Guidelines for Preparation of Laboratory Reports

Please refer to the Guide to Authors in the first issue of the year for Inorganic Chemistry for detailed instructions as to the preparation of a manuscript. This information can be obtained online from the ACS web server. This specific document is the guide to authors for Inorganic Chemistry. Your laboratory reports should take the form of a paper submitted for publication to Inorganic Chemistry. Copies of the ACS Style Guide are available in the Davidson stockroom to check out for assistance in the preparation of your reports. Reports should be typed or generated on a word processor. The departmental computer laboratory is available for your use in the preparation of these reports.

The cover page should include your name highlight somehow to indicate it is your report, your lab partner's name, your TA's name, the date the experiment was completed, the date the lab report was submitted and the signed VT Honor Pledge. Realize that an experiment is not completed until the characterization is done. All spectra should be included and labelled and presented as figures in Inorganic Chemistry format. This requires a figure number, a figure title and often a figure caption as all figures should be fully labelled so as to "stand alone." Tables also must be prepared in Inorganic Chemistry format with a table number, table title and must also be able to "stand alone." Your results section needs to present your synthetic chemistry with balance equations and important observations. All of your characterizational data should be reported in your results section one piece at a time and fully discussed in your discussion section. Remember you are charged with the task of proving to me you made the required compound.

Full Laboratory Reports will contain:

Abstract: A brief outline of what you accomplished in this experiment.

Introduction: This should include all relevant background information for your experiment, some historical data, particular uses for your compound or class of compounds, overall reactions, discussions of the characterizational techniques to be employed, etc.. It is very helpful to have this section of your laboratory report written prior to starting the experiment.

Good places to start looking for background information for your lab experiment and reports are textbooks and reference books covering inorganic chemistry/chemicals. We have provided some helpful information on the Reference Literature for Chemistry 4414 for your assistance. Please feel free to ask Prof. Brewer and your GTA for assistance with this important aspect of the laboratory course. It is often essential to look up papers cited by these references and textbooks.

Experimental: This part of the report gives the reader the details of what you did during your experiment including weights and volumes of reagents used, percentage yields, calculations need to be shown where applicable, instruments utilized to characterize your compounds, etc..

Results: Present your synthetic chemistry including balanced equations. Give all of your results and observations. Be sure to note color changes, crystal types, melting point, NMR, IR, UV-VIS (lambda max with extinction coefficients). Your report needs to include copies of the pertinent pages from your laboratory notebook. All characterizational data needs to be included as properly labeled figures or properly formatted tables.

Discussion: Discuss your synthetic chemistry highlighting important aspects. Identify your compound and prove that you made it. Give detailed explanations of your characterizational data with its interpretation relative to your proposed structure. Give explanations for low yields, i.e. what went wrong and why it affected your results. Discuss your results in the context of the available literature data.

Conclusions: Indicate your main conclusions highlighting that you have prepared the desired compounds. Suggestions for future improvement or future work are also included in this section.

References: You must cite properly all sources of information used in the preparation of your report.

How to reference the literature:
Journal Articles: Author's Last Name, Author's Initials Journal Name, Year, Volume, Pages.
Example: Bradley, P.; Suardi, G.; Zipp, R. J. Am. Chem. Soc. 1994, 116, 2859-2868.
Books: Authors Last Name, Authorís Initials Book Title, Publishers, Year Published, Pages.
Example: Cotton, F. A.; Wilkinson, G. Advanced Inorganic Chemistry, Wiley & Sons, 1972, 736-738.

Short laboratory reports will contain the Experimental, Results, Discussion, Conclusions and References sections only.

Sample Experimental Sections:

Sample experimental for the synthesis of ferrocene

Materials and Methods. All reactions were carried out under an inert atmosphere of nitrogen unless otherwise noted. Tetrahydrofuran (THF) was dried and distilled from Na/benzophenone before use. Cyclopentadiene was thermally cracked from its dimer before use. The chemicals FeCl₂.4H₂O, KBr, dicyclopentadiene, THF, and nBuLi solution were obtained from Aldrich. The FeCl₂.4H₂O, KBr, and nBuLi solution were used as received, without further purification. Deuterated chloroform was obtained from Cambridge Isotopes Laboratories and used without further purification.

¹H NMR spectra were obtained on a Bruker AM360 spectrometer as 1 mM solutions in CDCl₃. IR spectra were obtained on a Bomem 100 FTIR spectrometer using KBr pellets prepared by mixing ca. 1 mg of sample with 100 mg of KBr. Mass spectral data were collected on a Hewlett Packard 5988A MS instrument using electron impact ionization. Melting points were carried out in air using a meltemp.

Synthesis of Ferrocene, Fe(C₅H₅)₂. A solution of freshly cracked cyclopentadiene (10.0 mL, 0.122 moles) in distilled THF was deaerated with nitrogen and cooled to -78 °C. A solution of nBuLi (63 mL of a 2.0 M solution in hexanes) was added dropwise to the cyclopentadiene solution at -78 °C while still under nitrogen. After stirring for 30 min, a deaerated solution of FeCl₂.4H₂O (12.1 g, 0.0610 mol)in dry DMSO was added dropwise to the reaction mixture. After 15 minutes of stirring, the reaction was allowed to warm to room temperature. The solution was added rapidly to a 200 mL solution of ice in air. After stirring for 15 min, the orange suspension was filtered over a coarse fritted funnel. The crude orange product was spread on a watch glass, dried, and sublimed at room temperature yielding bright orange needles. Yield: 10.3 g (91%); IR (KBr, cm-1) ???? (s), ???? (m), ???? (vs); ¹H NMR (CDCl₃, delta, ppm) ?.??? (s, ?? H); mp ???-??? °C. MS (EI⁺, m/e) ??? (C₁₀H₁₀Fe⁺).

Sample experimental section for calculations

Computational Methods. All calculations were performed using CAChe Satellite 3.1 from Oxford Molecular on a PC client using an SGI server for calculations. The ligands were constructed and their geometry optimized by molecular mechanics (modified MM2). These were then used to build the [Mo(CO)₄(NN)] complexes. Geometry optimizations were performed using the molecular mechanics routine (modified MM2) utilized by CAChe. Molecular orbitals were calculated from the MM2 geometry using the Extended Huckel and ZINDO wavefunctions. Dipole moments were also calculated at the ZINDO level using the MM2 calculated geometry.