We then added 10cm3 ethanoic anhydride to the salicylic acid and swirled the contents, this mixes together the two chemicals. We then added 5 drops of concentrated sulphuric acid to the flask and thoroughly swirled the mixture, this creates the solution that makes the aspirin. We then warmed the flask for 20 minutes in a 400cm3 beaker of hot water which was approximately 60°C, we made sure the flask did not go above 65°C because this could have caused the contents to evaporate. Part 2: Using a 25cm3 measuring cylinder we measured out 15cm3 of ethanol into a boiling tube and then prepared a beaker half filled with hot water at approx. 75°C, we got this temperature by filling the beaker with cold water and slowly adding boiling water from a kettle until we reached the right temperature.
Experimental Methods: 1. SYNTHESIS OF 4-BENZOYL BUTYRIC ACID METHYL ESTER Materials required * 5 oxopentanoic acid : 2 gm (Aldrich) * Methanol : 50 ml * Acetic Acid (Rankem) Procedure: * 2 grams of 5 oxopentanoic acid was weighed and placed in a round bottom flask and then to it 50 ml of methanol was added. It was placed on a hot plate and the temperature was increased to 50 degrees under ambient air conditions.
In addition, phenolphthalein was added as an indicator. The aliquots were titrated against sodium hydroxide (NaOH) solution until end point was reached, after which volume of NaOH consumed was recorded. The value of the rate constant, k, obtained was 0.0002 s-1. The experiment was then repeated with 40/60 V/V isopropanol/water mixture and a larger value of k = 0.0007 s-1 was obtained. We concluded that the rate of hydrolysis of (CH3)3CCl is directly proportional to water content in the solvent mixture.
Fractional Distillation and Gas Chromatography (Investigative) Kevin Dural The University of Texas at Austin Fractional Distillation and Gas Chromatography (Investigative) Data and Results All data and results are attached. Included are carbon copies of written data and printed gas chromatography data. Discussion
Heat the solution until it is at 100 ˚C then continue heating for 75 minutes. Evolution of CO2 and NH3 is observed during heating. e. After 75 minutes of heating, stop stirring. Draw a little clear solution with a pipette, cool the solution to room temperature and measure its pH value with pH paper.
Then, 100mL 6M HCl was added to the same beaker also by using a graduated cylinder. The solution was stirred with a stirring rod. To make the 2M NaOH solution, 50mL deionized water was added to a 400mL beaker labelled “2M NaOH”. Then, 100mL 3M NaOH was added to the same beaker.
Place delivery tube in the bucket of water then into the water filled graduated cylinder (delivery tube should be approximately 5-10cm up the graduated cylinder) 10. Attach the end of the delivery tube, that is not in the bucket, to the hole of the cork 11. Pour the 50ml of HCL that you have measured, into the conical flask 12. As soon as all of HCL is poured into the conical flask, begin the stop watch, and close the top if the conical flask with the cork tightly 13. Measure rate of CO2 produced in the upside down 250 graduated cylinder (you will see that the water levels begin to decrease from the top of the cylinder.
Then an estimated (by trial and error) 1-3 grams of hydrated copper sulfate was added to a crucible with the lid on top. The total mass of the hydrated copper sulfate was recorded by subtracting the total mass of the crucible, lid, and sample from the mass of the crucible and lid (described in table 1.3). By attaching the wire triangle to the ring, the crucible was able to sit securely while having the bunsen burner underneath. Lighting the burner once again, each substance was heated for several minutes until estimated that the compound had changed color. Once a prevalent color change had been observed at approximately 4 minutes (blue green color) the crucible was set on the counter using the tongs to cool for approximately 5 minutes.
The mixture was vortexed and after centrifugation at 4000 rpm for 10 minutes, the absorbance of the organic layer (upper layer) was measured in UV-Vis spectrophotometer (Shimatzu) at 532 nm against blank using distilled water. TBA when allowed to react with MDA aerobically formed a colored complex [MDA-(TBA) 2 complex] which was measured with spectrophotometer. MDA concentration (measured as TBARS) was calculated as
Then, putting of choloform in amount of 10 mL and solution of Hanus iodine as amount of 10 mL into conical flask is realized. Addition of these two substance into otheraflask also occurs for blank. Next, waiting for these two samples for exactly 30 minutes is realized. Afterthat, solution of potassium iodine in amount of 15 mL and 40 mL water being distilled are added. Titration of last mixture is performed in company with 0.1 M Na2S2O3 until the obtaining of color in yellow.
Before starting the heating process, measure the weight of the crucible with its cover first and then tare the balance, and after that adding about 1 gram of the sample to the crucible with its cover, and then weigh it. Moreover, it is possible liberating harmful gases during the process of heating; therefore, being careful is important. The heating process ends when this sample changes the color to brown because water of hydration is removed to the sample. Additionally, give time to the small cool down and measure its weight. Next, transfer the sample to a 50 mL beaker and mixes with distilled water, which gets by rinsing the crucible with its cover in 8mL, so the solution is generated.
Then, the pipet was rinsed with distilled water. The bulbs were then attached to the pipette; filling and dispensing water were practiced using both bulbs. Furthermore, the 250-mL beaker was weighed, and its mass was recorded. After that, the Erlenmeyer flask was filled with 100 mL of distilled water. The temperature was recorded.
50 μL of these dilution solutions were separated on the TLC plate coated with SNISG. The plate was developed with petroleum ether: ethyl acetate (4:1) and the movement of solvent was usually controlled at 1 cm from the upper edge. After completion, the plate was dried until no solvent smell remained. It was sprayed with an ethanol solution containing 10% sulfuric acid, and heated at an infra-red drier until obvious color came up, as shown in Fig.2 (B.ab). Simultaneously, the amount of silver nitrate in the impact of isolative effect was investigated with the sample procedure, as shown in Fig.2
Introduction The purpose of this lab was to compare simple distillations of two sets of liquids by graphing the boiling points. One set of simple distillation of two liquids were supposed to have a boiling point difference of bout 30C while the other set of simple distillations had a melting point difference of about 57C. Furthermore, by conducting this experiment, students would develop a better understand of distillation and gas chromatography. Furthermore, I hypothesized that cyclohexane and p-xylene distill better than cyclohexane and toluene since cyclohexane and p-xylene have a larger boiling point difference than cyclohexane and toluene. The boiling point of cyclohexane is 80.74C while the boiling point for p-xylene is 138.23C and the boiling point for toluene is 110.6, thus
Experimental Clay-catalyzed dehydration of cyclohexanol Cyclohexanol (10.0336 g, mmol) was added to a 50 mL round bottom flask containing five boiling chips, Montmorillonite K10 clay (1.0430 g) was then added to the cyclohexanol and the mixture was swirled together. The flask was then placed in a sand bath and attached to a simple distillation apparatus. The contents of the flask were then heated at approximately 150 °C to begin refluxing the cyclohexanol. The distillation flask was then loosely covered with aluminum foil and the hood sash was lowered in order to minimize airflow. As the reaction continued, the temperature was adjusted in order to maintain a consistent rate of distillation.