FACULTY OF SCIENCE SCHOOL OF CHEMISTRY

CHEM3041

ANALYTICAL CHEMISTRY

SESSION 1, 2009

Faculty of Science - Course Outline - 2009

1. Information about the Course
NB: Some of this information is available on the UNSW Virtual Handbook
1

Year of Delivery Course Code Course Name Academic Unit Level of Course Units of Credit Session(s) Offered Prerequisite Hours per Week Number of Weeks Commencement Date

2009 CHEM3041 ANALYTICAL CHEMISTRY SCHOOL OF CHEMISTRY RD 3 6 UOC S1 CHEM2041 2 X LECTURE + 4 X LABORATORY 12 10 March 2009

Summary of Course Structure (for details see 'Course Schedule')

Component
Lectures Lecture 1 Lecture 2 Laboratory Lab Option 1 Lab Option 2 TOTAL Special Details

HPW
2

Time
10 11 am 3 - 4 pm

Day
Tuesday Wednesday Friday Friday

Location
Chem Sci M11 ABS 232 Chem Sci 162 Chem Sci 162

4 9 1 am 2 6 pm

6 None

2. Staff Involved in the Course

Staff Course Convener Additional Teaching Staff Lecturers & Facilitators Role Name Prof D B Hibbert A/Prof G Moran Contact Details Room 134 Dalton b.hibbert@unsw.edu.au x 54713 Room M61Chem Sci g.moran@unsw.edu.au x 54642 Room 224 Dalton n.kumar@unsw.edu.au x 54698 Room 133 Dalton p.thordarson@unsw.edu.au x54478 Room 124 Dalton j.brophy@unsw.edu.au x 54660 Chem Sci 162 Consultation Times Friday 10 1

Dr N Kumar

Dr Pall Thordarson Tutors & Demonstrators Technical & Laboratory Staff Other Support Staff Dr J Brophy Ms B Litvak Mr B Ward

UNSW Virtual Handbook: http://www.handbook.unsw.edu.au/2006/index.html

3. Course Details
Course Description (Handbook Entry)
2

Description of the course from UNSW Handbook This course builds on students existing background in analytical chemistry to develop both theory and practice relating to the latest analytical techniques used in industry and research. The course covers method development, method validation and measurement uncertainty; theory, operation, instrumentation and applications for the major techniques in instrumental analysis, including separation techniques, mass spectrometry, hyphenated chromatography-mass spectrometry techniques, elemental atomic spectroscopy and mass spectrometry. There is a strong emphasis on practical experience.

Course Aims

Student Learning 4 Outcomes

The course covers the major instrumental techniques of analytical chemistry, from a theoretical and experimental viewpoint. Applications to problems in biological, medical, industrial and environmental fields will be discussed. Students will gain hands-on experience in all major techniques covered in the course. At the end of this course you should be able to describe the major techniques of instrumental analysis, their capabilities and limitations. You should be able to compare different instrumental techniques in terms of their analytical performance, sample introduction methods and susceptibility to interferences. Given an analytical problem, you should be able to propose solutions, including appropriate techniques and be able to evaluate their suitability for the particular problem. You will be able to define the term quality as it applies to analytical chemistry; give examples of good and bad analytical results and their impact on society; state the seven principles of valid analytical measurement; describe the international (SI) measurement system and identify national and international bodies that are concerned with quality. You will also be able to explain why an analytical method must be validated before use; state the difference between validation and verification; describe how a method validation program is set up; state the eight parameters that should be investigated in a method validation program. At the end of the laboratory program, you should have an understanding of the types of instrumentation used in the major instrumental analytical techniques covered in the course. You should be capable of setting up a routine method, carrying out calibrations and analyses, determining analytical figures of merit (such as detection limit, precision and dynamic range) and evaluating potential interferences and matrix effects.

Graduate Attributes Developed in this Course Science Graduate 5 Attributes

Select the level of FOCUS
0 = NO FOCUS 1 = MINIMAL 2 = MINOR 3 = MAJOR

Activities / Assessment

1. 2.

3. 4. 5. 6.

Research, inquiry and analytical thinking abilities Capability and motivation for intellectual development Ethical, social and professional understanding Communication Teamwork, collaborative and management skills Information literacy

3 3

Laboratory course. Extension experiments. / QA assignment/ Assessment of practical reports. Lectures and applied problems discussed in class. / Exam.

2 2 3 1

Throughout course. /Exam Write up of practicals. / QA assignment/ Assessment of practical reports. Laboratory course. / Assessment of practical reports.

