Identifying An Unknown Solid Using Melting Point

I. LIQUID - Identification of an Unknown Liquid: Using the physical properties of Solubility, Density, and Boiling Point.

After each of the solids were completely dry, each was placed into a MelTemp device. The temperature at which each solid began to melt and completed melting was recorded.

In this lab, liquid-liquid extraction was performed to isolate a mixture of benzocaine and benzoic acid. 2.0107 grams of the mixture was first weighed out for the trials. When HCl was added to the mixture for the first acid extraction of benzocaine, an emulsion formed during inversion and venting that prevented a defined separation of the two layers. 8 mL of water was therefore added before continuing the extraction. The addition of NaOH then turned the top aqueous layer basic, indicated by the pH strips that turned blue when tested. A vacuum filtration isolated 0.29 grams of benzocaine and a MelTemp apparatus measured the crystal’s melting point ranges to be 85.1C-87.4C. For the base extraction of benzoic acid, the aqueous layers were retrieved

In determining the melting point range of the aspirin, a capillary tube (sealed at one end) was one-third-filled with the dried aspirin. The capillary tube and a thermometer were immersed in an oil bath. The temperature at which the solid started to melt and the temperature when the entire sample was completely liquefied were recorded as the melting point temperature range.

Other substances that dissolve in water also lower the freezing point of the solution. The amount by which the freezing point is lowered depends only on the number of molecules dissolved, not on their chemical nature. This is an example of a colligative property. In this project, you'll investigate different substances to see how they affect the rate at which ice cubes melt. You'll test substances that dissolve in water (i.e., soluble substances), like salt and sugar, as well as substances that don't dissolve in water (i.e., insoluble substances), like sand and pepper. Which substances will speed up the melting of the ice?

4- chlorobenzoic acid which was the aqueous layer has a theoretical melting point of 240-243°C, the organic layer, 4-chlorobenzyl alcohol has a theoretical melting point of 68-71°C. During our experiment we were unable to collect any data for the organic

pH was recorded every time 1.00 mL of NaOH was added to beaker. When the amount of NaOH added to the beaker was about 5.00 mL away from the expected end point, NaOH was added very slowly. Approximately 0.20 mL of NaOH was added until the pH made a jump. The pH was recorded until it reached ~12. This was repeated two more times. The pKa of each trial are determined using the graphs made on excel.

Three grams of a mixture containing Benzoic Acid and Naphthalene was obtained and placed in 100 ml beaker and added 30 ml of ethyl acetate for dissolving the mixture. A small amount (1-2 drops) of this mixture was separated into a test tube. This test tube was covered and labelled as “M” (mixture). This was set to the side and used the following week for the second part of lab. The content in the beaker was then transferred into separatory funnel. 10 ml of 1 M NaOH added to the content and placed the stopper in the funnel. In the hood separatory funnel was gently shaken for approximately one minute and vent the air out for five seconds. We repeated the same process in the same manner one more time by adding 10ml of 1M NaOH.

Substances A and B have an appearance of a white solid like. Substances A and B were put into a test tube and on the Bunsen burner. As a result, B melted faster than A. A was slow to melt. The reason why B melted faster than A is because it has a lower boiling point than substance A which made it melt faster. It also shows that A needs more energy than B to be broken down.

Discussion: As seen in the melting point determination, the average melting point range of the product was 172.2-185.3ºC. The melting points of the possible products are listed as 101ºC for o-methoxybenzoic acid, 110ºC for m- methoxybenzoic acid, and 185ºC for p- methoxybenzoic acid. As the melting point of the sample

In this experiment, the identity of an unknown compound will be deduced from analysis of physical properties, boiling points, IR spectra, chemical tests, and melting points of derivatives. This experiment allows for individual selection of chemical tests, order of steps, and additional analysis, as necessary, based on what is needed to determine identity of unknown.

Melting range would be closely related to a mixed sample whose constituents are most identical. In other words, melting point will have a wide range and would be below 200°C and above 95°C.

An ice bath was prepared in a large beaker and a small cotton ball was obtained. 0.5 g of acetanilide, 0.9 g of NaBr, 3mL of ethanol and 2.5 mL acetic acid was measured and gathered into 50mL beakers. In a fume hood, the measured amounts of acetanilide, NaBr, ethanol and acetic acid were mixed in a 25mL Erlenmeyer flask with a stir bar. The flask was plugged with the cotton ball and placed in an ice bath on top of a stir plate. The stir feature was turned on a medium speed. 7mL of bleach was obtained and was slowly added to the stirring flask in the ice bath. Once all the bleach was added, stirring continued for another 2 minutes and then the flask was removed from the ice bath and left to warm up to room temperature. 0.8mL of saturated sodium thiosulfate solution and 0.5mL of NaOH solution were collected in small beakers. The two solutions were added to the flask at room temperature. The flask was gently stirred. Vacuum filtration was used to remove the crude product. The product was weighed and a melting point was taken. The crude product was placed into a clean 25mL Erlenmeyer flask. A large beaker with 50/50 ethanol/water

The purpose of this lab was to study colligative properties. These properties are properties that are affected when a solute is added to a solvent. Thus, the amount is important, not the actual type of substance, for the colligative properties. A couple types of this property are the freezing point and boiling point of a substance. (1)

Brittain, C. G. (2009). Using Melting Point to Determine Purity of Crystalline Solids. Retrieved from http://www.chm.uri.edu/mmcgregor/chm228/use_of_melting_point_apparatus.pdf