June 19th, 2019

1. The 200 grams of KI that I recently ordered was transferred into a container that must have had some kind of residual contamination in it because it converted a portion of the iodide to iodine. It was only enough to discolor the crystals and as I had planned to convert the majority of it to HI(aq) for my work on metal iodides it isn't a huge problem. However, I did want some pure KI crystals to use to create a KI solution for analytical purposes. So I am going to recrystallize the KI.

2. Dissolved all 200 grams of KI into 150 mL of boiling water.

3. Filtered the solution through cotton to remove any particulates. There was a small amount of a black material in the KI crystals which was easily removed during the filtration.

4. By the time all of the rinses were complete the total volume of the solution was slightly greater than 300 mL. 200 grams of KI dissolves in ~97 mL of boiling water so I put the beaker with the solution back on the hotplate to evaporate some of the water.

5. The solution was boiled down to approximately 150 mL volume before the sides of the beaker were rinsed with a minimal amount of water and the beaker was put on the bench in the shed on a cooling rack and covered with a watch glass. I am going to leave it there overnight to see if I can get crystals of potassium iodide to grow.

 

June 20th, 2019

1. I removed the slurry of potassium iodide crystals from the refrigerator and transferred them to a cooler full of ice. I allowed the slurry to get as cold as possible before proceeding to the next step.

2. The potassium iodide slurry was vacuum filtered and the crystals were allowed to suction dry for about 10 minutes.

3. The damp crystals were then transferred to a ceramic baking dish and heated in a toaster oven at 350 oF until some of the crystals had just begun to completely dry.

4. The dish was taken out of the oven and the crystals of the hydrate were scrapped off the dish using a new razor blade. As the crust of still damn but very hot KI crystals was broken up they dried out more gently and formed beautiful solid crystals of KI hydrate. All of the rinses and filter papers used in working with the crystals were collected and transferred to the Iodine Recycling jar. This will be used for future runs of HI or for converting to I2.

Potassium Iodide Monohydrate Crystals and Iodine Recycling Jar


5. A 50 mL beaker was thoroughly cleaned and set up on the stir plate with a small stir bar. To this was added a 1 gram bar of .9995 platinum metal. 10 mL of aqua regia was added to the beaker and the stirring was turned on slow speed. The beaker was covered with a watch glass and the heat was turned on high.

6.The reaction proceeded slowly. As it progressed the aqua regia was slowly boiled off and was topped off with 10 mL portions of aqua regia as needed. As the reaction progressed the solution took on an orange color which intensified as it went on.

7. It took well over 100 mL of aqua regia to make enough progress through the platinum bar to be able to tell that progress was being made at all! I have had it stirring in boiling aqua regia now for 3.5 hours and if the rate of progress up until now is anything to go on this could literally take until tomorrow morning were I to keep at it. I will continue adding aqua regia to the beaker until I go to bed tonight and tomorrow morning I will continue working on dissolving the metal after I pick up some more muriatic acid from the store.

Begin Dissolving Platinum in Aqua Regia
Platinum Metal Dissolving in Aqua Regia
Platinum After Being Partially Dissolved 1 (1200x mag.)
Platinum After Being Partially Dissolved 2 (1200x mag.)

June 21st, 2019

1. I continued dissolving the platinum bar in the same manner as yesterday. As the acids in the beaker boiled off they were replaced with 10 mL portions of aqua regia made fresh before use everytime. By the time it was all said and done I had used over 200 mL of aqua regia to dissolve 1 gram of platinum and the process took a combined total of approximately 9 hours. As the acid in the beaker began to become sluggish in its reaction even after addition of fresh acid the solution was decanted and combined with other batches of acid used in the platinum dissolution.

2. I noticed as the reaction progressed that the platinum was dissolving into the aqua regia at a satisfactory rate at temperatures below the maximum. I had initially thought that the platnium wasn't reacting unless the aqua regia was at a rolling boil. However, for the last couple of hours of the reaction I turned the heat down to the point where it was only lightly boiling and the platinum seemed to react at the same rate as before. With the heat turned down the rate of loss of the aqua regia dropped dramatically.

3. Once all of the platinum had been dissolved I combined all the aqua regia solutions that I had used to carry out the reaction. The total volume of the brilliantly orange solution that resulted was about 35 mL. The volume of the solution was then reduced over low heat with stirring to 10 mL.

4. A small amount (~5 mL) of 16 M HNO3 was added to the chloroplatinic acid and this was allowed to evaporate away with the rest of the solution. This was done a total of 4 times. The purpose of this was to try to remove as much excess Cl- ion as possible. Also, chloroplatinic acid is insoluble in concentrated HNO3 and I was hoping that when all was said and done the chloroplatinic acid would crystallize out of solution. No such luck. So I transferred the chloroplatinic acid solution to a 10 mL volumetric flask and then q.s. with distilled water. I transferred this solution to a scintillation vial, labeled it, and put it on the shelf with the rest of the analytical reagents.

