4 lab reports the Introduction should consist of a short description of the experiment. This can include a summary of the main objectives or details of the principles behind the practical. The Introduction should be no more than a couple of paragraphs long. b) For L5 lab reports describing a synthesis the introduction takes the form of a scheme with a balanced equation including relative molecular masses for all starting materials and products. Details of the principles or main objectives may be stated. The introduction should be no more than one paragraph long. NOTE: if a practical consists of more than one experiment (synthetic step), the “Introduction”, “Experimental Procedure” and “Results and Discussion” must be composed for each reaction separately.

3. EXPERIMENTAL DETAILS / PROCEDURE This section must not be copied from the lab manual and should be written in prose/paragragh form – Not as a numbered list or as bullet points.

a) For L4 lab reports the experimental procedure should be a concise account of the meth-ods and procedures used in the practical, in sufficient detail for an experienced scientist to reproduce the experiment. Exact amounts used should be cited along with pertinent obser-vations. Any portions of the procedure that you were required to devise yourself, should be covered in greater detail. Include instrument settings but not the instrument operating in-structions. NOTE: If the same procedure was performed multiple times (i.e. on a number of different samples), then a general procedure should be included in this section, with exact quantities and observations for each individual run recorded as a table in the “Results & Discussion” section. b) For L5 lab reports covering synthesis based practicals describe the experimental proce-dure as you performed it, including the exact amounts and molar quantities that you used. This section typically does not include details of the apparatus setup / equipment used.

4. RESULTS and DISCUSSION a) For L4 lab reports begin this section by (neatly) presenting raw data. The remainder should be organized to follow the analysis and answer the questions outlined in the “Analy-sis and questions” section of the script. Relevant equations and calculation results should appear, but intermediate calculations (showing your working) should not. Note that answers should be phrased so that the reader does not need to see the question to understand the answer. b) For L5 lab reports this section includes analyses (if applicable), the actual results (includ-ing the %-yield based on the limiting reagent), and all observations. Relevant calculations appear. Spectroscopic data (acquired and provided data) are presented here (unless di-rected otherwise in the lab manual, e.g. as part of a question) in tabulated form with a cor-responding structure on top of each table (additional guidelines on how to present spectro-scopic data will be provided on Blackboard and the tutored morning sessions). The results and data are then discussed, i.e. interpreted and evaluated.

5. CONCLUSION (and RECOMMENDATIONS) Begin by stating whether the aim of the practical was achieved. If it was not cite the likely reasons for this. Follow this with statements of the key results or values obtained. a) For L4 lab reports, recommendations should make suggestions to improve either the ex-periment or results and should also include answers to questions that the practical script indicates should appear here. b) For L5 lab synthesis-based reports recommendations and numerical values should not to be cited. The general summary must be kept scientifically.

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6. APPENDIX a) For L4 reports sample calculations (including intermediate calculations), error treatment and values obtained (that demonstrate your working) should be included here. Remember to include units throughout the calculations and demonstrate unit conversions. For each type of calculations performed you only need to show your working once, although make sure the sample calculation you include is correct! b) For L5 reports answers to all questions feature after the conclusions (unless directed otherwise in the lab manual, e.g. directly related to a discussion topic). All acquired spectra should appear at the end of this section.

Note: For synthesis based reports (L5) the report (excluding spectroscopic tabulations and an-swers to questions) will typically not exceed 1 page per individual reaction. Further details on writ-ing a report will be covered in the morning sessions. These talks will also specify the minor differ-ences in the report requirements of the labs. These variations arise from the difference in the types of practical run in the two labs, and hence what their report emphasis is on.

The deadline for the submission of the Main Report is midnight one week after the practical started

and before the next practical day (see above). Late submission of reports will result in a reduction

of marks and reports more than five working days late will not be accepted (i.e. will receive a mark

of zero).

Reports can be submitted as soon as they are complete, in advance of the deadline. As outline

above submission is via Turnitin on Blackboard. Further instructions will be provided on Black-

board.