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Isabella Luquetta Lab Partner: Ahsemon Taijani Experiment 3: Chromatography --- Analyzing Analgesics by TLC and Isolation B-Carotene by Column Chromatography. September 20th, 2019 Lab T.A: Zuli Li

Introduction: In this experiment, we used a conducted chromatography by analyzing analgesics by TLC and Isolation of B-Carotene by Colum Chromatography. Based on the lab manual, chromatography is the separation of two or more compounds or ions caused by their molecular interactions with two phases: one moving, and one is stationary. [ CITATION Wel18 \l 1033 ]. There are two types of chromatography; Stationary phase and Mobile phase. The stationary phase; they involve Silica gel and alumina, [ CITATION Jos19 \l 1033 ]; [ CITATION Pav99 \l 1033 ] which is the one we used during the experiment. In the second part of the experiment, we isolated B-Carotene by doing Column Chromatography. This is the experiment where you separate b-carotene from a spinach leaf. [ CITATION Wel18 \l 1033 ]. Column chromatography is one of the most useful methods of separation and the purification of both solids and liquids. “Some of the major advantages of column chromatography is the ability to handle larger amounts of material” [ CITATION Pav99 \l 1033 ].

Experimental: Part A: TLC TLC Plate + Obtain Silica Plates + Get starting line (1cm bottom) + Solvent front ( ½ cm top ) + Apply Samples + Insert plate into solvent jar + See mobile plate rising up

+ Take plate where solvent reaches solvent front + Take it to UV + Grab another TLC plate + Apply 4 samples to unknown sample + do same as above Part B: Isolation of B-Carotene for Spinach leaves 1. Column Packing + Microcolumn & cotton + Add silica gel halfway + Add ½ sand + Clamp Vertically in hood 2. Extraction + Add 2g of frozen spinach + 15mL ETOAC + Smash with spatula to increase S.A + Decant Solution + Anhy Na2SO4 + Decant + Evaporate + Sample + Crude – B-Carotene + other pigment. 3. Isolation + Wet column by adding Pet. Ether (carefully) + Transfer Sample + Using bulb + Flash chromatography + Collect fractions (yellowish) Conical Flask + Evaporate all solvent B-Carotene

Table of Contents: Acetaminophen : C8H9NO2 Melting Point: 170C Boiling Point: >500C Molar Mass: 151.16 g/mol Appearance: Colorless Crystals Aspirin: C9H8O4 Melting Point: 135C Boiling Point: 140C Molar Mass: 180.16 g/mol Appearance: odorless white crystals Caffeine: C8H10N4O2 Melting Point: 238C Boiling Point:178C Molar Mass: 194.19 g/mol Appearance: White, prismatic Crystals

Ibuprofen: C13H18O2 Melting Point: 76C Boiling Point: 157C Molar Mass: 206.28C Appearance: colorless, crystalline solid

Ethyl Acetate: C4H8O2 Melting Point: -84C Boiling Point: 77.1C Molar Mass: 88.11 g/mol Appearance: clear colorless liquid/ fruit odor Acetic Acid: C2H4O2 Melting Point: 16.6C Boiling Point: 117.9C Molar Mass: 60.05 g/mol Appearance: clear, colorless liquid B-Carotene: C40H56 Melting Point: 183C Boiling Point: 633C Molar Mass: 536.9 g/mol

Appearance: Red to brownish-red crystals Anhydrous Sodium Sulfate: Na2SO4 Melting Point: 884C Boiling Point: ---Molar Mass: 142.04 g/mol Appearance: Colorless crystals odorless

Results: Acetaminophen Aspirin 4/5.1 = .784 4.5/5.1 = .882 Table 1: Rf Values of TLC 

Ibuprofen 4.8/5.1 = .941

Unknown for the TLC was Acetaminophen

Compound: 4.2cm Standard: .3cm Rf: .3/4.2 = 0.71

Caffeine 2.5/5.1 = .490

Unknown 4/5.1 = .784

Sample: .3cm; .3/4.2 = 0.71

Discussion: For our Rf values, they were all over .5 except for Caffeine, which was .490. We only did one trial because there really was no point in doing two, if we could just put the unknown on the first plate. The unknown for this experiment was Acetaminophen. You could see from the table that they had the same Rf values. We correctly isolated the Beta - Carotene after pumping hexane and the petroleum either. The solvent separated and caused a yellow line to appear. There were failures in the experiment which made it hard to get the correct measurement and the standard Rf values. The values that are there are from the sample that was on the board, for us to compare the data too. Conclusion: In the conclusion of this experiment, the theoretical data that we got in discussion class and the results that we got were connected. The data revealed that the Beta- Carotene was isolated correctly and comparing it to the data that we got on the board, it had the correct Rf values. An example that is used in the real-world and using these techniques are drug testing. In some other cases it can also be used to distill liquor or any other alcoholic drink.

Works Cited Pavia, D. L. (1999). Isolation of Chlorophyll and Carotenoid Pigments from Spinach. Introduction to Organic Laboratory Techniques: A Microscale Approach 3rd Edition.

Touchstone, J. C. (2019, June 5). Chem.Libre Texts. Retrieved from Thin Layer Chromatography: https://chem.libretexts.org/Ancillary_Materials/Demos%2C_Techniques %2C_and_Experiments/General_Lab_Techniques/Thin_Layer_Chromatography Weldegirma, S. (2018). Experimental Organic Chemistry. University of South Florida, Tampa: ProCopy Inc....