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11 Nov 2019
Create a flowchart
SEPARATION, PURIFICATION AND IDENTIFICATION OF TWo UNKNOWNS IN A MIXTURE Overview: The time has come for you to determine your own procedures for carrying out a project! Be sure you keep detailed lab notes on everything you do in this multi-lab project. You will only be given credit for procedures that are recorded clearly in your lab notebook. You will be given a mixture containing two unknowns, each containing one or more functional groups: one is a solid carboxylic acid -one is a liquid that is not a carboxylic acid-boiling point is between 95 and about 200°C -separate the two compounds, getting the best recovery you can of each -purify each of the two compounds Your goals are to (you will be asked to report percent recovery - identify the two compounds Minimum required propcrtics of the compounds to be determincd: For the solid carboxylic acid -melting point H NMR spectrum (but NOT 1SC NMR) IR spectrum run as a KBr pellet TLC to assess purity For the liquid - boiling point - H NMR spectrum 3C NMR spectrum - IR spectrum - GC to assess purity Some experimental notes 1. Both unknowns are generally soluble in the organic solvent methyl tert-butyl ether (MTBE) and not very soluble in water, 5% NaOH will be available in case you think of a good use for it in the separation. 2. Various recrystallization and NMR solvents will be available. If you don't see what you want, ask 3. Some resources for structure ideas once you know the mp or bp and functional group are: a. the CRC Handbook of Tables for the Identification of Organic Compounds (not the same thing as the regular CRC handbook) - available in stockroom. b. http://www.colby.edu/chemistryicm html Warning: Always consider at least a t or-5'C range around your observed melting or boiling point. here is no guarantee that your unknown c ompound is listed in these resources
Create a flowchart
SEPARATION, PURIFICATION AND IDENTIFICATION OF TWo UNKNOWNS IN A MIXTURE Overview: The time has come for you to determine your own procedures for carrying out a project! Be sure you keep detailed lab notes on everything you do in this multi-lab project. You will only be given credit for procedures that are recorded clearly in your lab notebook. You will be given a mixture containing two unknowns, each containing one or more functional groups: one is a solid carboxylic acid -one is a liquid that is not a carboxylic acid-boiling point is between 95 and about 200°C -separate the two compounds, getting the best recovery you can of each -purify each of the two compounds Your goals are to (you will be asked to report percent recovery - identify the two compounds Minimum required propcrtics of the compounds to be determincd: For the solid carboxylic acid -melting point H NMR spectrum (but NOT 1SC NMR) IR spectrum run as a KBr pellet TLC to assess purity For the liquid - boiling point - H NMR spectrum 3C NMR spectrum - IR spectrum - GC to assess purity Some experimental notes 1. Both unknowns are generally soluble in the organic solvent methyl tert-butyl ether (MTBE) and not very soluble in water, 5% NaOH will be available in case you think of a good use for it in the separation. 2. Various recrystallization and NMR solvents will be available. If you don't see what you want, ask 3. Some resources for structure ideas once you know the mp or bp and functional group are: a. the CRC Handbook of Tables for the Identification of Organic Compounds (not the same thing as the regular CRC handbook) - available in stockroom. b. http://www.colby.edu/chemistryicm html Warning: Always consider at least a t or-5'C range around your observed melting or boiling point. here is no guarantee that your unknown c ompound is listed in these resources
Deanna HettingerLv2
31 Jul 2019