The isolation and purity of crude acetylferrocene were tested through column chromatography. Crude acetylferrocene was observed to be an orange powder with a mass of 2.28 g. The percent yield was 124% ((2.28g/1.84g) x100%). The high percent yield was due to the high amount of sodium bicarbonate added in the previous lab. .100 g was weighed out on an evaporation dish. 6.00 g of silica gel was obtained in an Erlenmeyer flask. The solvent used was 100 mL of 80:20 petroleum ether/ethyl acetate. The silica gel and solvent were slurred together and poured quickly into the column through a funnel. The slurry was white and cloudy. The slurry was packed and made two layers: silica gel as the bottom layer while the clear solvent as the top layer. 5 mm of sand was added and resided on the top of the silica gel layer. …show more content…
The solution was added to the column. The column sides were rinsed with the solvent to make sure all the solution was on top of the silica gel. The mixture was drained to the top of the silica gel and the solvent was added to fill the column again. The solution of acetylferrocene and the solvent ran through the silica gel. It separated into two bands. The first band was yellow and at the bottom while the second band was orange and was at the top. There was more of the yellow band than the orange band. There was no third red band so the impurity, diacetylferrocene, was not produced. The solution was drained and collected into four test tubes. One contained just the solvent, two contained the yellow band (F1) and one contained the orange band (F2). The test tubes were changed when the band color changed in the column. A TLC was performed, comparing F1, F2, and commercial
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
The lab started off by measuring critical materials for the lab: the mass of an an empty 100 mL beaker, mass of beaker and copper chloride together(52.30 g), and the mass of three iron nails(2.73 g). The goal of this experiment is to determine the number of moles of copper and iron that would be produced in the reaction of iron and copper(II) chloride, the ratio of moles of iron to moles of copper, and the percent yield of copper produced. 2.00 grams of copper(II) chloride was added in the beaker to mix with 15 mL of distilled water. Then, three dry nails are placed in the copper(II) chloride solution for approximately 25 minutes. The three nails have to be scraped clean by sandpaper to make the surface of the nail shiny; if the nails are not clean, then some unknown substances might accidentally mix into the reaction and cause variations of the result.
At the fingerprint region, there was an intense peak at 734. 51 cm-1, which could be the C-CL stretch found in dichloromethane, which means the product might not have been pure. This lab was successful to an extent because we were able to obtain the product, 2-naphthyl ether, but it was not pure since the IR spectrum showed traces of dichloromethane. Also the percent yield of the product was over 100%. Some sources of error in this experiment were that since the product in vial 3 had solidified, we had added a drop of dichloromethane to the vial, resulting in the C-Cl peak of the IR spectrum.
Set the wavelength to 470 nm, this is to measure the tetraguaiacol. Set the spectrophotometer to zero by using a blank. The blank should contain 13.3 mL of distilled water, 0.2 mL of guaiacol, and 1.5 mL of enzyme extract in a clean test tube. After, transfer a portion of this mixture into a cuvette, cover the top of the cuvette with Parafilm and then place the cuvette into the spectrophotometer and set it to
Based on the result from the bromine test conducted, the clear appearance of the 4-methylcyclonexene demonstrated that the bromine had all been used up, and there is an unsaturated compound present. Infrared spectroscopy was another method of identifying an alkene. Figures 1 and 2 show the IR spectra for the reactant (4-methylcyclohexanol) and the product (4-methylcyclohexene), respectively; each were compared and analyzed. The IR spectrum for 4-methylcyclohexanol revealed a broad peak at 3328 cm-1, signifying an OH group and therefore an alcohol. In contrast, the IR spectrum for 4-methylcyclohexene no longer showed that broad band, but instead displayed a sharp peak at 1651 cm-1, representing a double bond and therefore an alkene.
However, this mixing can be minimized by not allowing the solutions to mix at the top of the column through adding a new solvent only once the old one is below the top of the
Nonetheless, the light yellow solid was purified by using the recrystallization technique. The formation of o-nitroacetanilide is inevitable and in order to eliminate it, 95% ethanol is used as the solvent of choice. The ortho isomer is soluble in the cold alcohol solution whereas p-nitroacetanilide in insoluble. As a result, the ortho isomer remains in the liquid solution and the final product, the p-nitroacetanilide is isolated with a final vacuum
In this laboratory experiment, 3.030 g of Isopentyl Acetate was synthesized and formed by the esterification of acetic acid with Isopentyl Alcohol. 1.0 mL of Sulfuric acid was used as a catalyst in the reaction. The excess Isopentyl Acetate was used to shift the reaction to the right for esterification to occur. During the extraction, the excess of acetic acid and Isopentyl alcohol was extracted with sodium bicarbonate, and further purification of the Isopentyl acetate was done after through drying with anhydrous sodium sulfate and through simple distillation. The percent yield of the Isopentyl Acetate was 46.6 percent with a theoretical yield of 6.502g. In this laboratory experiment the acetic acid was in excess and the Isopentyl Alcohol was the limiting reagent,
Identification of Unknown Solutions and Ammonium Salts preAice Chemistry Lab Report Descriptions of unknown solutions: Unknown Descriptions A Clear, colorless, odorless liquid. B Clear, colorless, odorless liquid. C Clear, red-brown, odorless liquid D Clear, yellow-orange, odorless liquid.
The crude tetraphenylnaphthalene in a 25-ml Erlenmeyer flask and dissolved in boiling isopropyl alcohol (12 ml). The solution was cooled to room temperature and further cooled in an ice bath for 30 minutes. Crystallization of colorless crystals occurred. The product was collect in a Hirsch funnel and washed with isopropyl alcohol. The solid was left to dry over the weekend.
In this experiment, 9-fluorenone, a ketone, was reduced to fluorenol, an alcohol. The product was then identified using melting point and IR data, and percent yield was calculated. Reduction is one of the two processes that occur during a redox reaction, and it involves the gain of an electron by one of the species. The other species in the reaction loses an electron, and is by definition oxidized. In this experiment, fluorenone, the oxidizing agent, was reduced, and sodium borohydride, the reducing agent, was oxidized.
Observations: 1. The first step had to be repeated due to not following proper instructions. I did not grease the screw, so as I was shaking the mixture, solids were forming around the screwpart of the separatory funnel. 2. When adding 5.0 mL of NaOH to the unknown mixture and shaking it for about 30 seconds, layers had formed.
Teflon was discovered by Dupont chemist. When Dr Roy J. Plunkett use polytetrafluoroethylene to make an experiment with chemical refrigerants, he tries to pump the gas tetrafluoroethylene into hydrochloric acid and he does not see anything happen in the outside. When he hold the cylinder that contain tetrafluoroethylene, he sees the cylinder still heavy. After that, he thinks it is a good idea to cut the cylinder to see what happen in the inside . When he cut it out, he sees the tetrafluoroethylene have polymerized and it as a waxy powder.
The objective of the experiment completed was to form the product 9,10-dihydroanthracene-9,10-α,β-succinic anhydride from anthracene and maleic anhydride. The reaction that took place is named a Diels-Alder reaction, defined as an addition reaction in which a diene unites with a double or triple bond of an unsaturated compound to form a 6-membered-ring. The following reactions below depict the ways in which dienes and dienophiles join to form products. Anthracene functioned as a diene and maleic anhydride functioned as the dienophile. Xylene was used as a solvent that provided a quicker way of reaction between the two starting materials.
A small amount of sand was added after the layer of cotton. After that, a layer of silica filled almost 1/3 of the column. Finally, another small amount of sand was added just above the silica. The column was given a little tap with an aspirator to make the silica more compact. Figure 2.