In this experiment, preparative gas chromatography was performed to isolate components present in a mixture before infrared spectroscopy was utilized to determine the separated parts. At the start of the lab, unknown # C-2 at 170C was provided for testing. When the GC was ran, the retention time for fraction 1 started with 2.12 minutes and ended with 2.96 minutes. The retention time for fraction 2 started at 4.56 minutes and ended at 5.96 minutes. After centrifugation, a small amount of the sample was pulled to the bottom of the conical vials to be used in the infrared spectroscopy. For fraction 1, two main peaks developed at 3336.14 cm-1 and 2878.08-2962.24 cm-1. For fraction 2, two main peaks also formed at 3265.26 cm-1 and 1635.72 cm-1. …show more content…
Unknown # C-2 was injected into a separation column that was coated with a polar stationary phase. This apparatus was held in an oven so that the sample could be heated to vaporization under 170C. An inert gas, like helium in this case, acted as the mobile phase since it carried the vapor through the column to the thermal conductivity detector, forming 2 peaks along the process. The first fraction was concluded to be 3 pentanol since its peaks included 3336.14 cm-1, an alcohol functional group, and 2878.08-2962.24 cm-1, an alkane functional group. Since the two components in this lab had identical boiling points, separation cannot rely solely on the volatility of each compound. Instead, a polar gas chromatography was utilized to isolate a mixture based off of its interactions with hydrogen bonds. Although 3 pentanol is polar with an alcohol group attached to its end, its hydrocarbon chain decreases its solubility in water, making it possess a lower affinity for the stationary phase and elute first. In the second fraction, only one main peak could be identified at 3265.26 cm-1 that matched the provided IR spectra. This peak represents another alcohol group which limits it down to 3-methyl-butanol, 2 heptanol, 2 octanol, and 1 hexanol. Since this was the second fraction, it must be more polar than the first fraction to elute last. Therefore, by elimination, the second fraction was identified as 3-methyl-butanol. This structure includes an alcohol group. However, its shorter hydrocarbon chain increases its solubility in water while its methyl group decreases in dispersion forces, making 3-methyl-butanol more polar than 3 pentanol. Overall, preparative gas chromatography proved to be mostly successful in this experiment since this technique was able to separate the
Since it is also a solvent, it has many cleaning uses. We predicted at once that is could be isopropanol because of its smell. Question: “What is the identity of unknown 6 in test tube 20?” Hypothesis: If I test the characteristic properties of unknown 6 then I will see its properties to be the same or similar to isopropanol.
The difference in this chemical and physical properties will aid in their separation. Processes like solubility, gravitational filtration and recrystallization will be used to separate the substances present in Panacetin. The melting and boiling point of the substances will help in concluding on which of these compounds will be presented at the end of experiment. Procedure and observation The Panacetin content was weighed approximately 3.0493g and transferred to the Erlenmeyer flask; 75ml of dichloromethane (CH¬2CL2) was added to the content. The dichloromethane (CH2Cl2) dissolved the sucrose, leaving the active unknown agent and aspirin behind.
The area under each peak allows the calculation of the quantity of the referred component. As expected from gas chromatography analysis, two peaks were seen demonstrating that here are two components in the mixture. Using the fraction #1, the first and biggest peak represents the isopropyl and the smallest represents toluene. This demonstrates that, as expected, the first collection was mainly composed by isopropyl because isopropyl has less boiling point (Table #1). On the contrary, for the last (third) collection GC analysis, the smallest peak represents isopropyl and the highest peak represents toluene.
Question: Describe what happened to the original spot of plant pigment extract? The spot traveled from the faint line on at the tip of the chromatography paper and it then created bands of colors. The original color of the plant extract was a black color and the once it was immersed in developer four it then started to travel up the paper strip. How do your Rf values compare with those of your classmates? They were similar but some were different due to errors in the experiment.
One pair had a 50:50 mixture of cyclohexane: toluene while the other pair had a 50:50 mixture of cyclohexane: p-xylene. For both distillations, we were to collect the first milliliter and the last several drops in order to run a GC for each fraction. Furthermore, for both distillations, students obtained 30ml of their designated 50:50 mixture in a 50ml round bottom flask. By properly using the simple distillation apparatus, students were able to record the temperature of the distillate, we recorded the temperature for every 1ml. Once students collected the first 1ml, the 25ml of distillate and the remaining drops, we were able to determine the mole fraction of cyclohexane by using gas chromatography.