1 gram of platinum = (1/195.084) moles platinum = 0.00512 moles of platinum
0.00512 moles of platinum → 0.00512 moles chloroplatinic acid
0.00512 moles / (10/1000) mL solution =
0.5126 (so ~0.5) molar solution of chloroplatinic acid

June 22nd, 2019

1. 0.98 grams of black palladium metal powder that had been precipitated out of a solution of palladium nitrate in nitric acid using sodium borohydride was dissolved in 10 mL of aqua regia. At first nothing much happened beyond the acid becoming dark but on mild heating the palladium rapidly dissolved with the concurrent evolution of nitrogen dioxide gas. Luckily the watch glass covering the beaker caught any of the solution that might otherwise have been sprayed out of the beaker by the reaction.

2. After rinsing the droplets on the sides of the beaker and the watch glass back into the solution the total volume was about 20 mL. This was reduced down to just under 10 mL in volume with gentle heating and stirring.

3. The deep red solution was transferred to a graduated cylinder in order to measure all of the washes necessary to rinse the PdCl2 solution into a scintillation vial for storage.

0.98 grams palladium = (1/106.42) moles palladium = 0.00939 moles of palladium
0.00939 moles of palladium → 0.00939 moles palladous chloride
0.00939 moles / (12/1000) mL solution =
0.783 molar solution of palladous chloride

Palladous Chloride PdCl2 Dissolving in Aqua Regia

4. 1 gram of rhenium was dissolved in a small amount of 16 molar HNO3. This was then transferred to a 10 mL graduated cylinder and the solution was q.s. to 9 mL. This was transferred to a scintillation vial along with two 1 mL washes of the clinder.

1 grams rhenium = (1/186.207) moles rhenium = 0.00537 moles of rhenium
0.00537 moles of rhenium → 0.00269 moles perrhenic acid
0.00269 moles / (11/1000) mL solution =
0.244 molar solution of perrhenic acid

June 23rd, 2019

1. KI + I2 + H2O → KI3 • H2O
Prepared potassium triiodide by dissolving 10 grams (KI = 166.0028 g/mol, 10 grams of KI = 0.06023 moles KI) of potassium iodide in 10 mL of boiling water . To this was added (I2 = 253.80894 g/mol, 0.06023 moles of I2 =  15.289 grams crystal iodine) and this was heated and stirred until all of the iodine reacted. As the reaction progressed an extra 3 grams of KI was added to the beaker. This should place the KI firmly in excess and this can be filtered off after crystallization of the product and added to Iodine Recycling. 

2. Although the stoichiometric amount of iodine was added to the KI solution much of it seemed to not react. Losses of iodine to evaporation were significant. The solution was boiled for a short while until the iodine crystallizing on the walls of the beaker had halfway covered the mouth of the beaker in a film of iodine crystals. 

3. The remaining iodine was filtered out, washed with water, patted dry with paper towels, and returned to the bottle of Recycled Iodine in the inventory. All of the washes and filter papers were put into the Iodine Recycling Jar. In the end 30 mL of an aqueous solution of unknown concentration of potassium iodide was obtained. 

Iodine Crystals Formed During the Reaction
Solution of Potassium Triiodide

4. A solution of thallium(I) sulfate was prepared by dissolving 0.92 grams of elemental thallium in dilute sulfuric acid. (Tl = 204.3833 g/mol, 0.92 grams = 0.00450 moles Tl) The final volume of the solution was 12 mL. This gives a final concentration of 0.00450 moles / (12 mL /1000 mL per liter) = 0.375 molar Tl2SO4

June 24th, 2019

1. Dissolved 1 gram of ruthenium metal by combining it with a mixture of 4 grams of KOH and 4 grams of KNO3 and then melting the mixture in a crucible over a medium flame. The ruthenium dissolved in the fused salts producing an extremely dark green melt. The melt solidified when removed from the heat and then quickly began to turn a deep red-orange color in the humid air.

2. The melt was dissolved in ~75 mL water to produce a dark red-orange solution. This was then evaporated over low heat using gentle stirring until it's volume was reduced to about 20 mL. The beaker was covered and put on ice. 

3. After 45 minutes the beaker was removed from the ice and the mother liquor was drained from the crystals. The crystals were put in an evaporating dish and dried overnight in a desiccator with dry magnesium sulfate. It produced black crystals that were scraped up and put into a scintillation vial. The mother liquor was combined with the washes from the beakers and the evaporating dish and the ~30 mL of liquid was sealed in scintillation vials to await further processing. 

June 25th, 2019

1. Dissolved 1 gram of .999 gold in 10 mL of aqua regia. The process started out at room temperate and then the heat was turned on high. However, even starting cold the entire bar of gold had dissolved in about 15 minutes (MUCH shorter than platinum!) The solution was reduced in volume with medium heating and gentle stirring and then transferred to a scintillation vial. After adding in the washes the final volume of the chloroauric acid solution was 11 mL. 

