A. The Notebook. In real life the purpose of a laboratory notebook is to provide an accurate permanent record of exactly what was done and of what happened as a result. Often years pass between the performance of an experiment and the realization of the complete significance of the result. Obviously one's memory cannot be trusted to retain all the details of the work and the existence of a well kept record under such circumstances is imperative. The notebook is also essential if a patent is to be applied for.

Your lab notebook should be a clear record of how you performed your synthesis and of what happened. All difficulties you experienced, all modifications you made, and all suggestions for improvement you might make should be detailed. The notebook should be kept as work progresses, and not written up two weeks later. A number of notebooks of previous inorganic prep students are available and you are encouraged to consult them for a preview of difficulties and for suggestions and improvements when your synthesis has been done before (see the instructor for this information). Your notebook will be used for this purpose in the future.

Specific expectations for the notebook are:

* The notebook should be of the type that has duplicate pages with carbon paper between. This type of notebook is slightly more expensive but allows for the removal of the duplicate copy to serve as the report for the experiment, while you still have the notebook in your possession.

* The notebook should be clearly labeled on the outside.

* The first few pages should be reserved for an index.

* Each entry should include the date (written out to avoid confusion) at which it is entered into the notebook. Also include the time so that significant observations can be related to how long a reaction has been proceeding.

* The description of each preparation should include, before any part of that experiment is performed, the following items:

• A brief description of the purpose of the preparation including theory and the structure of the molecule being synthesized.
  
  
• Any references to the literature which have been utilized.
  
  
• MSDS sheets for each of the chemicals used.
  
  
• A brief description of the best synthetic route for preparing the compound, including special techniques, precautions, expected yield, physical characteristics and method of characterization.
  
  
• A list of the chemicals and items of equipment required, with quantities scaled to a suitable level.
  
  
• Any purification necessary for the solvents or starting materials before the reaction is begun.
  
  
• Drawing of apparatus to be used, if a special setup.
  
  
• The balanced chemical equation for the reaction to be carried out, with special conditions such as T, P, inert atmosphere, etc.
  
  
• Structure of starting material and product, showing proper bond angles and stereochemistry, if appropriate.
  
  

* A detailed description of the actual laboratory work is to follow. This should include diagrams of the apparatus utilized, balanced chemical equations representing the transformations to be carried out, and all observations, including spectra, and what you conclude from the spectra obtained. A well-written description will allow a reader to actually visualize what took place

* The final comments and conclusions should include:

• An identification of the purity of the product, as determined by physical or spectral properties. NMR spectral peaks should be labeled.
  
  
• The percent yield of the product obtained.
  
  
• A summary of the weaknesses of the preparation.
  
  
• Any suggestions for improvement in the procedure.
  
  

* Additional information on the laboratory notebook can be found in your text (Chapter 3) or the texts by Angelici (page 10) and Jolly (page 439), both of which are in the Reserve Room of the Science Library.

B. The Report. Each of your preparations will be written up in the form of a Note to the journal Inorganic Chemistry; therefore it will include a title, abstract, brief introduction, detailed experimental section (written in past tense), a results and discussion section (separate or combined), a paragraph of conclusions, followed by any acknowledgements. References should use Inorg. Chem./JACS style. See recent issues of Inorganic Chemistry for examples of Notes. Note that for figures showing NMR spectra, the peak assignments should be included on the spectrum. The structures of the reactant(s) and product(s), including expected bond angles, should be included. Note the last paragraph of your text’s Chapter 3: "Failure to reference material obtained elsewhere is grounds for failure. Even if an idea from elsewhere is "put into your own words" rather than being directly copied or quoted, it must be referenced."¹

C. The Product. Quality as well as quantity is important. Quality will be judged by purity (melting point, spectral characterization, etc.) and appearance (color, size of crystals, etc.). Quantity will be judged by the percent yield. This will be compared to the value claimed in the literature. It should be noted that these numbers usually seem too high.

All products must be turned in, in a container suitable for long term storage in an ordinary laboratory. This means that products which hydrolyze or oxidize in air must be torch-sealed in a nitrogen-filled all-glass ampoule or storage tube (made from a test tube). The samples will be looked at when first turned in and then again every week until the end of the semester. All products must be well labeled with your name, the compound’s IUPAC name, experiment date, yield in grams, % yield.

References

1. Szafran, Z.; Pike, R. M.; Singh, M. M. Microscale Inorganic Chemistry, A Comprehensive Laboratory Experience; John Wiley & Sons: New York, 1991; p. 35.