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The effect of monomer, initiator and catalyst ratios on polymer chain length and strength test of polycaprolactone.

By Thayer Stowers Abstract The goal for this lab is to create polymers using variable amounts of initiator and catalyst and to test if longer strands of polymers have greater force resistance than shorter monomer chains. Polymers were made using scoopula and puck molds. Assigned amounts of monomer, initiator and catalyst were used. Two different tests were created to test the strength of each polymer. It was expected that longer stranded polymers are stronger because there are greater intermolecular forces. The data from the rodtest show that as initiator amounts decrease the strength of the polymer increases. The mass drop test data was inconclusive because of inconsistencies in testing. Introduction The goal of this lab was to polymerize monomers into variable length polymers and design a testing method to assess the physical properties of different variable length polymers and to explore the relationship between polymer chain length and polymer strength. A monomer is the small molecule of the polymer that link together to form polymers. Polymers are mostly made of compounds with a similar structure but have different lengths. Chain growing polymerization is when sequentially adding one monomer to a polymer at a time to the end of a chain. An initiator is what begins the process of polymerization by making the monomer change its structure by unwinding. The unwound monomer molecule will cause a reaction to another monomer molecule to also unwind, causing the two unwound molecules to bond. Intermolecular forces between polymer chains can determine a polymers Properties. Because polymer chains are long, the interchange forces are expanded beyond the attractions between molecules. The catalyst is what lowers the energy that is used to start a reaction. It will allow the reaction to happen at a low temperature and will allow it to happen more rapidly. Polymers are made up of long change molecules, they have a low density, low melting point, and are usually unreactive for its chemical properties. Chain growing polarization will create our polymers, however, the question that needs to be answered is how much catalyst and initiator will be needed to see the polymerized monomers made into variable length polymers. As the Initiator goes down, the Polymer chains get longer, the polymer strength increase because of the intermolecular forces goes up. Methods: This experiment uses potentially dangerous chemicals. The specific items that should be used during this lab for safety precautions should be eye protection, lab apron and disposable gloves that should be worn when using potentially hazardous chemicals. All work must be conducted in fume hoods. Two scoopula molds and one puck mold must be created in order to shape the polymer. Two create the scoopula molds, two slightly mismatched scoopula’s and set them together. Cut a piece of metaled backed tape and firmly tape the two scoopula’s together. Next thoroughly grease the inside of the scoopula mold with the designated test tube brush. Next use the vacuum grease and put a plug in the bottom of the scoopula mold and seal it with more tape. To be sure that there are no cracks or leeks in the scoopula, add a little water into the mold and if there are no sign of leeks, the scoopula mold will

work. In order to create the disk, get a tin foil disk and cover the inside with grease in order to make it ready for the mold. In order for the polymerization reaction to occur, first you must use a magnetic stir bar in an Erlenmeyer flask. Add 85ml of caprolactone to the flask. There were several different groups that used different amounts to make chain lengths. Our group would add 0.29ml of 1-octanol using the 1-ml syringes. Next, use the stands in the fume hoods and a clamp, rearrange the hot plate, the Erlenmeyer flask and thermometer in order for the reservoir bulb of the thermometer is submerged in the mixture but does not come in contact with the stir bar in the bottom. Slowly heat the mixture to 120-130 C with rapid stirring from the stir bar. Next, record the time when the reactants arrive at 120 C and regularly check the viscosity of the mixture by lifting the thermometer out of the flask and watch how the mixture drips from the thermometer. Once the viscosity of the mixture increases to a syrupy mixture. The time it takes to change the viscosity depends on the polymers monomer to initial and catalyst ratio. Lastly pour the reaction contents into the set molds. Place molds in the oven. The test that was used on the Polymer from scoopula molds was to place it between two tables and put increasing amounts of weight on the part that was directly above the ground and placing a metal hook on the rod and placing more weight on and write down what weight the rod broke on. For the puck a hammer was set on a swing arm and would write down the heights that the pucks would break. To better explain, we were testing the heights that a puck would break on impact by using a hammer on a swing arm, hitting the puck. Results Table 1-Rod Breaking Test: This table shows the set weights set on each of the polymers during the test. Group Letter Test 1 (grams) Test 2 (grams) average breaking point (grams) A B D E 650 800 1032 982 550 600 800 1032 982

Table 2- Puck impact Test: This test shows the level that the pucks from set polymers broke from set heights. Angle Degree From Drop Group Letter Test 1 A B 15deg 60deg Test 2 Test 3 Test 4 Test 5 Test 6 n/a n/a n/a n/a n/a n/a n/a

15deg 30 deg n/a


30deg 60deg

15deg 45 deg n/a



90deg 30 deg 30 deg 15 deg 75 deg n/a n/a n/a n/a n/a n/a n/a n/a n/a

15deg (spoon not puck) 30deg n/a 15deg (Square not puck) 30deg n/a 45deg n/a n/a

The puck test confirms that the polymers with less catalyst and initiator are more impact resistant. Both tests show that D is the strongest as well as the most impact resistant because the initiator is lower causing it to be Discussion The purpose of this lab was to see if longer or shorter stranded polymers were stronger/more impact resistant. The polymer has shorter strands if more of the catalyst and initiator is used in the creation. After the weight test and impact test the results that were found were that polymers with longer strands were stronger and impact resistant. In the impact test, in test one, polymer B had a higher impact resistance than those of the other Polymers, except D. However, in the remaining tests, it shattered at or below the other polymers, except D. Since D had the most accurate results of being strong and shatter resistant, it is the most favorable of the polymers created. The Rod test concludes that the polymers with less of a catalyst and initiator are stronger than those that are made with more catalyst and initiator. This is due to the fact that the polymers with less catalyst and initiator have fewer, longer chains which could provide more support making it stronger. With this lab, I am not satisfied with the results that we had gotten because, with the hammer puck test, the pucks would have had some impact after the first drop, and if it didn’t creak, it would have been affected, causing it to be inaccurate. And with the puck, we had run out of pucks, making the testing inaccurate. I was not present during the Metal rod test, and was not able to come to an opinion with this test. If I was going to reconstruct this lab, I would have created more scoopula molds for each set polymer to create an accurate test rather than the pucks.