Spring 2014 CHEM- 458 Inorganic Chemistry Laboratory Thurs 6:00 10:00 PM or Fri 1:00 5:00 PM (QDH 318)

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1 Spring 2014 CHEM- 458 Inorganic Chemistry Laboratory Thurs 6:00 10:00 PM or Fri 1:00 5:00 PM (QDH 318) Instructors: Prof. Joel Rosenthal TA: Tian Qiu Web: Office: BRL 034 BRL 007 Office Hours: By Appointment By Appointment REQUIRED MATERIALS Packet of Inorganic Lab Procedures Website: /Chem458_2014.html COURSE INFORMATION This course will serve as an introduction to the synthesis and characterization of inorganic compounds. Students will be exposed to a diverse set of synthetic methods and a wide range of characterization techniques in order to learn about the molecular and electronic structure of inorganic and organometallic complexes. The main objectives of this laboratory course include: 1. Illustration of some of the principles of inorganic chemistry 2. Training in the techniques of inorganic chemical synthesis 3. Training in the presentation of experimental data and discussion of experimental findings 4. Training in the use of scientific reference materials for the interpretation and discussion of experimental results 5. Development of a research attitude and skill set The experiments in this course have been selected to provide you an opportunity to become familiar with advanced and air- free synthetic techniques. These experiments will also emphasize several physical methods along with their use in elucidating the structure and electronic properties of inorganic compounds. Finally, these experiments highlighted have been designed to help you understand how experimental observations can be correlated with data and theory, while allowing you to develop a appreciation for and interest in inorganic chemistry and synthesis. COURSE ORGANIZATION We will perform four different two- week experiments in this course. These four experiments are but a few of the many, which could have been chosen for this course. Inorganic chemistry is a diverse field that has expanded rapidly to include a wide array of topics, ranging from the traditional study of main croup and transition metal coordination compounds, to the areas of organometallics and bioinorganic chemistry.

2 The experiments that will be conducted during this lab course are as follows: Lab 1: The Synthesis and Characterization of Some Coordination Compounds of Nickel A study of coordination compounds and the determination of structure from magnetic susceptibilities and optical absorption spectroscopy. Lab 2: The Synthesis and Characterization of [Mo(CO) 4 (piperidine) 2 ] and its Triphenylphosphine derivatives A study of the reactivity of a transition metal carbonyl and an introduction to the use of physical methods to obtain structural information. Lab 3: Preparation and Properties of Ferrocene A study of an organometallic sandwich compound and the effect of a metal on reactivity and properties of an organic ligand Lab 4: Preparation and Properties of Cobaloximes: Vitamin B 12 Model Compounds A study of an inorganic coordination complex useful as a model to illustrate the unconventional properties of Vitamin B 12. COURSE SCHEDULE AND PREPARATION Two weeks have been allotted for each experiment in this course. Adequate preparation before coming to lab is necessary to make the most effective use of each 4 hour lab period and ensure the safety of all working in the lab. Each lab has been planned and organized so that each student will have to answer questions about the experiment and interpret data obtained in the laboratory. You are urged to become familiar with the literature of inorganic chemistry and should consult it when answering the questions associated with each lab experiment. The use of reference books is allowed, but should not serve as a substitute for the performance of all laboratory exercises. The experimental procedures, protocols and questions to be answered will be provided to you at the beginning of this course and should be studied thoroughly prior to starting work in the laboratory. Laboratory Schedule Week of 3/3 Week of 3/10 Lab 1 Week of 3/17 Week of 3/24 Lab 2 Week of 3/31 Spring Break Week of 4/7 Week of 4/14 Lab 3 Week of 4/21 Week of 4/28 Lab 4