Laboratory pre-lab questions / Mark for pre-lab/ QA assignment Other attributes Professional accreditation attributes
2 3 4

None
RACI membership of professional body See http://www.raci.org.au/

UNSW Virtual Handbook: http://www.handbook.unsw.edu.au/2006/index.html Learning and Teaching Unit: http://www.ltu.unsw.edu.au Learning and Teaching Unit Learning Outcomes: http://www.ltu.unsw.edu.au/ref4-2-1_outcomes.cfm 5 Faculty of Science Science Graduate Attributes: http://www.science.unsw.edu.au/guide/slatig/sciga.html

Level of Material Delivered

[ ] Introduction to material [x] Emphasised and taught in depth [ ] Reinforced and additional expertise [ ] Competencies applied Quality assurance in the analytical laboratory. Quality control methods; method validation.

Major Topics (Syllabus Outline)

High-performance liquid chromatography (HPLC), instrumentation required, separation techniques, detectors used, and applications. Solid-phase extraction. Ion analysis; ion chromatography and capillary electrophoresis. Flame and electrothermal atomic absorption spectroscopy, cold vapour mercury and hydride generation techniques, inductively-coupled plasma atomic emission spectrometry (ICP-AES). Introduction to elemental mass spectrometry; ICP Mass Spectrometry. Mainstream analytical mass spectrometric principles and methods: Introduction to mass spectrometry; Instrumentation; Mass Spectrometry with volatile compounds GC/MS; Mass spectrometry with involatile compounds including biomolecules LC/MS and MALDI; Quantitative mass spectrometry, Tandem mass spectrometry (MS/MS)

Relationship to Other Courses within the Program

The course is a mainstream chemistry course that integrates with other level three course and with the honours year.

4. Rationale and Strategies Underpinning the Course

Rationale for learning and 6 teaching in this course , i.e., How this course is taught? Teaching Strategies The integration of lectures and laboratories supports Engaging 1. Effective learning is supported when students are actively engaged in the learning process. 2. Effective learning is supported by a climate of inquiry where students feel appropriately challenged and activities are linked to research and scholarship. Examples from chemical practice allow Contextualising 6. Students become more engaged in the learning process if they can see the relevance of their studies to professional, disciplinary and/or personal contexts. We also have undertaken Designing to 10. Clearly articulated expectations, goals, learning outcomes, and course requirements increase student motivation and improve learning. 12. Graduate attributes - the qualities and skills the university hopes its students will develop as a result of their university studies are most effectively acquired in a disciplinary context. Teaching in the use of laboratory groups supports 14. Learning cooperatively with peers rather than in an individualistic or competitive way may help students to develop interpersonal, professional, and cognitive skills to a higher level. How the assessment supports and assists the learning Timely feedback and marking of practical reports allows students to follow the thread of the course. The examination brings together the strands to complete the learning experience.

LTU Teaching Philosophy: http://www.ltu.unsw.edu.au/ref3-3-5_teaching_portfolio.cfm#philosophy

5. Course Schedule
Week Week 1 Lectures (day), Topics & Lecturers Tuesday, Wednesday Mass Spectrometry Tuesday, Wednesday Mass Spectrometry Tuesday, Wednesday Mass Spectrometry Tuesday, Wednesday Chromatography Dr Kumar Tuesday, Wednesday Chromatography Dr Kumar Tuesday, Wednesday Chromatography Dr Kumar Tuesday, Wednesday Chromatography Dr Kumar Tuesday, Wednesday Elemental analysis A/Prof Moran Tuesday, Wednesday Elemental analysis A/Prof Moran Tuesday, Wednesday Quality Assurance Prof Hibbert Tuesday, Wednesday Quality Assurance Prof Hibbert Tuesday, Wednesday Quality Assurance Prof Hibbert

Some of this information is available on the Virtual Handbook and the UNSW Timetable .
Practical (day), Topics & Lecturers Data Analysis practical Gibson Computer laboratory. Dalton Ground Floor See roster (WebCT) Data Analysis report due Assignment and Submission dates (see also 'Assessment Tasks & Feedback')

Week 2

Week 3 Week 4 Week 5 Week 6 * Week 7 Week 8 Week 9 Week 10 Week 11 Week 12

See roster See roster See roster See roster See roster See roster See roster See roster See roster See roster Last date for practical submissions Practical reports due no more than two weeks after the experiment is done. Marked reports will be returned within two weeks of submission

*NB: As stated in the UNSW Assessment Policy: one or more tasks should be set, submitted, marked and returned to students by the mid-point of a course, or no later than the end of Week 6 of a 12-week session'

7 8

UNSW Virtual Handbook: http://www.handbook.unsw.edu.au/2006/index.html UNSW Timetable: http://www.timetable.unsw.edu.au/

6. Assessment Tasks and Feedback

Task % of total mark Assessment Criteria Release Date of Submission WHO Feedback WHEN HOW

9 Practical reports Examination

50

See below for detailed marking scheme Answers to questions given correctly. Discussion shows knowledge and understanding of the course.

