Thursday, May 28, 2020
Tuesday, May 26, 2020
- Notes on "Uranium Red"
- Atomistry Article on Uranyl Sulfide
- Google Books The Chemical News and Journal of Industrial Science, Volume 10
- "Hydrosulphate of Sulphide of Sodium" and how to prepare it.
Tuesday, May 19, 2020
- Begin experiment to produce cesium uranyl chloride
- A solution of 1.02 grams of uranyl sulfate is reacted with a solution of barium chloride to produce uranyl chloride.
- Molar mass of uranyl sulfate = 366.09 grams per mole
- 1.02 grams of uranyl sulfate = 0.00278620 moles
- Two molar equivalents of barium chloride are 0.00557240 moles
- Molar mass of barium chloride dihydrate = 244.26 grams per mole
- Required amount of barium chloride dihydrate = 1.361114480 grams
- The uranyl chloride solution is combined with two molar equivalents of cesium chloride
- Molar mass of cesium chloride = 168.36 grams per mole
- Required amount of cesium chloride is 0.93816930 grams
- The solution is then evaporated down to obtain crystalline cesium uranyl chloride
- Continue synthesis of hydrazine hydrochloride
- All of the solution made yesterday was centrifuged to remove all traces of barium sulfate.
- The centrifuged solution was transferred to a bottle for storage until the water can be evaporated off.
Monday, May 18, 2020
- Begin experiment to produce solid hydrazine hydrochloride (note Pt experiment on pg 1573 of THoPIC)
- 10 grams of hydrazine sulfate is dissolved in a minimal amount of room temperature water.
- Molar mass = 130.12 grams per mole
- 10 grams of hydrazine sulfate = 0.076852 moles
- Add 18.77 grams of barium chloride dissolved in a minimal amount of room temperature water.
- 244.26 grams per mole for the dihydrate
Monday, May 11, 2020
- Begin experiment to produce sodium uranate and potassium uranate. http://uranium.atomistry.com/uranium_trioxide.html
- Sodium uranate will be produced by the reaction of sodium hydroxide with hydrated uranium trioxide. In contact with water uranium trioxide readily forms uranic acid H2UO4 and so a small amount of water is added to the UO3. After combining the trioxide with water a solution of sodium hydroxide is added to the slurry.
- 0.5 grams of uranium trioxide was used. This was wetted down with a small amount of water with stirring before the NaOH was added.
- About 30 mL of ~50% NaOH was added to the beaker with stirring and the mixture was allowed to heat and stir for a couple of hours total for the reaction to go to completion (indicated by all of the solid UO3 hydrate on the bottom of the beaker turning into an orange-yellow solid.
- Filtered, rinsed, and dried overnight. After photographing this material was recycled.
- Potassium uranate will be produced by the reaction of heated potassium chlorate with uranium trioxide. http://uranium.atomistry.com/potassium_uranate.html
- 0.9 grams of uranium trioxide.
- This reaction works well. However, it is recommended that the potassium chlorate and uranium trioxide be carefully ground into an intimate mixture and that stoichiometric amounts of potassium chlorate are used.
- Then heat in a closed crucible until all generation of gas ceases.
- The solid is then cooled and mixed with water in which it disintegrates rapidly.
- Filtered, rinsed, and dried overnight. After photographing this material was recycled.
- Begin experiment to produce uranyl sulfate
- Uranyl sulfate trihydrate will be produced by the reaction of dilute sulfuric acid with uranyl hydroxide UO2(OH)2 http://uranium.atomistry.com/uranyl_sulphate.html
- 0.8 grams of uranium trioxide placed in a 100 mL evaporating dish
- Molar mass of uranium trioxide = 286.29 g/mol
- 0.0027943693 moles of uranium trioxide
- 16 mL of 1.75% sulfuric acid was added
- 1.75% sulfuric acid, density = 1.0192 grams/mL
- Every mL contains 0.017836 grams or 0.000181853 moles of sulfuric acid
- Molar mass of sulfuric acid = 98.079 g/mole
- The uranium trioxide dissolved readily in the dilute sulfuric acid when heated in an evaporating dish on the boiling water bath.
- Evaporated down. Multiple cycles of addition of water, evaporating down until solid is observed, redissolving in water, and then evaporating back down again eventually yielded a crystalline product.
- This product was dissolved in water and transferred to a scintillation vial.
- 0.0027943693 moles of uranyl sulfate is 1.022990 grams of uranyl sulfate
- Molar mass of uranyl sulfate is 366.09 g/mole
All of these experiments can be seen on YouTube at: https://www.youtube.com/watch?v=lJBC8eN1U1E
Thursday, May 7, 2020
- Continue evaporating down the liquid left over from the synthesis of the ammonium peruranate. I have been working on it for three days now and it's about halfway through it's slightly more than 1 liter starting volume of liquid (water, ammonia, dilute H2O2, ~400 mLs of mostly absolute IPA and some absolute ethanol). It is depositing a yellow powder as it reduces down.
