Introduction: Chemical equilibrium is a crucial topic in Chemistry. To represent and model equilibrium, the thermodynamic concept of Free energy is usually used. For a multi-component system the Gibbs free energy is a function of Pressure, Temperature and quantity (mass, moles) of each component. If one of these parameters is changed, a state change to a more energetically favorable state will occur. This state has the lowest free energy. When the free energy of all states are equal to each other, the system is at equilibrium. The Heat that is relased or absorbed during a state change absorbed is known as latent heat. For a binary mixture such as durene and naphthalene, the Clausius-Clapeyron equation (cf. Appendix) relates the latent …show more content…
Once the initial set up was complete, the group collected the first sample of Durene by placing a test tube in a beaker, tearing this system, and then adding in the appropriate amount of Durene. The group then proceeded to melt the sample in the boiling water. The Durene sample was then placed into the ice water bath, and immediately the temperature probe started. As the sample cooled, the group noted at what time the first signs of crystallization occurred. After the sample cooled to about 45°C the run halted, and Naphthalene was added to the sample by the same process used to acquire the first sample of Durene. While these trials were running and being completed, similar trials were conducted for a mixture that started with a sample of Naphthalene. Durene was added to this sample in the same manner as Naphthalene to the Durene sample. The group followed the provided tables when creating the mixtures for each run. While the lab procedure called for the experiment to take two weeks the group completed the experiment in one lab period. The group then proceeded to export its data to a flash drive from the GLX. However, after exporting only three trials, the GLX froze and would no longer operate. All of the group’s data was lost, and the group had to redo the experiment. The only differences in procedure the second time the lab was performed were the experiment was carried out over two weeks instead of one as one set of trials were conducted at one
The mixture was transferred to an ice bath to crystallize the product, after which the product was collected by vacuum filtration on a Hirsch funnel, washing the flask with small aliquots of cold xylene and pouring the solution over the crystals, allowing the vacuum to thoroughly dry the product. Additional drying was achieved by transferring the product to filter paper and pressing the crystals to remove any excess moisture. The product was then weighed and a melting point determined. A comparative TLC was run in Hexanes:Ethyl Acetate solvent against maleic anhydride to verify the purity of the
The product was placed in a Craig tube and several drops of hot (100°C) solvent (50% water, 50% methanol, by volume) was added and heated until all of the crystals dissolved. The Craig tube was plugged and set in an Erlenmeyer flask to cool. Crystallization was induced once the mixture was at room temperature by scratching the inner wall of the tube. It was then placed into an ice bath for ten minutes until crystallization was complete. The tube was then
The product was then suspended in 2 ml of water with a stir rod in a 50 ml Erlenmeyer flask and heated to boiling. Water was added in one milliliter increments until all the product was dissolved (18 ml added total). The saturated solution was allowed to slowly cool, and gradual white crystal formation was observed. Recrystallized product was collected once more by suction filtration with the Hirsch funnel once crystallization ceased. Collected product dried on a watch glass for a week, weighed 0.14 g (1.2 mmol), and the melting point was 139°-141°
The apparatus used was the vacuum filtration, which is faster than the gravity filtration and can only be used with a Büchner funnel. When using the Büchner funnel, a filter paper needs to be inside of the funnel, as well as, a rubber stopper placed on the funnel to guarantee a good seal. After the experiment was completed, a pure sample of Dulcin was obtained because the exact melting point was determined to be 171.5-172.1°C while the literature value was 173-174°C which is a narrow range. The Rf values also support the reasoning that Dulcin is pure because the Rf value for
The first part of the lab began by one lab member adding 10.0 mL of DI water to a test tube while another lab member obtained a beaker full of ice and salt. After both these steps were complete the test tube was put in the beaker full of ice. Immediately following the test tube be being placed in the beaker, a temperature probe was inserted into the test tube. The initial temperature was recorded and after the temperature was recorded in 30 second increments. Once the water exhibited supercooling and then remained consistent at .1 °C for 3 readings it was determined that the water had froze and formed crystals. Evidence that crystals formed allowed for it to be confirmed that the water actually hit freezing point at .0
The melting point of the final product, diphenylacetylene, was found to be 65-68 degrees Celsius which is right around the ideal 61 degrees Celsius melting point; this shows that purification during the lab worked and that the sample was almost 100% pure. Since only 0.01g of diphenylacetylene was collected and the theoretical yield was calculated to be 0.049g, this experiment had a 20.41% yield. A few sources of error that explain the low percentage could be the loss of crystals when transferred from the test tube to the suction apparatus or when they were transferred from the suction apparatus to the filter paper to be dried and then weighed. Crystals could have also been lost if more than 5 drops of methanol was added because excess methanol would dissolve the crystals. The experiment was successful when looking at the crystals collected from the addition step and the elimination step; however, to improve the percent yield and collected product the the test tubes could have been allowed to cool down in the ice bath past the 5 minutes to ensure all the crystals formed
This process starts and ends with square boxes, using arrows to show the flow of the process from start to finish. An upside-down triangle indicates a storage point with no inspections enabling me to save tune and prepare in advance. Rectangles are steps in the process with approximate times in each. Decision points are shown with diamond shapes with arrows following yes and no responses.