Expected in week following experiment

Report assessor

Within 2 weeks of submission of report

Annotated report. Completed result sheet

50

This marking scheme will apply to the nine practical exercises you will be required to attempt (including the initial data analysis). The total mark for all practicals contributes 50% to the overall mark for the course. Compound Possible marks Total Pre-laboratory exercise Late submissions: One day late = subtract up to 5 marks. Zero for this section if handed in after 5 pm. 10 = all questions attempted in a reasonable manner, with less than 25% of answers wrong 7 = 50-74% answers correct 5 = 21-49% answers correct 3 = less than 20% answers correct but > 50% attempted 2 = less than 20% correct and 15-50% attempted. 1 = less than 15% attempted and more than 5% correct 0 = less than 5% Total for Pre-laboratory exercise 10

Flowchart Late submissions: If handed in at beginning of class = up to 3 marks. Zero for this section if not handed in 15 min after start of laboratory class. 5 = Satisfactory (no additions required) 3 = Requires some additions 1 = Unsatisfactory flowchart submitted 0 = No flowchart submitted Total for flowchart 5

Risk assessment Late submissions: If handed in at beginning of class = up to 3 marks. Zero for this section if not handed in 15 min after start of laboratory class. 5 = Satisfactory (no additions required) 3 = Requires some additions 1 = Unsatisfactory risk assessment submitted 0 = No risk assessment submitted Total for risk assessment 5

Report Due 1 pm on Friday 2 weeks after experiment is performed. For each day after that up to 10 marks (10% of total) will be subtracted (weekend days excluded)

Part 1 = Overall layout

10 = high quality layout, all sections included, laid out in a clear and

logical fashion 6-9 = Good layout that follows reasonably well the standard format with a clear flow of sections and only some minor flaws in formatting and the like 2-5 = Average layout, doesnt follow and/or skips the standard format and/or major formatting mistakes that make the report difficult to read 0-1 Poor quality layout of a report that makes it really hard to read Total for overall layout Section 1 Executive summary 15 = All key element of a good concise executive summary included, neatly formatted and without any errors 11-14 = Good executive summary with only 1-3 minor flaws (spelling, grammar, layout and the like). All key results included. 6-10 = Satisfactory executive summary but either a number of minor flaws and/or some of the key results missing or poorly presented. 1-5 = Poor executive summary, major flaws, mistakes and/or a number of results omitted. 0 = Executive summary missing or contains no valuable information (e.g., just the heading) Total for executive summary 15 10

Section 2 Introduction and methodology

15 = Short quality introduction and methodology. It should give a brief description of the technique and methods used, the sample(s) analysed, how the unknown was determined (e.g., from a calibration curve) and

the method(s) to determine uncertainties. 10-14 = Good introduction with only some minor flaws such as being a bit long or not covering well one of the key components of an introduction and methodology section 4-9 = Average introduction, either too long or too short and/or containing a number of important omission and flaws 1-3 = Unsatisfactory introduction and methodology that lacks most of the content expected from a good introduction and methodology 0 = Introduction and methodology missing or contains no valuable information (e.g. just the headings). Total for introduction and methodology 15

Results and Discussion

27-30 = High quality results and discussion: all the results are clearly reported, reasonably within the expected values, uncertainties included and correctly calculated, uncertainty determination well explained/demonstrated with an example, significant figures correct, easy to follow how results have been obtained from raw data (e.g., by graphs and the attached excel file). Discussion brief but demonstrates insight into the quality of results obtained, what could be improved, what may increased the uncertainty. Only at most 1-3 minor errors (e.g. typos) 20-26 = Good quality results and discussion that contains most of the above sections expected but with 1-2 significant deficiencies such as flaws in uncertainty calculations, significant figures mistakes, values out of range (e.g. due to a factor of 1000 error) and/or discussion that lacks

insight 11-19 = Average Results and discussion that includes the key components but has a number of significant mistakes, results out of range or omissions. 1-9 = Poor quality Results and discussion section with significant sections completely missing and/or incorrect, e.g. not showing any uncertainties, no discussion, not including an excel spreadsheet. 0 = Missing results and discussion or no information included (e.g., just the headings. Total for Results and discussion 30

Questions Each experiment has at least two questions. All questions have the same weight.

