Introduction
The purpose of this experiment was to identify the composition of over-the-counter analgesics by the method of Thin Layer Chromatography (TLC). The TLC method is used for rapid qualitative analysis of mixtures to determine and identify its components and purity. A development solvent was used to separate the analgesics found in both the known drug sample and an unknown sample of over-the-counter medications. The pertinent techniques for this experiment are spotting the stationary phase with the samples, placement of stationary sample in mobile phase chamber for development, observation under a UV light, and further development in iodine chamber.
Experimental Scheme
Figure 1 Figure 2
Anacin Salicylamide
Procedure
12 micropipettes were prepared in lab by heating the middle of capillary tubes over a flame. The capillary tubes
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After the completion of the micropipettes preparations, two silica TLC plates were prepared by drawing a line 1 cm from the edge of the silica TLC paper and divided into five parts with a ruler and a graphite pencil. One of the prepped silica TLC was used as the Reference Plate and the second as the Unknowns plate. The reference plate was spotted with Acetaminophen, Aspirin, Caffeine, Safinamide, and the standard reference mixture. The Unknowns plate was spotted with solutions identified as solution 1 through 4 and the last spot was spotted with the standard reference mixture. The micropipettes were used for spotting the two silica TLC plates after each was dipped in a separate solution. Effort was made to avoid over spotting or cross contamination of the solutions. Both prepped silica TLC plates were placed in the Development Chamber (DC), that had 0.5% glacial acetic acid in ethyl acetate as solvent.
For this lab, zeolite and magnetized zeolite were synthesized and compared with charcoal to find out with would be the most effective in the sequestering of Procion Red dye. Finding the concentration and absorbance of each zeolite, magnetized zeolite, and charcoal, along with a calibration curve, the best adsorbent is determined. Charcoal was the overall best sequestration of the Procion Red dye, since the adsorbent was highest compared to the others. Introduction Pollution has increased in the environment over the years, so the purpose of this experiment is to find the best adsorbent of chemicals to reduce the pollution.
Next, about 10 mL of both solutions, Red 40 and Blue 1, were added to a small beaker. The concentration of the stock solution were recorded, 52.1 ppm for Red 40 and 16.6 ppm for Blue 1. Then, using the volumetric pipette, 5 mL of each solution was transferred into a 10 mL volumetric flask, labelled either R1 or B1. Deionized water was added into the flask using a pipette until the solution level reached a line which indicated 10 mL. A cap for the flask was inserted and the flask was invented a few times to completely mix the solution. Then, the volumetric pipette was rinsed with fresh deionized water and
For the miniscale techniques used in this lab, 10 mL of cyclohexane was used and 20 mL of toluene was used. For the microscale technique,
Therefore, liquid-liquid and acid-base extraction techniques were successfully performed to separate the components of the Excedrin tablet. According to the TLC analysis results, the compounds (aspirin, acetaminophen, and caffeine) were successfully isolated from the analgesic (Excedrin tablet). In figure 1, the separation of the compound in the TLC analysis correlates with the TLC analysis in figure 2. Furthermore, Rf index calculations of the TLC analysis demonstrated that the compounds (aspirin, acetaminophen, and caffeine) were separated. The Rf calculations of aspirin in table 1 shows an Rf value of .491; however, in table 2 the Rf value of aspirin was calculated to be .784.
This study was conducted with a partner, since some parts of the experiment were able to be done simultaneously. One partner prepared a TLC developing jar by pouring a small layer of 4:1:1 propanol/acetic acid/water into a developing jar. A solvent wick was made by wetting a piece of filter with the solvent, and it was placed in the jar. A silica coated TLC plate was obtained, and a spotting line was carefully drawn approximately 1.5 cm from the bottom of the plate using a pencil. Extra care was taken to not touch the plate with bare skin.
