Experiment 2A

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California State University, Long Beach *

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223A

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Chemistry

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Feb 20, 2024

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pdf

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4

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13 Experiment 2A: TLC Analysis of Analgesic Drugs Instruction Sheet You will need to bring to your lab section: 1. A lab notebook with procedures written in your own words 2. ‘Making the Connections’ text 3. A HARD COPY of this document (3 pages Worksheet) 4. A RULER (with cm scale) Tips for effective time management: You can use the time spent developing TLC spots to work on questions. Worksheet/Report : Found in the next three pages. This is due at the end of the lab period. NO other reports need to be submitted besides the Worksheet.
14 Experiment 2A: TLC Analysis of Analgesic Drugs Worksheet Lab Section ____________ Last Name ____________First_________ Date: ____________ Lab Partner’s Name ________________ Unknown Code (A, B, C, …) ________ (20 Points Possible) TLC results: Part 1) Use the plates below to draw a representation of the TLC plates: Each plate should contain the standard solutions and the right plate for your unknown. Clearly show how each measurement was determined by a ruler for the calculation of R f values. (2 points) Part 2) Report and calculate the R f values for each of the spots. (4 points, 1 point for each blank) Eluent (Solvent Mixture) used to develop plate: ____________________________ Compound Spotted R f values Aspirin Ibuprofen Your unknown
15 Part 3) Which analgesic drug was your unknown? (1 point) Part 4) Is your unknown pure? What is the evidence of its purity (or contamination)? (1 point) Part 5) Change the Eluent type to Ethyl Acetate: Hexane (50:50), use the plate below to draw a representation of the TLC plate. The plate should contain a mixture of the standards for comparison. (1 point) Part 6) Report the R f values of Part (5): (1 point) Compound Spotted R f values Aspirin Ibuprofen Your unknown Part 7) Compared to Day 1 (Worksheet Part 2), does this change in solvent type in Part (5) affect the R f values? Rationalize your observations. (2 points) Part 8) (a) In addition to the solvent mixture chosen as Eluent in this experiment, name the solvent that was used to create the spotting solution of your unknown. (1 point) (b) Does the solvent in Part 8(a) affect the R f values in this entire experiment? Briefly explain. (1 point)
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16 Additional Questions: 1) A mixture of benzoic acid, para-xylene and benzaldehyde is spotted on a silica gel TLC plate and developed using Ethyl Acetate with 0.5% acetic acid as the solvent. Predict the relative R f values for the three components in the sample (highest to lowest). (2 points) 2) Arrange the following solvents in order of increasing polarity (least polar to most polar): (2 points) Diethyl Ether, Propyl Amine, 3-Methyl-Pentane, Acetone 3) If you ran an unknown sample on a TLC using 3-Methyl-Pentane as eluent and observed only one spot with a Rf value ~0.05, is it safe to assume that it is a pure compound? If not, how can you check it out using TLC? (2 points)