Analysis Lab Report Flash-Column Chromatography
Introduction
Flash-Column Chromatography is another useful technique used to separate and purify complex mixtures of compounds. In this experiment, TLC is used to determine the best solvent system for the column. Due to Flash-Column Chromatography1 being an inexpensive technique, many scientist use this process for drug and natural product purification.
Method
By using the information from Experiment 6B, the TLC solvent system used was 30% EtOAc: 70% Hex. Experiment 7 was broken into two parts, Part One and Part Two. For Part One TLC was used to determine the eluents and the polarity of p-tert butylphenol and p-tert-butylbenzoic acid. First, the TLC plate (1.5 cm x 3.0 cm) was labelled with three lane, 1 for p-tert butylphenol, 2 for p-tert-butylbenzoic …show more content…
Furthermore, in Part Two Column Chromatography, a 23.40 mg of p-tert butylphenol and 26.20 mg p-tert-butylbenzoic acid were combined into one scintillation vial and placed in a safe place. Then, 3 cm x 3 cm TLC plates were used and labeled with seven lanes each until the reaction was completed. Moreover, a 10 mm column was packed with cotton the size of a nickel at the bottom of the column using a clothes hanger. The column was clamped in the ring stand in the hood, and roughly 7 inches of dry silica was added using a powder funnel. The dry silica was transferred into an Erlenmeyer Flask. The column was approximately ½ filled with Hexanes. Hexanes was added to the Erlenmeyer flask filled with dry silica, swirled, and quantitatively transferred into the column. The stopcock was opened and the Erlenmeyer Flask was placed underneath the column. By using the air-line, Hexanes was forced until no bubbles were formed, the silica gel was flat, and making sure the column was never dry. The column was clamped in one of the working spaces where the test tubes and other materials could be reached. Once clamped and secured, the 30% EtOAc:70% Hex sovent system was quantitatively dispersed into the column while making sure
Flash-Column Chromatography is another useful technique used to separate and purify complex mixtures of compounds. In this experiment, TLC is used to determine the best solvent system for the column. Due to Flash-Column Chromatography1 being an inexpensive technique, many scientist use this process for drug and natural product purification.
Method
By using the information from Experiment 6B, the TLC solvent system used was 30% EtOAc: 70% Hex. Experiment 7 was broken into two parts, Part One and Part Two. For Part One TLC was used to determine the eluents and the polarity of p-tert butylphenol and p-tert-butylbenzoic acid. First, the TLC plate (1.5 cm x 3.0 cm) was labelled with three lane, 1 for p-tert butylphenol, 2 for p-tert-butylbenzoic …show more content…
Furthermore, in Part Two Column Chromatography, a 23.40 mg of p-tert butylphenol and 26.20 mg p-tert-butylbenzoic acid were combined into one scintillation vial and placed in a safe place. Then, 3 cm x 3 cm TLC plates were used and labeled with seven lanes each until the reaction was completed. Moreover, a 10 mm column was packed with cotton the size of a nickel at the bottom of the column using a clothes hanger. The column was clamped in the ring stand in the hood, and roughly 7 inches of dry silica was added using a powder funnel. The dry silica was transferred into an Erlenmeyer Flask. The column was approximately ½ filled with Hexanes. Hexanes was added to the Erlenmeyer flask filled with dry silica, swirled, and quantitatively transferred into the column. The stopcock was opened and the Erlenmeyer Flask was placed underneath the column. By using the air-line, Hexanes was forced until no bubbles were formed, the silica gel was flat, and making sure the column was never dry. The column was clamped in one of the working spaces where the test tubes and other materials could be reached. Once clamped and secured, the 30% EtOAc:70% Hex sovent system was quantitatively dispersed into the column while making sure