Using two separate aseptic pipettes, 250 µl of LB broth were added to each micro test tube and mixed gently. Likewise, using two separate, aseptic pipettes for each tube, 100 µl of solution was added to the appropriate agar plate. After, using a new loop for each plate, the solution was spread gently across their surfaces. Lastly, the plates were stacked, taped together, and labelled before placing them upside down in an incubator set at 37°C
These difficulties might have caused me to make mistakes on the amount needed to pipette or the type of substance. Overall, next time I would have made sure to pay closer attention to the pipetting portion of the procedure. Furthermore, we could extend this experiment by trying different kinds of
Lab 8: Chromatographic Analysis of Analgesic Drugs Written by Gurleen Bhangoo Robinjot Kaur CHEM 3301-02 Professor Jeffery Crisman 21 March 2023 Abstract: Chromatography is an analytical method that is used to separate a mixture of chemical compounds into their individual components, allowing the individual components to be thoroughly analyzed. In this experiment, thin-layer chromatography (TLC) is performed to identify an unknown drug, and then column chromatography is used to separate out the components of the drug. The given unknown will contain one of the following drugs: Advil, Anacin, Aspirin, BC Powder, Excedrin, Excedrin Tension Headache, or Tylenol, where each drug will consist of a mixture of 1-3 compounds. The presence of caffeine
In this lab, we tested 8 known ingredients to find what ingredients was in our unknown A and unknown B medications. We first tested the water solubility of our knowns and unknowns. We found that of the knowns, cornstarch and acetaminophen were the only ones not water soluble. The unknowns were also not water soluble. Th next test was the pH test.
Materials and Methods The chemicals used to perform this experiment were distilled water, sodium chloride (NaCl), ice,
Leah Romero 10/30/2017 Conclusion Lab 3 Chem 102L In lab 3, fundamentals of chromatography, the purpose was to examine how components of mixtures can be separated by taking advantage of different in physical properties. A huge process in this lab was paper chromatography, which was used to isolate food dyes that are found in different drink mixes. The different chromatograms of FD&C dyes were compared to identify which dyes are present in each of the mixes.
INTRODUCTION A gas chromatograph (GC) can be utilized to analyze the contents of a sample quantitatively or in certain circumstances also qualitatively. In the case of preparative chromatography, a pure compound can be extracted from a mixture. The principle of gas chromatography can be explained as following: A micro syringe is used to inject a known volume of vaporous or liquid analyte into the head or entrance of a column whereby a stream of an inert gas acts a carrier (mobile phase). The column acts as a separator of individual or chemically similar components.
known as cation-exchange or anion-exchange chromatography, depending on whether the solutes to be exchanged are positively or negatively charged. Size Exclusion Chromatography: Here the molecules are separated according to their molecular weight and it is suitable for molecules having molecular weight of 2000 Daltons or more. Largest molecules are eluted first and the smallest molecules last. Affinity Chromatography: Here the stationary phase contains specific groups of molecules which can absorb the sample if stearic and charge related conditions are satisfied d.
For TLC profiling, 4 TLC plates were prepared for the testing of each solvent. As shown in Figure 1, the green food dye was placed at the bottom center, specifically 0.5 cm away from the bottom of the plate, with the use of a capillary tube. Each one of the silica plates were then vertically placed in a small beaker with its inside surrounded by a filter paper saturated with the solvent to be tested and a small amount of the same solvent at the bottom. The TLC plate was then taken out when the rising solvent was about to reach the top of plate. The ammonia: 1-butanol solvent was tested 7 times due to some personal
The developing solution was poured into a tank and was tightly covered with a glass lid, and the tank was allowed to be saturated to ensure that the solution was equilibrated in the gas phase. Silica plate for TLC analysis: A horizontal line was drawn with a pencil on the plate and it was about 1 cm above the bottom of the plate. The horizontal line was drawn faintly so as to avoid damaging the silica gel on the plate. On the horizontal line, two marks were made and one was named A and the other B. These marks were made towards the centre of the plate at a distance apart because when spots are made at the edge of a plate, the result would be an improper travel of the samples as the solvent advances on the plate.