Names: Gerrell Fontenette, Jasper White Daisha Riddle, Derrick Portis CHM 1045L Section: 13 Date: 2/9/2012

LABORTATORY REPORT CHEMISTRY 1045 LAB EXPERIMENT 2 Identification of Substances By Physical Properties Purpose To become familiar with procedures used on evaluating physical properties and the use of these properties in identifying substances Reagents and Media Distilled water Ethyl Alcohol Cyclohexane Unknown solutions (liquid and solid) Naphthalene Tolene

Apparatus and Materials Balance Test tube rack 250-mL Beaker Dropper 10-mL pipet Capillary tubes 50-mL beakers 5-mL Graduated cylinder Small test-tubes Thermometer

Safety Precautions 1. Wear personal protective wear (lab coat and safety glasses). 2. Ensure a secure fit between the rubber hose and Bunsen burner and gas outlet to avoid leakage of gas into the laboratory 3. Use a crucible tongs when removing the beaker of hot water.

Names: Gerrell Fontenette, Jasper White Daisha Riddle, Derrick Portis CHM 1045L Section: 13 Date: 2/9/2012

Procedure A. Solubility 1. Take each of the three solvents (Water, Cyclohexane, and Ethyl Alcohol) and place 2 to 3-mL in three separate small test tubes. 2. Place a few crystals of naphthalene in each test tube 3. Use a cork to cover the top of the test tube and shake briefly 4. Record observations 5. Repeat procedure #1, 2, 3 using the other solute (toluene, unknown liquid, unknown solids) 6. Record conclusion using abbreviations S(soluble), SP(sparing soluble), and I(insoluble) B. Density 7. Weigh about 1.5g of your solid unknown to the nearest 0.001g and record the weight 8. Take the pipet and fill a dry 10-mL graduated cylinder with a solvent in which unknown insoluble. DO NOT LET THE LIQUID TOUCH THE SIDE OF THE CYLINDER. 9. Record the volume to the nearest 0.1-mL 10. Add the weighed solid the cylinder 11. Tap the cylinder against the table till the solid beneath the surface of the liquid. 12. Record the volume to the nearest 0.1-mL Density of a Liquid 13. Weigh a dry 50-mL Erlenmeyer flask to the nearest 0.001g. 14. Obtain at least 15-mL of the unknown liquid in a dry test tube. 15. Using a 10-mL pipet, add exactly 10-mL of the unknown liquid into the 50mL Erlenmeyer flask 16. Quickly weigh the flask containing the 10-mL to the nearest 0.0001g. 17. Using your CALIBRATED pipet and weight of this volume of unknown, calculate its density. 18. Record your results and SHOW your calculations Important Note: save the liquid for your boiling point determination C. Melting Point 19. Obtain a capillary tube and small rubber band 20. Seal one end of the capillary tube by carefully heating the end on the edge of the flame of a Bunsen burner, until the end completely closes. 21. Pulverize (beat) a small portion of your solid-unknown sample with the end of a test tube on a clean watch glass 22. Partially fill the capillary with your unknown by gently tapping the pulverized sample with the open end of the capillary to force some of the sample inside.

Names: Gerrell Fontenette, Jasper White Daisha Riddle, Derrick Portis CHM 1045L Section: 13 Date: 2/9/2012

23. Drop the capillary into a glass tube about 38 to 50 cm in the length, with the sealed end down to pack the sample into the bottom of the capillary tube. 24. Place the rubber band about 5 cm above the bulb on the thermometer and out of the liquid. 25. Carefully insert the capillary tube under the rubber band with the closed end at the bottom. 26. Place the thermometer with attached capillary into the beaker of water so that the sample is covered by water, the thermometer does not touch into the bottom of the beaker, and the open end of the capillary tube is above the surface of the water.. 27. Observe the sample in the capillary tube. 28. On the first drop of the solid melting, record the temperature range of that and when the solid has melted. 29. Using a thermometer (calibrated) and correct these temperatures to the true temperature and record the melting point and melting point range D. Boiling Point 30. Determine the boiling point of your solid unknown by adding about 3-mL to a dry test tube. 31. Fit the test tube with a two-hole rubber stopper that one slit insert your thermometer into the hole with the slit and one of your right-angle bend glass into the other hole. 32. Add one or two small boiling chips to the test tube to ensure even bottom into the sample. 33. Position the thermometer so that it is about 1cm above the surface of the unknown liquid. Clamp the test tube in the ring stand and connect to the right-angle-bend. Taking a length of rubber tubing that reaches to the sink. 34. Assemble your apparatus. 35. Heat the water gradually and water for change in temperature. 36. The temperature will become constant at the boiling point of the liquid. 37. Record the observed boiling point. 38. Correct the observed boiling to the true boiling point at room atmospheric pressure using your thermometer-calibration curve. The formal point (b.p. at 1 atm=760mm Hg) can now be calculated the nomograph. Your boiling point correction should not be more than +5C. E. Unknown Identification 39. Find the unknown substances contained in the table 2.1. 40. Compare the properties that you have determined for your unknowns with those on in the table. 41. Identify your unknowns and record your results.