The stilbene dibromide precipitated immediately as small plates. The mixture was cooled under tap water helping crystals form. The mixture was cooled before collecting the product by a vacuum filtration. For the crystals not to stick in the flask, the solution was washed with small amounts of ice cold methanol. When done pouring, the isolated solid dried for a few minutes in the filtration. To increase drying time, the crystals were pressed down. When the solid was collected, data such as melting point, percent yield and infrared spectroscopy spectrum values were collected.
Tube 4 now should only have crude solid in the tube and it is then weighed. The tube is placed into a 50℃ water bath and then approximately 0.5 -1 ml of methanol is added, as well as H2O until the solution gets cloudy, once the solution is dissolved it is cooled to room temperature and then iced. The crystals are then collected using a Hirsh funnel. Next a small amount (~ 0.1g) of the crystals are placed into a melting point tube and placed into the melting point machine to record the unknown neutral substances melting point.
It was desired to compare a theoretical value of enthalpy of combustion to a literature value. To do this, the theoretical value was calculated using a literature value for the heat of sublimation of naphthalene, the heat of vaporization of water and average bond energies, given in Table 1 of the lab packet.1 Equations (1) and (5) were used to calculate the theoretical enthalpy of combustion of gaseous naphthalene, where n was the number of moles, m was the number of bonds, and ΔH was the average bond energy:
The week after, a recrystallization was performed on the previous week’s crude product. The product ethereal solution was first heated on a steam bath until dry. During the heating, a beaker of methanol was collected and also placed on the steam bath. Once the product was dry, it was cooled to room temperature and then placed in an ice-water bath. The now boiling methanol was added to the crude crystals and a recrystallization was performed. Once completed, the now purified product was collected via Buchner vacuum filtration and stored in drawer to dry for a week. Afterwards, a melting point range of the purified product was obtained by using a Mel-temp apparatus. Lastly, an
To apply thermal analysis to the two-component system, naphthalene-biphenyl at atmospheric temperature. The analysis will be represented by a solid-liquid phase diagram (freezing point diagram).
The purpose of this experiment is to separate a mixture of salicylic acid and naphthalene using extraction, recrystallization and sublimation techniques. Extraction is the separation of compounds from a mixture based on their relative solubilities in different solvents. Sublimation is the process of separation by which a substance transitions from the solid phase into the gas phase, skipping the liquid phase. Recrystallization involves dissolving a substance in an appropriate solvent then crystallizing it as it cools (impurities remain in solution). The melting points of the substances were determined in order to assess their purity and the percent recovery of pure naphthalene and salicylic acid were calculated. According to the results, the melting point of pure naphthalene was between 86°C -89°C range, whereas for pure salicylic acid was 167°C -170°C. Both determined melting points were higher compared to the literature value of 80.26°C and 158.6°C for pure naphthalene and salicylic acid respectively. Lastly, the percent recovery for pure naphthalene and salicylic acid were 17.7% and 71.2% accordingly.
The beaker was slowly heated on a hot plate with low stirring until most of the stilbene was dissolved. 0.4 g of pyridinium tribromide was measured and added to the beaker after 5 minutes of heating. Small amounts of ethanol were used to clean the sides of the beaker. The beaker was heated for an additional 10 minutes on low temperature. An ice bath was prepared. The beaker was removed from the hot plate and left to cool to room temperature. Once at room temperature, the beaker was placed in the ice bath for 15 minutes. The solid product was collected through vacuum filtration and the product was weighed and a melting point was taken. Waste was disposed of in the correct waste bins and lab bench was cleaned
The objectives of this lab are, as follows; to understand what occurs at the molecular level when a substance melts; to understand the primary purpose of melting point data; to demonstrate the technique for obtaining the melting point of an organic substance; and to explain the effect of impurities on the melting point of a substance. Through the experimentation of three substances, tetracosane, 1-tetradecanol and a mixture of the two, observations can be made in reference to melting point concerning polarity, molecular weight and purity of the substance. When comparing the two substances, it is evident that heavy molecule weight of tetracosane allowed