Friday, June 26, 2020
- The thallium(I) carbonate synthesis was a success but most of the thallium was somehow lost. I am not sure where it went but I think that most of it was mechanical losses. The thallium was converted to the chloride, filtered off, and dried. 260 mg of dried thallium(I) chloride was obtained.
- Molar mass of TlCl = 239.82 grams per mole
- 0.260 grams of TlCl = 0.00108415 moles
- Synthesis of cesium nonachloridodithallate(III) Cs3[Tl2Cl9].
- Molar mass of CsCl = 168.36 grams per mole
- Three molar equivalents is 0.5475 grams of CsCl
Thursday, June 16, 2020
- I decided to go with making the thallium(I) carbonate from the metal first. I combined the thallium nitrate and thallium sulfate solutions and neutralized the solution. The thallium metal was then precipitated out using sodium borohydride.
- The metal was allowed to settle out and then the solution was removed using a syringe.
- The metal was washed with distilled water several times to remove as much nitrate ion as possible.
- Working on the assumption that no thallium metal was lost there is 4.8 grams of thallium metal in the sample.
- Atomic weight of thallium = 204.383 grams per mole
- 4.8 grams of thallium = 0.0234853192290 moles of thallium
- Molar mass of sulfuric acid = 98.079 grams per mole
- 0.0234853192290 moles of sulfuric acid = 2.303416624670 grams of sulfuric acid
- 1.57 M sulfuric acid = 0.00157 moles per mL
- Number of mLs of 1.57 M sulfuric acid needed to completely react with 4.8 grams of thallium metal = 14.95880 mL
- I evaporated down the thallous nitrate some more yesterday and let it sit overnight to obtain some even better crystals than before.
Wednesday, June 15, 2020
- Completed the synthesis of a solution of thallium(I) nitrate from 2.10 grams of thallium metal in 4% nitric acid. After dissolving all of the metal yesterday and allowing the solution to cool overnight I discovered beautiful crystals in the solution this morning.
- Another 2.7 grams of thallium metal was begun dissolving in 1.57M sulfuric acid two days ago but after taking so long to dissolve I added in 50 mL of the 4% nitric acid which effected dissolution of the chunk of metal within minutes.
- Both solution were evaporated down some with stirring before being stored covered for the night at the ambient temperature.
- The solution of 2.7 grams will be converted into thallous bromide and the solution of the 2.1 grams will be converted into thallous chloride in order to conduct the experiments.
Monday, June 15, 2020
- Synthesis of thallium sulfate carried out by putting 2.70 grams of thallium metal into ~125 mL of heated 1.57M sulfuric acid with constant stirring.
- "Clerici's solution which has picked up impurities in use and thus become brown (due to malonic acid decomposition products) can be regenerated, according to Rankama, by dilution of the concentrated solution to four times its volume with distilled water, treating with 1 g. of powdered charcoal per 100 g. of concentrated solution, heating, stirring and filtering. The solution is then clear. Thallium is precipitated from it as TlCl and converted to thallium(I) sulfate with sulfuric acid. The latter is then converted to TlOH (see p. 877) by treatment with Ba(OH)2, which is in turn converted to thallium(I) carbonate (seep. 884) by saturation of the hot solution with CO2 and evaporation. After recrystallization, the thallium(I) carbonate is used as described above for the preparation of thallium formate and malonate." HoPIC page 886
Sunday, June 14, 2020
- Completed synthesis of 11.41 grams of uranyl sulfate trihydrate from uranium trioxide that I made from 5 grams of DU shavings and 1 grams of NU shavings.
Monday, June 8, 2020
- Synthesis of Barium Chlorate 17.51
- A mixture of 13 g. of potassium chlorate, 7.42 g. of ammonium sulfate and 37.12 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 16.96 g. of barium hydroxide octahydrate dissolved in 20 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.
- Final yield 11.35 grams of slightly damp crystals.
Saturday, June 6, 2020
- I produced uranium red using the alternate synthesis described in the atomistry article on uranyl sulfide. Potassium uranate was combined with excess uranyl nitrate and both dissolved in water with stirring. It takes 10-15 minutes for them to go into solution. Then enough potassium hydroxide solution was added to just make a small amount of solid diuranate precipitate. After this hydrogen sulfide gas generated by the reaction of sulfuric and and sodium sulfide was bubbled through the mixture until a vividly orange compound precipitates out of solution. Addition of more potassium hydroxide solution at this point produces a beautiful uranium red that has a true blood red color. In fact it is so blood red that it is virtually indistinguishable from blood while stirring. So long as the solid stays in the solution it was in the uranium red retains its color. On drying particles made of a black and red substance are formed.
- Video of true blood red uranium red preparation on YouTube
- Video of true blood red uranium red preparation on BitChute
Monday, June 1, 2020
- I filtered off the uranium red yesterday and decided to dry it just to see what would happen. I was not confident that the color would hold after drying. However, when I looked at it under the scope today after it had fully dried I saw to my complete astonishment particles composed of a mixture of a black substance and a red substance were breaking themselves into pieces! Furthermore when I looked with the naked eye down on the level of the watch glass I could see tiny particles of uranium red jumping up from the mass of crystals! I could not tell if the particles were breaking themselves apart with such force they were launching pieces into the air or if unbroken particles were jumping about (I suspect the former but I have no direct evidence for this). I recorded a clip the particles breaking themselves into pieces.
- Video of particles on YouTube
- Video of particles on BitChute
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