10 = All questions answered correctly and concisely, demonstrating full understanding of the topic(s) covered. 5-9 = At least half of the questions answered correctly 1-4 = Less than half of the questions answered correctly 0 = No correct answers provided to the questions give

Total for questions

10

Grand total
!

100

7. Additional Resources and Support

Text Books Principles of Instrumental Analysis by Douglas A. Skoog and Stanley R. Crouch ISBN 0495012017 - EAN 9780495012016 - Sell ISBN 0495012017 th Brooks Cole Hardcover 1080 pages, 6 Edition 2006 or Skoog, Holler, & Nieman, "Principles of Instrumental Analysis", 5th Edition, Saunders College Publishing, 1998. P 543.08/5 P P 543.08/5 S P 543.08/5 U Course Manual Printed laboratory manual including guides and other material available from the University Bookshop All material is on WebCT Quality Assurance in the Analytical Chemistry Laboratory, D B Hibbert, Oxford University Press, New York, (2007) P 543.028/2 Data Analysis for Chemistry : An Introductory Guide for Students and Laboratory Scientists, D. Brynn Hibbert and JJ Gooding, Oxford University Press, New York, (2006) P 540.72/20 Others will be distributed by individual lecturers Recommended Internet Sites Societies

Required Readings Additional Readings

See WebCT site Royal Australian Chemical Institute http://www.raci.org.au/ Students of Chemistry Society (UNSW) http://www.chem.unsw.edu.au/schoolinfo/socs.html Laboratory Chemical Sciences Building 162 Gibson Computer laboratory Ground floor, Dalton Building

Computer Laboratories or Study Spaces

8. Required Equipment, Training and Enabling Skills

Equipment Required Enabling Skills - training which maybe required to complete this course Laboratory coat, safety spectacles, closed shoes OH&S briefing Awareness of School plagiarism guidelines

9. Course Evaluation and Development

Student feedback is gathered periodically by various means. Such feedback is considered carefully with a view to acting on it constructively wherever possible. This course outline conveys how feedback has helped to shape and develop this course. Mechanisms of Review Course Review Last Review Date 2008 Comments or Changes Resulting from Reviews

The practical component of the course has been reviewed, particularly the manual, write up, and marking schemes. As a result of student feedback a more detailed marking scheme for each practical has been devised (see section 6) As a result of student feedback we agreed to implement the following The laboratory manual will be completely re-written. Re-write experiments with clearer focus on what we want you to do. Providing template for write up Try and coordinate marking schemes (make staff produce a marking scheme) Make what marks are given for results clearer. Re-write statistics appendix and make it apply to all experiments. First laboratory period to be a workshop on errors and uncertainty. Using Excel show how to calculate measurement uncertainty for selected experiments with previous years data. Make some practicals 3 hours with tutorial preceding. We will drop the Flame-AAS and IR in favour of the data analysis workshop and a ESI-MS experiment. We like the idea of prelabs and will bring them into WebCT to be completed before the laboratory on line. They will attract some marks. All laboratories in chemistry will have to do Risk assessments. Again these might be completed and checked on line.

