Using a 50 mL beaker and an analytical balance, 34.523g of urea was measured out and placed under the fume hood. At this time the heat plate was set to 80°C. A 100 mL beaker was placed on the balance and zeroed out, then used to measure out 40.117g of Chlorine Chloride. The 100 mL beaker containing Chlorine Chloride was placed on the heat plate and a small stir rod was added. The Urea was added to the Chlorine Chloride after waiting a little for the heat plate to warm up and warm the beaker up. The stir rod was turned on at this point, and then the Urea was added to the Chlorine Chloride. After moving the mixture around and pushing the solids closer to the stir rod with a spatula the mixture became a liquid solution and became very viscous so the rpm of the stir rod was upped. After sitting a while the solution was colorless and clear except for the small air bubbles in the solution. The mixture of the two solids had now turned into the desired solution of reline.
After the reline had time to cool a coulometric titrator was used to test the percent mass of water in the reline solution. This was done by setting coulometric titrator was turned on and put into data collection mode. A small sample of the reline was put into the titrator by using a pipet that was put on a balance. This was used to determine the mass of the sample used so it could be input into the instrument. The reline was dropped into the titrator and the mass of the sample was recorded and put into the instrument so that the titration could start. After a little the percent water by weight was given and recorded.
After the reline had time to cool a coulometric titrator was used to test the percent mass of water in the reline solution. This was done by setting coulometric titrator was turned on and put into data collection mode. A small sample of the reline was put into the titrator by using a pipet that was put on a balance. This was used to determine the mass of the sample used so it could be input into the instrument. The reline was dropped into the titrator and the mass of the sample was recorded and put into the instrument so that the titration could start. After a little the percent water by weight was given and recorded.
With the reline made, the heat plate was turned on once again and set to 40°C. 8.4mg of HAuCl4 was measured out on a balance in a 50 mL beaker and added to 5 mL of reline until it was dissolved. This was placed on the heat plate and stirred.While that was warming up 4.4mg of NaBH4 was added to another 50 mL beaker and also given 5mL of reline and placed on the heat plate next to the other beaker with the gold. After stirring both mixtures until homogeneous, the NaBH4 reline solution was slowly dripped into the HAuCl4 reline solution. This caused the color of the HAuCl4 reline solution to go from a yellow clear liquid to a dark purple or black solution. The solution was stirred for several minutes to ensure the reaction had completed.
The gold nanoparticle solution was extracted from the beaker using a micropipette and put into six 1.5 mL centrifuge tubes, each tube getting 1 mL of the solution. Once each tube was filled they were placed into the centrifuge that was set to 10000 rpm for 5 min. The centrifuging was repeated till the gold nanoparticles came out of solution and became stuck on the walls of the tube or collected on the bottom of the tube. The solution was clear and colorless rather then dark purple at this point. The gold nanoparticles were then out of solution, so the reline was able to be taken out of all but two of the tubes with normal pipet. The other two tubes that still had reline were removed and placed in storage for later, this was because one of the tubes is needed for UV-Vis and the other as backup or a second point for the UV-Vis. The other four tubes with no reline were going to go through a process of cleaning the gold nanoparticles of the reline, as this was required for the AFM. This cleaning process consists of first adding one mL of ethanol to the tubes. Then the gold was put back into solution with the ethanol that was added, this was done when the tubes were vortexed and sonicated, and when the gold was back into solution they were put but back into the centrifuge for 10 min at 10000rpm or till they came back out of solution. The ethanol was removed and one mL of new ethanol was added. On the third run through new ethanol was added and the gold was put back into solution in prep for the tests. Two carbon stickers were placed on the SEM plate and two mica plates were prepped. The preparation process for the mica plates were to hole punch circles of mica from a mica sheet and use tape to remove the first few layers and then placing them in a petri dish. One drop from one of the tubes was added to one of the carbon plates and then the rest of the tube was set aside for storage. This was repeated on the rest of the carbon and mica plates. All four of the plates were covered and given time to allow the ethanol to evaporate.
The gold nanoparticle solution was extracted from the beaker using a micropipette and put into six 1.5 mL centrifuge tubes, each tube getting 1 mL of the solution. Once each tube was filled they were placed into the centrifuge that was set to 10000 rpm for 5 min. The centrifuging was repeated till the gold nanoparticles came out of solution and became stuck on the walls of the tube or collected on the bottom of the tube. The solution was clear and colorless rather then dark purple at this point. The gold nanoparticles were then out of solution, so the reline was able to be taken out of all but two of the tubes with normal pipet. The other two tubes that still had reline were removed and placed in storage for later, this was because one of the tubes is needed for UV-Vis and the other as backup or a second point for the UV-Vis. The other four tubes with no reline were going to go through a process of cleaning the gold nanoparticles of the reline, as this was required for the AFM. This cleaning process consists of first adding one mL of ethanol to the tubes. Then the gold was put back into solution with the ethanol that was added, this was done when the tubes were vortexed and sonicated, and when the gold was back into solution they were put but back into the centrifuge for 10 min at 10000rpm or till they came back out of solution. The ethanol was removed and one mL of new ethanol was added. On the third run through new ethanol was added and the gold was put back into solution in prep for the tests. Two carbon stickers were placed on the SEM plate and two mica plates were prepped. The preparation process for the mica plates were to hole punch circles of mica from a mica sheet and use tape to remove the first few layers and then placing them in a petri dish. One drop from one of the tubes was added to one of the carbon plates and then the rest of the tube was set aside for storage. This was repeated on the rest of the carbon and mica plates. All four of the plates were covered and given time to allow the ethanol to evaporate.
The two tubes that were left over were taken and drained of three fourths or 0.75 mL of the reline in both the tubes using a micropipette. Then 0.75 mL of ethanol was added to both of the tubes. Both of the tubes were sonicated and vortexed so that a homogeneous mixture is created between the reline and ethanol. Four more tubes were pulled out and one mL of ethanol was added to each of the tubes. Once the UV-Vis was turned on and the ethanol background was set, using a pipet, the tube with the reline ethanol solution was put into the quartz cuvette. The other two tubes filled with ethanol were squeezed into the cuvette and the solution was mixed by sucking the solution into the pipet and squeezing it back into the cuvette multiple times. After this the UV-Vis was used to test the solution and the results which would be a bump in the 500-600 range. The AFM was also tested after it was confirmed that something was made.
This process was repeated except the synthesis of reline but with different concentrations of water, 2.5 mL of water, 5 mL of water, and 7.5mL of water from the same batch of reline that was made at the beginning.
This process was repeated except the synthesis of reline but with different concentrations of water, 2.5 mL of water, 5 mL of water, and 7.5mL of water from the same batch of reline that was made at the beginning.