3 LABORATORY SAFETY The Right to Know Law states that you have the right to be informed of any risks associated with your work in this laboratory. To understand the general risks and hazards involved in working with in a lab environment with common glassware, solvents and chemicals, all students should read the Safety & Right- to- Know Training for Students (distributed in class and available on course website) and MUST complete "Basic Right- To- Know Safety Training for Undergraduate Teaching Laboratory Students". This online training course can be accessed at: Students must successfully complete the online quizzes associated with this course and print out the certificate that demonstrates they have mastered this safety information. Each student must present this certificate before entering the lab to begin conducting experiments. Without the proper preparation and attention to detail, chemistry experiments can be dangerous. Moreover, most chemicals have some level of toxicity associated with them and no student is immune to accidents. Every experiment in this course carries with it some element of danger; if you do not feel that you have the time, facilities or proper level of preparation to do an experiment with the appropriate level of caution and care, then DO NOT CONDUCT THE EXPERIMENT. In general, when uncommon chemicals or pieces of laboratory equipment are used in an experiment, the laboratory protocol will indicate extra precautions, which might be needed. MSDS sheets detailing the physical properties and potential physiological effects of all the chemicals used in this course are on file and may be examined at any time. In general, before you work with a chemical for the first time, it is good practice to refer to reference information that details what kind of extra precautions, if any, might be needed. The following safety precautions should always be taken: 1. Goggles must be worn properly at all times whenever a chemical or eye hazard is present. For reasons of fairness and personal hygiene, the department cannot loan goggles. There must be no exceptions to everyone in the lab wearing goggles when any hazard is present. This begins when anyone in the lab starts gathering equipment or chemicals. The ONLY TIME that it is acceptable to not wear personal protective equipment in the teaching laboratory is during a pre- lab quiz in which there are no hazards present. It is the responsibility of the TA to insure that no lab work begins until all students have put on their personal protective equipment. 2. There are no exceptions to the above rule. If a student is found working in the lab without proper eye- protection, that student will be expelled from the lab and receive a failing grade for the experiment in progress. 3. Lab appropriate clothing must be worn by students in the laboratory. Exposed skin from the neck down should be minimized following the guidelines in the Safety & Right- to- Know Training for Students. 4. Be sure that you know the location of all safety equipment (eye washes, safety shower, fire extinguishers, etc.) and learn what to do in the event of a fire, a chemical spill or exposure before you begin any experimental work. 5. No variations to the experiments as written may be performed without the explicit approval of the instructor. 6. If a student comes to lab unprepared to conduct an experiment in a cautious and careful manner it represents a hazard for all students in the class. Students that are unprepared for a given experiment may be dismissed from that lab session. 7. BE CAREFUL when handling chemical reagents. Avoid contact with your skin and inhaling vapors. Almost any chemical can be toxic if absorbed into the body in large enough

4 quantities. Proper experimental techniques, procedures and manipulations are critical to your safety and that of your classmates. If you are unsure of the proper manner in which to carry out a given experiment or manipulation be sure to check with the instructor or TA. 8. In the case of a spill, immediately inform the lab TA and follow the appropriate cleanup and disposal procedures. LAB NOTEBOOKS Orderly record keeping is essential in a laboratory as thorough record keeping greatly simplifies the task of writing lab reports. It also helps when trying to troubleshoot problems that may arise during an experiment. In an industrial setting or other professional research environment, a laboratory notebook is a legal record of research activities. Inventions and ideas that are not properly documented may not hold up in patent litigation. A portion of your Lab Report grade will be based on your lab notebook (see below). Some points to note are given below. LAB REPORTS 1. The laboratory notebook must be bound, not looseleaf. Your notebooks will be graded so your entries must be neat, legible and in pen. Copies of the relevant notebook pages must be turned in along with your report (see below). 2. Each page must be dated 3. Before you begin in the lab, write the title and a brief introduction/purpose statement on each page. Write out all reactions and determine molecular weights of all species to be used. 4. During the lab, record the laboratory procedure as you do them. Indicate actual amounts of reagents used (calculate number of moles, etc.), all observations and the results. 5. Your notebook should have printed number pages 6. Use tables for data when appropriate 7. Mistakes should be crossed out with a single line. Do not erase or use correction fluid. 8. Changes to procedures should be clearly noted 9. Note that you do not need to use complete sentences and you may use an outline format if you wish. Be sure to include all relevant information as a rule of thumb, someone else should be able to accurately repeat your work, using only your notebook as a guide. Lab reports are the written documentation of the work that you performed in the laboratory. An outsider skilled in chemistry should be able to read your report and understand what you did, why you did it and what you discovered. You will find that good written and verbal communications skills are keys to a successful career in the sciences. Note that each student is responsible for turning in their own lab report for each lab experiment. When writing your lab reports, envision yourself as graduate student writing up your research for publication in a journal. The lab report should be divided into logical sections following the outline discussed below. Details on what should be included in each section are listed. As with all scientific reports, it should be written in past tense (since you presumably are writing the report after you did the work) and with passive voice. You may find the ACS Style Guide to be a useful resource for scientific writing. Your reports should be prepared on a word processor and both spelling and grammar are important. Additional figures and calibration curves not included in the main lab report along with copies of your lab notebook should be added in an appendix. Be sure to label your figures and tables. Keep in mind that the reader may not be familiar with your experiment.

