Laboratory Experiment: Allotropic Forms of Sulfur Objective In this experiment, the different forms of sulfur will be examined after they are produced. Special emphasis will be placed on the physical appearance of the test tube sample and the magnified crystals. The changes observed will be physical changes, because the sulfur identity will not change at each step. Materials Test Tube (1) Test Tube Holder Large Beaker Sulfur Bunsen Burner Magnifying Glass Filter Paper Funnel Introduction Sulfur exists in several different allotropic forms depending on the surrounding conditions (pressure, temperature) and the arrangement of groups of sulfur atoms. Sulfur is an element well known to the ancients, and is referred to in Genesis as “brimstone”. In this lab, we will produce monoclinic sulfur by SLOWLY melting some sulfur in a test tube and cooling it in filter paper. The monoclinic crystals will then be examined under a magnifying glass. A 2nd test tube will also be heated, this time to boiling, and the sulfur will be poured into a beaker of cold water, thus producing amorphous sulfur. The amorphous sulfur will also be examined for physical characteristics. Finally, after a few days, the monoclinic sulfur crystals and the amorphous sulfur will be re-examined. Pre-Lab Worksheet: Allotropic Forms of Sulfur Please use the helpful sources (internet, dictionary, your textbook, etc.) to answer the following questions. 1. What is an allotrope? 2. Which group on the periodic table does sulfur belong to? 3. How is sulfur naturally found? 4. What are two allotropic forms of sulfur? Please sketch each crystal structure. 5. What does the word “amorphous” mean? 6. What is a diatomic molecule? 7. What is a polyatomic molecule? 8. What are the formulas for each type of polyatomic molecule sulfur can exist as? 9. What does the word “viscous” mean? 10. Sulfur melts to form a ________ , _________ liquid, and burns with a ________ flame. 11. What is the melting point of sulfur? The boiling point? 12. What are three examples of how sulfur can exist combined with other elements? Please list the chemical formulas for these substances. 13. How does the polyatomic molecule S8 exist? Please sketch either a ball and stick model or a space-filling model. Procedure Part A 1. Fold your filter paper into a cone-shaped funnel. Lay these aside for later use. 2. Fill a test tube 1/3 full with sulfur. 3. CAREFULLY melt the sulfur by holding the tube in an inclined position about 4 inches above a small Bunsen flame. Rotate the tube slowly as the sulfur melts. At no time should the color of the sulfur turn dark brown!! 4. Using the funnel as a support for your filter paper, pour the melted sulfur into it. As soon as crystals have formed from the edge to the center of the surface, and just before it all turns solid, unfold the paper. Examine the crystals with your magnifying glass. 5. Make a drawing of the crystals in your lab notebook. 6. Observe crystals after 48 hours and record changes, if any occur. (Mark filter paper with your name.) Part B 1. Fill a test tube 1/3 full with sulfur. 2. Heat sulfur with the Bunsen flame until it boils. Tip the tube now and then and note the color and consistency changes. (DO NOT BECOME ALARMED IF THE SULFUR STARTS TO BURN). Pour the boiling sulfur into a beaker of cold water, keeping the mouth of the tube moving in a circle. 3. When threads of sulfur have cooled (a few minutes), pour away the water. Observe and touch the threads for texture, color, etc. Document your observations in your lab notebook. 4. Place sulfur on a paper towel marked with your name. Observe physical characteristics over the next 48 hours. Data and Observations - in your lab notebook (you may take photographs) Observations During Melting of Sulfur Physical Characteristics of Sulfur Crystals Sketch of Monoclinic Sulfur Crystals Observations of Crystals in 48 hours Observations During Boiling of Sulfur Physical Characteristics of Amorphous Sulfur Sketch of Amorphous Sulfur Observations of Amorphous sulfur in 48 hours Part A Part B Clean-up Procedures 1. After the test tubes have cooled, return them to the central location where you received them. Since the sulfur is insoluble in water, the test tubes will not come clean, and will be used again for this lab in future classes. 2. Label your samples and place them at the back of the room for future observations. 3. Clean and dry all of your equipment and return it to your drawer. You can use the soapy squirt bottle solution under the sink for cleaning equipment. 4. Using damp paper towel, wipe the lab benches down to remove any traces of sulfur powder. Discard this in the trash can. 5. Using a damp cloth, wipe the lab benches down a second time. 6. (Last hour of the day) When the Bunsen burners are cool, please return them to the appropriate location. Please put the strikers away too. 7. Place the soapy solution back under the sink. 8. Double-check your work area for cleanliness. 9. Wash your hands with soap and water. Conclusions and Questions You have observed six different forms of sulfur in this activity. First, the powdered sulfur you began with was the orthorhombic allotrope. After being heated carefully, the sulfur melted to pale yellow λ-sulfur (lambda-sulfur). This liquid solidified and formed monoclinic sulfur crystals. When a second sample of sulfur was heated more strongly, sulfur vapor was emitted, and a more viscous blackish liquid formed, which is called μ-sulfur (Mu-sulfur). When the μ-sulfur was poured into the cool water, amorphous sulfur was observed. After several days, the amorphous allotrope will turn brittle and return to the orthorhombic form. Each form of sulfur has a different molecular structure. The following table summarizes the various allotropic forms of sulfur. Allotropic Forms of Sulfur Form Orthorhombic Monoclinic Amorphous Lambda Mu Vapor Formula Structure S8 Rings Varies Chains and rings Tangled robe Solid-liquid S2 molecules S8 Rings Appearance Rhombus Needles Phase Solid Solid S8 Rings Sn Chains Thin, yellow Liquid Thick, red- yellow black Liquid gas Questions 1. Compare and contrast each liquid form of sulfur from each part of this experiment. 2. When the liquid Mu-sulfur forms during Part B of this experiment, the structure changes from a ring structure to a chain structure. Knowing this information, can you speculate why the liquid became more viscous compared to the pale yellow liquid from Part A? 3. Why does the color change during heating? 4. Describe the process by which you produced monoclinic sulfur. What properties differentiate it from other allotropic forms of sulfur? 5. Describe the process by which you produced amorphous sulfur. What properties differentiate it from other allotropic forms of sulfur? 6. When sulfur is produced in large quantities for industry, it is often stored in large piles outside. This used to be done with large piles of road salt, but this practice caused considerable environmental damage and is no longer done. Explain why it is still feasible to store sulfur in this manner. 7. Research and list 4 uses of sulfur.