- I suspect the yellow solid may be ammonium peruranate. As the last of it is reduced down the final remaining liquid will be water. If the solid dissolves then that speaks towards it being ammonium peruranate which is soluble in water.
- An experiment was conducted to attempt to synthesize strontium uranate.
- The urano-uranic oxide produced yesterday was ground with an excess of strontium chloride using a mortar and pestle until it was a fine powder. This was transferred into the crucible and heated using the Meker burner on full heat. Heating began at 14:44.
- Melting point of strontium chloride = 874oC
- Strontium uranate produced in this way is a yellow crystalline insoluble in water but readily soluble in dilute hydrochloric acid.
- The material was heated for about 45 minutes until 15:30. the result was a light brown powder with slightly yellow flecks in it. However, as the mixture cooled down the material was universally a light brown color.
- The yellow flecks turned white and readily dissolved in water leading me to believe they were excess strontium chloride.
- The brown material did not dissolve in water nor did it fully dissolve in RFNA. The nitric acid solution turned yellow indicating the presence of uranyl ion but not all of the solid reacted.
- If the synthesis was successful the product was definitely contaminated with something.
Wednesday, May 6, 2020
- The ammonium peruranate that was dried in the desiccator overnight was collected off the filter paper and transferred to a vial. Only about 400 mg of a reddish-brown powder were recovered. This was labeled and put in the inventory. The filter paper was put in uranium recycling.
- An experiment was conducted to try to produce uranium trioxide and urano-uranic oxide (triuranium octoxide) from ammonium diuranate
- 2 grams of ammonium diuranate was placed in an 100 mL evaporating dish. This dish was put into the oven at ~232oC (450oF).
- Begin heating at 14:17
- After 30 minutes the material had turned a pinkish-orange color.
- After 60 minutes the material had not changed much in appearance.
- Conclusions: The cool material was broken open at which point it was observed that the color change was present throughout the entire body of the material. It should probably be ground and subjected to another round of calcination for 30-60 minutes making sure to stir it occasionally.
- 2.5 grams of ammonium diuranate was placed in an 100 mL crucible. This was covered and heated over the Meker burner with a full flame.
- Begin heating at 14:23
- The material turned black at first but after about 30 minutes the material began turning green.
- After an hour the material had a distinct green color.
- Conclusions: The material needs to be heated like this for ~30 minutes on full heat at which point the heat should be turned off. The material, once cool, should be ground into a powder and subjected to another 30-60 minute round of calcination. Once all of the orange color is gone and the material is totally green the heating should be discontinued and the material allowed to cool.
- Washing the final material with distilled water should remove all lingering traces of ammonium diuranate.
Tuesday, May 5, 2020
- The ammonium diuranate I produced yesterday was "dissolved" in 3% hydrogen peroxide. While all of the ammonium diuranate readily disappeared from the filter paper the solution was at no point clear.
- I added more 3% H2O2 until the mixture was semi-transparent.
- I then added a few hundred milliliters of anhydrous isopropanol to precipitate out the ammonium peruranate. This was filtered off and dried in the desiccator overnight.
Monday, May 4, 2020
- Recrystallized 25 grams of ammonium sulfate
- Filtered recycled uranyl nitrate
- Added concentrated ammonium hydroxide to precipitate ammonium diuranate with about half of the solution of recovered uranyl nitrate
- Addition of less concentrated ammonia when precipitating out ammonium diuranate seems to result in a precipitate that is more difficult to filter.
- A pH of perhaps 10 is best?
- It is very difficult to get all of the uranyl nitrate to precipitate. There always seems to be a slight yellow tinge to the filtered solution every time no matter how high the pH is.
- In the end I only precipitated half of the uranyl nitrate as ammonium diuranate. This was filtered off and dried as before.
Sunday, May 3, 2020
- Bottled dried ammonium diuranate I made the previous day and dried out overnight over 3A molecular sieves.
- Recycled uranium waste into a single solution of uranyl nitrate
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Barium Chlorate Synthesis (Reduced by a factor of 20/70 or ~0.2857142857)
- A mixture of 35.02 g. of potassium chlorate, 20 g. of ammonium sulfate and 100 ml. of hot water is evaporated in a porcelain dish with constant stirring until a thin slurry forms.
- After cooling, a fourfold quantity of ethyl alcohol is added, resulting in the separation of insoluble potassium sulfate from the ammonium chlorate.
- The potassium sulfate residue is filtered and washed several times with alcohol.
- The filtrate is freed of alcohol by distillation.
- The ammonium chlorate residue (Caution: ammonium chlorate has a tendency to explode!) is reacted in a porcelain dish on a steam bath with a sufficient quantity of hot concentrated barium hydroxide octahydrate solution (at least 45.7 g. of barium hydroxide octahydrate dissolved in about 46 ml. of hot water) so that the ammonia odor disappears completely and the solution finally gives a definite alkaline reaction.
- It is then evaporated to dryness.
- The residue is dissolved in a fivefold quantity of water, and carbon dioxide is bubbled through the solution until the precipitation of barium carbonate is completed.
- The barium carbonate is filtered off and the solution evaporated to crystallization.