After finding the Rf values of the four known compounds, solvent 1 (99.5% ethyl acetate/0.5% acetic acid) was chosen, due to the wide range of results, for the remaining experiments. Ibuprofen, our known tablet, gave a similar Rf value to our previous results for Ibuprofen. For Anadin extra, there were three compounds identified as Caffeine, Paracetamol and Aspirin as the Rf values of the drug were close to the values of these three compounds in the first part of the practical. For both of these known drugs, the Rf values acquired were close to my predictions before the experiment. For the unknown powder, we obtained Rf values of 0.52 and 0.76 so we believe that the unknown powder contains Aspirin and Ibuprofen.
The resulting sample weights displayed in the above data table show that a significantly greater amount of mesitylene was collected compared to toluene. Since a larger amount was taken, the mesitylene sample was likely not as pure as the toluene sample. In order to determine the identity and purity of both samples, each were run through high pressure liquid chromatography (HPLC) and gas chromatography with mass spectrometry (GS-MS). The purity of the mesitylene distillation could be improved by drawing out more sample in the middle of the distillation and setting it aside as an intermediate. This way, the only samples collected would condense at the beginning and the end of the distillation, and would therefore be purer.
The overall aim of our experiment was accomplished due to the fact that the compound produced was tested to be pure paracetamol. Its purity was tested by TLC, melting point range and NMR analysis. For the Melting Point Range Determination, samples of our re-crystallised p-aminophenol and paracetamol were placed into capillaries and into the melting point apparatus where data was recorded during the melt. Then, for the Thin Layer Chromatography, a TLC plate was prepared with four small dots loaded with p-aminophenol, our recrystallised p-aminophenol, our resultant paracetamol and commercial Panadol® respectively. When TLC was completed, it was transferred to a UV lamp box for analysis and data collection.
Aim The purpose of this lab was to separate a mixture of carboxylic acid (p- toluic acid), a phenol (p-tert-butylphenol) and a neutral compound (acetanilide) using solvent extraction. Introduction Solvent extraction is a process that separates compounds from a mixture by a solvent.
The vacuum filtration technique resulted in a 89mg recovery of CaCO3 which was an 11% loss. The gravity filtration had a lower % loss, and therefore a higher percent recovery. The main way to lose the compound was in the flask where the calcium carbonate was mixed with the acetone. It was difficult to transfer all of the calcium carbonate and not leave a small amount of solid residue at the bottom of the flask. The gravity filtration resulted in a higher recovery.
The development of Gas Chromatography (GC) to be an analytical technique to separate the components of a mixture
Solubility of the compound was determined in different solvents like hydrochloric acid, sul-furic acid, sodium hydroxide, methanol, ethanol, acetone, ethyl acetate, chloroform, DMSO, glacial acetic acid, n-hexane, cyclohexane, n-octanol, diethyl ether, benzene, toluene and wa-ter, followed by the preparation of saturated solution with those solvents which shows good solubility with the synthesized compound and then plotted a linear calibration curve to de-termine the concentration. The solubility determination was based on the USP Criteria (Low Y and Law SL., 1996; Lalitha Y and Lakshmi PK., 2011). 2.7.3. pH 10 mg of the synthesized compound was weighed accurately and placed into three separate volumetric flasks containing suitable solvents
Both processes separate mixture based on boiling point. Fractional distillation does it on a larger scale whereas GC does it on a small scale Source: http://www.shimadzu.eu/gas-chromatography Discussion on analysis This technique requires a stationary phase and a mobile phase. The mobile phase being the carrier gas is comprised of an inert gas such as helium, argon or nitrogen. The stationary
This experiment aims to separate the components of the green colored food dye and get the TLC profile of each eluent collected. III. Experimental Procedure Before starting with the column chromatography for food dye, the right solvent must be chosen between 2-butanol with acetic acid, ammonia in butanol, 1 part 1-butanol 1 part acetic acid, and 2 parts methanol 1 part water. In choosing the appropriate solvent for column chromatography, the solvent system must give a TLC profile wherein most of the spots are well separated and has a Rf value within 0.3-0.5.
DETERMINATION OF PERCENTAGE ETHANOL IN BEVERAGES 1. Introduction to Gas Chromatography Gas chromatography is a very powerful separation technique for compounds that are reasonably volatile. The components of a sample partitions into two phases, the 1st of these phases is a immobile bed with a great surface area, and the other is a gas phase that permeates through the immobile bed. The sample is evaporated and passed by the mobile gas phase or the carrier gas through the column. Samples separates into the stationary liquid phase, based on their solubilities at the given temperature.