Each member of a team will write his or her own report. Your report must be presented to me in a hard-copy format. No electronic copies will be accepted. Your report is to be written in clear and coherent English! Please obey all of the rules of English grammar. Run spell and grammar check. Do not use the first person in your reports (e.g., I; my; we; our; etc.)! The report needs to be typed and double spaced. Tables and graphs must be done electronically with a program such as Excel. For any chemical structures you submit, the drawings must be done with ChemDraw.
Your lab report must include all of the following to be complete:
Your Name, your partner's name and the Date the report is submitted
The Title of the Experiment
Unknown Number (zero credit without the unknown number)
Abstract (summary not to exceed three sentences) - An abstract is usually written after the report has been constructed, as it is a summary of the report and not a summary of the experiment.
1. Make tables of your data from temperature (boiling point) versus volume of distillate readings (two tables - one from simple and one from fractional distillation data; [measurements taken every 2ml from 0ml to 24ml]
2. Inject your original unknown mixture into the gas chromatograph and determine the Rf values for the first and second component. Report those values. Use the integration function to determine the relative percentages of the first and second component. What are those percentages?
3. An injection into the gas chromatograph of either your 6 or 24ml sample allows you to determine which component in the unknown mixture corresponds to the high boiling and which to the low boiling component. Compare with the original mixture in #2 above. From the gc injections, is the first component the high or low boiling component? Explain.
4. Using the gas chromatography injections of the original unknown mixture (from #2 above) against the authentic samples that are provided, determine the identity of your two unknown components; high and low boiling components. Compare the boiling points from your distillation and Rf values obtained by injection of the original mixture to the boiling points and Rf values of the authentic samples. What are the identities of your two components?
Conclusion (not to exceed 100 words)
In the discussion section comment on the separation differences you achieved using simple and fractional distillation; this comes from your temperature (boiling point) versus volume of distillate readings. What were the identities of the components of your unknown mixture? How does your data allow you to absolutely identify the components of the mixture. Be complete in your analysis and write a convincing conclusion.
Attach your carefully labeled graph to the back of your report with a staple. This is a plot of the temperature (boiling point) versus the volume of distillate, with the temperature on the y-axis and the volume on the x-axis (on this graph there will be two curves: one for simple and one for fractional distillation (from the data table referenced in #1 above).
Note on Graphs - Make sure your graphs utilize the full extent of the page, and make sure that your x- and y-axes are appropriate for the data. For example if your temperature is from 70-120oC, make sure your y-axis has a range (top to bottom) that is close to that range. Don't show that data (70-120oC) on a graph with a y-axis that goes from 0-150oC. Additionally make certain that all data points are visible on your graphs (i.e., I want to be able to see the data points even though you may connect the points with a line) and that each curve is clearly labeled as simple or fractional.
This is a single report - NOT TWO. In addition to this report make sure to complete your lab notebook conclusions. The report needs to be typed and double-spaced. You are not required to prepare the report in two columns like the example paper indicated below. Please obey all of the rules of English grammar. Try to be concise and exact. Complete any structure drawings using the ChemDraw program. When you submit this report, please include your spectra and downloaded spectra. Absolutely do not forget to include your unknown number in a readily visible location at the top of the report. You will receive zero credit for your report if you fail to do so.
IMPORTANT! - Your reports must be written independently. You may help one another but do not plagiarize in any form. Your report is to be written in clear and coherent English! Do not use the first person in your reports (e.g., I; my; we; our; etc.)! Do not write in the command form for any part of your report (e.g. of command form; "Avoid contact with this chemical."; "Do not inhale the fumes."; etc.)! Write in the past tense! EXAMPLE - "The organic layer was extracted three times with a 5% sodium hydroxide solution. The basic extracts were combined, cooled in an ice bath and acidified with 10% hydrochloric acid".
The following link (Quinn_JOC_2013.pdf) will take you to a recent paper by Quinn et al. that describes the isolation of some interesting natural products from an Australian marine sponge. Please use this paper as a model for constructing your own reports. Please follow the format employed there. This is the standard format used for a paper in the Journal of Organic Chemistry published by the American Chemical Society. The order of parts for the paper is:
Title (Also be sure to include the unknown number here.)
Author list (This will be you.)
Abstract (It may not exceed one paragraph. This is a summary of your report. Write it last.)
Introduction (I would use this part to introduce the experiments chronologically with some mention of how they apply in a global sense to the identification of the unknowns. If you want to talk about any theory this is the section where those entries are made.)
Results and Discussion (This will be the longest portion of your report where the results from each experimental method are presented with explanation and discussion.)
Conclusions (Make certain that your summary also includes the unknown number and the identity of the two components.)
Experimental (This details the steps along the way. Look to the example paper and refer to your lab manual as well as entries in the procedures of your lab notebook.)
Make certain that you address the results of each experiment (Extraction, Recrystallization, Melting Points, Thin Layer Chromatography and Spectroscopy) in each appropriate section of your lab report.
From the SDBS website (http://sdbs.riodb.aist.go.jp/sdbs/cgi-bin/cre_index.cgi), download the IR and CNMR spectra for your neutral component to confirm the identity of your unknown. Combine these with your own spectra that you will attach to this report.
After consulting the MSDS website (http://hazard.com/msds/index.php), report briefly on the hazards associated with your unknown. I expect that for each unknown you will write a short paragraph.