Names: Gerrell Fontenette, Jasper White Daisha Riddle, Derrick Portis CHM 1045L Section: 13 Date: 2/9/2012

Procedure Modifications C. Melting Point 1. We filled the capillary tube with the substance up to 5cm within the tube. 2. We used another melting point apparatus named MSRS Digi Melt to find the melting point of the solid. 3. We place the capillary tube into the MSRS and observe the process through a designated microscope. 4. We set the temperature to reach a peak of 60C. D. Boiling Point 5. We decided to not use the water 6. We proceed by placing the test tube with liquid unknown substance directly over the fire. Observations A 1. The liquid unknown mixed with the water formed bubbles at the top of the solution B 2. During the density procedure, not all of the flakes fell to the bottom, and it abnormally took the flakes to fall to the bottom. C 3. During the melting point, the solid become a liquid with the first drop being recorded at 53.3C. Then the solid completely melted at 55C D 4. During the boiling point, the liquid completely evaporated in less than a minute. The temperature recorded at 67C indicates when the solution began to boil.

Names: Gerrell Fontenette, Jasper White Daisha Riddle, Derrick Portis CHM 1045L Section: 13 Date: 2/9/2012

Data A. Solubility Alcohol Water Insoluble Naphthalene Insoluble Toluene Soluble Liquid Unknown Insoluble Solid Unknown *To be expected [sparing soluble] B. Density Solid Final volume of liquid in cylinder Initial volume of liquid in cylinder Volume of Solid Weight of Solid

Cyclohexane Soluble Soluble *Soluble Soluble

Ethanol Sparing Soluble Soluble Soluble Soluble

6.2 mL 5.0 mL 1.2 mL 1.4971 g

Liquid Volume of Liquid Volume of luqid corrected for the pipet correction Weight of 50-mL Erlenmeyer plus~10mL of unknown Weight of 50-mL Erlenmeyer Weight of liquid

10.0 mL 9.88 mL 49.2115 g 41.4441 g 7.7674 g

Names: Gerrell Fontenette, Jasper White Daisha Riddle, Derrick Portis CHM 1045L Section: 13 Date: 2/9/2012

C. Melting Point of Solid Unknown Observe Melting Point Correction Observed melting point range Correction

55.3C 55.49 2.0C 2.0C

D. Boiling Point of Liquid Unknown Observed Corrected Estimated True

68.5 C 68.685C 72.755C

E. Unknown Identification Solid Unknown Liquid Unknown

p-Dichlorobenzene Hexane

Names: Gerrell Fontenette, Jasper White Daisha Riddle, Derrick Portis CHM 1045L Section: 13 Date: 2/9/2012

Discussion Ethanol is soluble in all alcohols except sparing soluble in NaphthaleneCyclohexane is expected to sparing soluble in the Hexane, and soluble for the rest of the alcoholWater is insoluble in all alcohol except for p-DichlorobenzeneAlso Cyclohexane was observed as soluble in the liquid unknown when it was expected to be sparing soluble We found the solid unknown through the melting point observations and concluded that substance was p-Dichlorobenzene. Our processed involved finding the melting point and matching the physical properties according to the provided chart. When finding the boiling point, we missed read the thermometer, as we waited for the liquid to completely evaporate. The procedure was to observe for the first sign of boiling. We collaborated with members of another group to find accurate boiling temperature. Conclusion We were taught using the following properties would help us identify the unknown substances which were: o Density o Solubility o Melting Point o Boiling Point We learned that the melting point is the phase for when solid becomes liquid Hexane has a higher melting point than its own boiling point It was easier to find the melting point of p-Dichlorobenzene instead of the boiling point, since the boiling point was high according to the chart. Finding the estimated true boiling point taught us that we can find the normal boiling point by decreasing the atmospheric pressure.