Experiment #2

Experiment #2 - CH242 EXPERIMENT #2 CHEMICAL AND...

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CH242 EXPERIMENT #2 CHEMICAL AND SPECTROSCOPIC IDENTIFICATION OF UNKNOWN ORGANIC COMPOUNDS Background In this lab you will be given a series of unknown compounds, either in pure form or as a mixture of two compounds. Your task is to separate the components (if necessary) and, using an assortment of instrumental and wet chemical methods, unambiguously establish the chemical identity of your unknown compounds. Unknown 1 will be a pure (single) compound of relatively simple structure. Unknowns 2 and 3 will be supplied to you as a mixture, which will require separation prior to structure identification. Unknown 4 will be a pure (single) compound of more complex structure. Instrumental Methods (required for all unknowns unless otherwise indicated): 1 H NMR, 13 C NMR (optional for unknowns 2 & 3), IR, and MS. Mandatory Wet Chemical Methods For Unknown 1: Attempt all the available functional group tests and prepare an appropriate derivative for your unknown (see below for more details on derivative preparation). In addition, determine the melting point of your unknown if it is a solid. Mandatory Wet Chemical Methods For Unknowns 2 and 3: Attempt all the available functional group tests for each unknown. In addition, determine the melting point of each unknown that is a solid. Wet Chemical Methods For Unknown 4: Wet chemical methods are NOT required, but may be used to aid/confirm your spectroscopic analysis. In addition, determine the melting point of your unknown if it is a solid.
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1. Procedural Guidelines for the separation of unknowns 2 and 3 (supplied as a mixture): You will need to develop a procedure for the separation of unknowns 2 and 3 based on the following information: One of the components in your mixture is either a carboxylic acid or a phenol. Your second component is not a carboxylic acid or a phenol and also does not contain any functional group more acidic than water. We also strongly recommend that you use an extraction procedure based on the above information in order to separate your compounds. Further, we recommend that you purify all solid unknowns by recrystallization. Very important!!! Some liquid unknowns may be sufficiently volatile to be lost if left on the rotary evaporator for a long time. If your unknown is a liquid, make sure that you keep an eye on it while on the rotary evaporator! 2. Make sure to record the physical characteristics of each unknown. Include characteristics such as color, odor, whether it is solid or liquid. 3. Determine the melting point for all solids. Take care that an accurate measurement is made and that you report your value as a range. This becomes an important clue to the identity of your unknown . Functional group tests
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Experiment #2 - CH242 EXPERIMENT #2 CHEMICAL AND...

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