Au + HNO3 + 4 HCl → HAuCl4 + NO + 2 H2O
Atomic weight of gold is 196.96657 amu, thus 1 gram of gold = 0.005077 moles of gold.
Molarity of final solution is 0.005077 moles / (11 mL / 1000 mL per liter) =
0.4615 molar chloroauric acid.

June 28th, 2019

1. Dissolved 1 gram of .999 iridium by fusion with a mixture composed of 4 grams KOH and 4 grams KNO3 as was done for ruthenium on June 24th, 2019. The iridium powder rose to the surface of the melt in a ring around the surface of the crucible and then caught fire in a dazzlingly beautiful display of orange-ish fire. 

2. The solid melt was extracted with water to produce an yellow-orange-ish solution (clearly different from the deep red-orange as ruthenate). Much of the metal was found not to have reacted. This was put through a second fusion with KOH and KNO3 and that melt was dissolved with water once cooled and added to the first solution. 

3. 4 grams of barium acetate was dissolved in 100 mL of water. After this the iridate solution was decanted to remove as much of the solid particles as possible. 

4. The solutions were combined and a beige precipitate of what I presume to be barium iridate formed. I have not yet been able to find enough information on the compound to be 100% sure. 

5. The ruthenate produced on the 24th was dissolved in hot water and another solution of 4 grams barium acetate in 100 mL of water was prepared. 

6. The solutions were combined to produce a reddish precipitate of barium ruthenate. 

7. Both barium iridate and barium ruthenate were filtered (the waste was treated with magnesium sulfate to precipitate excess barium as harmless barium sulfate), placed on paper towels, and placed in separate desiccators with dry magnesium sulfate acting as the desiccant. 

Barium Ruthenate
Barium Iridate

June 29th, 2019

1. The dried barium ruthenate and barium iridate was collected and transferred to a labeled scintillation vials. The final yield was 3.05 grams of barium ruthenate. A second precipitation of barium iridate was carried out from the extraction of the second melt. However the yield of barium iridate thus far is 5.00 grams. It should be noted that neither of these is absolutely dry although they did break up into a powder. 

2. Dissolved 5.17 grams of indium in concentrated HNO3 which was added a few milliliters at a time until a final volume of approximately 10 mL. Stirring was carried out and the beaker was heated. Copious amounts of NO2 gas was given off in the reaction (in the future it would be a better use of these vapors if they were run through the gas bubbler to regenerate dilute HNO3). The result was a clear solution. 

In + HNO3 = In(NO3)3 + NO + H2

Atomic weight of indium is 114.818 amu, thus 5.17 grams of indium = 0.0450 moles of indium. 
Molarity of final solution is # moles / liters final solution thus 0.0450 moles / (11 mL / 1000 mL per liter) =
4.093 molar indium(III) nitrate

June 30th, 2019

1. Created a thorium nitrate solution from a 1 gram sample of commercial thorium nitrate. Although the label indicates this compound is a hydrate it does not specify which one it is. I used the pentanitrate in my calculations simply because it is the most common hydrate of thorium nitrate. The result was a clear solution. 

Molar mass of thorium tetranitrate pentahydrate is 570.146 
1 gram of Th(NO3)3•5H20 = 0.0017539 moles Th(NO3)3•5H20, thus 0.0017539 moles / (10 mL / 1000 mL per liter) =
0.17539 molar Th(NO3)3•5H20

Level of activity observed from the solution + background: approximately 65 CPM or 0.42 microsieverts per hour

2. Prepared a stock solution of uranyl acetate dihydrate by dissolving 1.5 grams of uranyl acetate dihydrate in 8.9 mL of water and 1.1 mL of glacial acetic acid. All of the solid did not dissolve and it was impossible to tell if this was a precipitate caused by sodium ions in the water or if the solution was just saturated. The solubility of uranyl acetate dihydrate is only 7-8 grams in 100 mL of water. The solution was stored in an amber glass bottle to protect it from UV radiation. 

Molar mass of UO2(CH3COO)2·2H2O is 424.146, thus 2 grams = 0.004715 moles which in 10 mL solution = 0.4715 molar UO2(CH3COO)2·2H2O. 
Level of activity observed from the solution + background: approximately 28 CPM or 0.18 microsieverts per hour. D.U. was used in making the uranyl acetate dihydrate.

3. Prepared some samarium triiodide hexahydrate by dissolving several grams of samarium in concentrated hydriodic acid. The amounts were not important as the goal was simply to generate some samarium triiodide hexahydrate crystals for future experiments. Once all of the metal was dissolved the solution was allowed to boil in the open until most of the color had left it and a light yellow liquid was all that was left. The solution was then filtered and then reduced in volume some more with moderate heating and gentle stirring. Once the volume was down to about 20 mL the beaker was removed from stirring, the stir bar was removed, the beaker was covered with Parafilm and placed in a cooler with ice for crystallization. 


Return to the Main Laboratory Notebook Page
Return to the Poor Mans Chemist Homepage