CHANGES OF STATE EXPERIMENT 5 OBJECTIVE The objective of this experiment is to determine the freezing point using a graph of temperature versus time and to determine melting points. EQUIPMENT AND CHEMICALS Paradichlorobenzene Biphenyl 400 ml beaker 100 oC thermometer Ring stand with wire screen Split cork Melting point tubes Bunsen burner DISCUSSION Matter exists in three states: solid, liquid, or gas. The particular state that matter exists in depends upon the temperature and atmospheric pressure. When sufficient heat is applied so that the individual molecules can overcome their attraction for each other, a transition from one physical state to another occurs. The freezing point is the temperature at which a liquid begins to change to a solid and at which point both states of matter (solid and liquid) exists at the same time. Therefore, the melting and freezing points are the same temperature. When a substance goes from one state of matter to another, it is referred to as a change of state. PROCEDURE PART A DETERMINATION OF FREEZING POINT The paradichlorobenzene will be heated past its melting point and allowed to cool. While cooling, the temperature and time will be recorded. A graph will be plotted to determine the freezing point of he paradichlorobenzene. 1. Set up the apparatus as demonstrated by the instructor. 2. There will be a beaker containing boiling water set up on a hot plate. Insert a thermometer into a large test tube containing paradichlorobenzene, place the test tube into the boiling water and allow the paradichlorobenzene to melt. Continue to heat until the temperature of the dichlorobenzene is above 65 oC. 41 3. While the paradichlorobenzene is heating, add 300 ml of water to your apparatus and heat the water to 40 oC. 4. Quickly transfer the melted paradichlorobenzene test tube to your beaker with the 40 oC water and support as shown in the demonstration apparatus. 5. Gently stir the paradichlorobenzene with the thermometer while it cools. When the temperature in the test tube reaches 65 oC, record the temperature every 30 seconds until the paradichlorobenzene completely solidifies. 6. Plot a cooling curve using the temperature versus time data. Plot time on the horizontal axis and temperature on the vertical axis. 6. Extrapolate the temperature plateau on your graph across to the horizontal axis to find the freezing point of the paradichlorobenzene. PART B: MELTING POINTS 1. Dab the open end of a melting point tube into a small sample of biphenyl. 2. Turn the tube open end up and gently tap bottom of the tube to pack the biphenyl to the bottom of the tube. Repeat this process until there is about 5mm of sample packed into the bottom of the tube. 3. Prepare two samples as above. 4. Attach the melting point tube (the open end up) to the end of the thermometer using a rubber band. 42 5. Setup the melting point apparatus as demonstrated by the instructor. 6. Heat the water rapidly until the biphenyl in the melting point melts and note this temperature. 7. Cool the water bath well below the temperature at which the biphenyl melted. 8. Attach the second melting point tube with the biphenyl in it to the thermometer. 9. Rapidly heat the water to about 10 oC below the melting point noted earlier. 10. Slowly heat the water and note the temperature range at which the biphenyl begins to melt until it completely melts. 11. Obtain an unknown compound and determine its melting point range. 43 This page left intentionally blank. 44 NAME ____________________ DATE ____________________ SECTION _________________ CHANGES OF STATE REPORT SHEET EXPERIMENT 5 COOLING CURVE DATA Time Temperature Time 0:00 0 7:00 14:00 0:30 7:30 14:30 1:00 8:00 15:00 1:30 8:30 15:30 2:00 9:00 16:00 2:30 9:30 16:30 3:00 10:00 17:00 3:30 10:30 17:30 4:00 11:00 18:00 4:30 11:30 18:30 5:00 12:00 19:00 5:30 12:30 19:30 6:00 13:00 20:00 6:30 13:30 20:30 65 C Temperature Time Temperature MELTING POINTS Rapid MP Gradual MP Melting point of biphenyl (69 – 71 oC) ___________ oC ___________ oC Melting point of unknown ___________ oC ___________ oC 45 Freezing Point: ________ oC Paradichlorobenzene Cooling Curve 46
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