CATEI

2008

Student Focus Group Other

none none

Science CATEI procedure: http://www.science.unsw.edu.au/guide/slatig/catei.html

10. Administration Matters

Expectations of Students Workload Contact hours are 6 per week, in weeks 2 - 13 and 2 hours per week in weeks 1,14. The major out-of-class workload is associated with the laboratory program. Pre-laboratory work is expected to take 30-60 minutes per week and post-laboratory write-up is expected to take 3-4 hours per week. Laboratory reports should be submitted to Ms Litvak in Chemical Sciences 165B. A cover sheet should be completed and an dated acknowledgement received. See http://www.chem.unsw.edu.au/coursenotes/CHEM3041/ or WebCT for down-loadable cover sheets Information on relevant Occupational Health and Safety policies and expectations at UNSW: www.riskman.unsw.edu.au/ohs/ohs.shtml School of Chemistry OH&S policy and requirements see laboratory manual and WebCT. To be admitted to a laboratory, you must wear safety glasses, a lab coat and covered shoes (no thongs, open sandals or clogs). You must also complete all safety pre-lab work, risk assessment or other prescribed preparation relating to carrying out safe laboratory work. Visitors are not allowed to undergraduate laboratories without the permission of the lab supervisor. Note a risk assessment must be completed before any laboratory work can be done. Examination Procedures Candidates for CHEM3041 must demonstrate a satisfactory performance in both laboratory work and the written examination. A mark of fifty percent is regarded as the minimum acceptable performance in the laboratory. Students who do not attain this mark in their laboratory work may not be awarded a pass in the subject irrespective of their performance in the examination. Laboratory reports, laboratory notebooks and satisfactory completion of pre-laboratory assignments all contribute to the final laboratory mark. Full details of expectations are given in the introduction to the lab manual and section 6 of this outline.

Assignment Submissions

Occupational Health and 10 Safety

Equity and Diversity

Those students who have a disability that requires some adjustment in their teaching or learning environment are encouraged to discuss their study needs with the course convener prior to, or at the commencement of, their course, or with the Equity Officer (Disability) in the Equity and Diversity Unit (9385 4734 or www.equity.unsw.edu.au/disabil.html). Issues to be discussed may include access to materials, signers or note-takers, the provision of services and additional exam and assessment arrangements. Early notification is essential to enable any necessary adjustments to be made. Information on designing courses and course outlines that take into account the needs of students with disabilities can be found at:
www.secretariat.unsw.edu.au/acboardcom/minutes/coe/disabilityguidelines.pdf Grievance Policy
11

School Contact Dr Gavin Edwards Director of Teaching g.edwards@unsw.edu.au Tel: 9385 4652

Faculty Contact Dr Noel Whitaker Associate Dean (Education) n.whitaker@unsw.edu.au Tel: 9385 7930

University Contact University Counselling Services Tel: 9385 5418

10 11

UNSW Occupational Health and Safety: www.riskman.unsw.edu.au/ohs/ohs.shtml UNSW Grievance Policy: http://www.infonet.unsw.edu.au/poldoc/student_grievance_resolution.pdf

11. UNSW Academic Honesty and Plagiarism

What is Plagiarism? Plagiarism is the presentation of the thoughts or work of another as ones own. *Examples include: direct duplication of the thoughts or work of another, including by copying material, ideas or concepts from a book, article, report or other written document (whether published or unpublished), composition, artwork, design, drawing, circuitry, computer program or software, web site, Internet, other electronic resource, or another persons assignment without appropriate acknowledgement; paraphrasing another persons work with very minor changes keeping the meaning, form and/or progression of ideas of the original; piecing together sections of the work of others into a new whole; presenting an assessment item as independent work when it has been produced in whole or part in collusion with other people, for example, another student or a tutor; and claiming credit for a proportion a work contributed to a group assessment item that is greater than that actually contributed. For the purposes of this policy, submitting an assessment item that has already been submitted for academic credit elsewhere may be considered plagiarism. Knowingly permitting your work to be copied by another student may also be considered to be plagiarism. Note that an assessment item produced in oral, not written, form, or involving live presentation, may similarly contain plagiarised material. The inclusion of the thoughts or work of another with attribution appropriate to the academic discipline does not amount to plagiarism. The Learning Centre website is main repository for resources for staff and students on plagiarism and academic honesty. These resources can be located via: www.lc.unsw.edu.au/plagiarism The Learning Centre also provides substantial educational written materials, workshops, and tutorials to aid students, for example, in: correct referencing practices; paraphrasing, summarising, essay writing, and time management; appropriate use of, and attribution for, a range of materials including text, images, formulae and concepts. Individual assistance is available on request from The Learning Centre. Students are also reminded that careful time management is an important part of study and one of the identified causes of plagiarism is poor time management. Students should allow sufficient time for research, drafting, and the proper referencing of sources in preparing all assessment items.
* Based on that proposed to the University of Newcastle by the St James Ethics Centre. Used with kind permission from the University of Newcastle Adapted with kind permission from the University of Melbourne.

The School has also produced a guide for students in chemistry courses, including examples of acceptable and unacceptable conduct, guidelines on avoiding misconduct in laboratory contexts and examples of acceptable referencing procedures for essays and literature reviews. This guide is available at http://www.chem.unsw.edu.au/coursenotes/plagiarism/Plagpolicy.03.pdf and is reproduced where appropriate in course manuals and on course websites.