5 The following sections should appear in your lab reports. 1. Title Concisely describes lab content 2. Name Identify yourself 3. Abstract Conveys a sense of the full report concisely and effectively 4. Introduction Successfully establishes the context, objectives and purpose of the lab. Presents interesting questions or issues related to the lab. 5. Experimental Methods This section describes the physical work you did in the lab. You must provide enough detail to allow for your experiments to be replicated. 6. Results Opens with a few sentences describing the main findings of the lab presenting visuals where appropriate. The section should clearly and accurately present your experimental findings with sufficient support. You should include data tables of raw data where appropriate (see table 1 below), calibration plots and figures (spectra, diagrams etc.). This section should not contain an in depth discussion of what the results mean. 7. Discussion This section should be used to indicate the significance of your experimental results. An explanation of how the findings are linked to the context of the lab should be included. This section should also be used to address questions and issues related to the lab and discuss answers to these questions. 8. Conclusions Describes what has been learned by completing the lab experiments. 9. References All references should be listed as endnotes according to the American Chemical Society Style 10. Appendix Include a photocopy of your Lab Notebook pages for the experiment COURSEWORK AND GRADING Final grades for this course will be determined as follows: Laboratory Reports 20% Each Lab (80% Total) The reports will be due one week after the completion of the experiment. Late reports will be penalized 5 points for each day they are late. No lab reports will be accepted for grading after the last scheduled meeting of the lab. Laboratory Technique and Presentation 5% Each Lab (20% Total) This portion of the grade will be assigned by the TA based on preparation for and performance in the lab. REGRADING All requests for regrades must be submitted in writing within 24 hours of the material being returned. Please note, the entire lab report will be regraded; if grading errors are found the final grades may be higher or lower than the original score. Also note that photocopies may be made prior to returning lab reports. If answers are altered, it will be obvious, provable and reported to the UD Office of Student Conduct (see below). ACADEMIC INTEGRITY Academic dishonesty will not be tolerated in this class. Such behavior is unethical, creates a negative atmosphere and inhibits learning. This later point is most critical as the material covered in this course is critical to your education and may be important to your future career path. It is expected that you will learn the material covered in this course because you will need it to be a functional chemist. If you have any questions about this issue, please review the University of Delaware s Academic Dishonestly Policy:

6 LEARNING GOALS It is anticipated that upon completion of this course, students will be able to meet the following: Apply major principles and experimental findings in chemistry in the analysis and solution of a research problem Employ appropriate experimental and analytical methods in the collection and analysis and interpretation of data Carry out laboratory work using best practices of chemical safety and hygiene Work effectively as a member of a research team Understand and practice the ethically correct collection, representation and interpretation of data Present clear and concise reports in both oral and written formats HELPFUL REFERENCES 1. Inorganic Chemistry 4 th Ed, Shriver and Atkins 2. Inorganic Chemistry 4 th Ed, Huheey and Keiter 3. Basic Inorganic Chemistry 3 rd Ed, Cotton and Wilkinson 4. Advanced Inorganic Chemistry - 6 th Ed, Cotton, Murillo and Bochmann 5. Physical Methods for Chemists 2 nd Ed, Drago 6. Orbital Interactions in Chemistry, Albright, Burdett and Whangbo 7. Physical Inorganic Chemistry, Kettle 8. Organometallic Chemistry 2 nd Ed, Spessard and Miessler 9. The Organometallic Chemistry of the Transition Metals 3 rd Ed, Crabtree