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February 22 2012 4 22 /02 /February /2012 15:43

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Aluminium and zinc alloying: The gray residue from the aluminium alloy was dissolved in hydrochloric acid to dissolve the aluminium oxide. Some fizzing was observed and the solution turned a dirty gray. Zinc was added and after some initial hydrogen production it stopped.  More hydrochloric acid was added and the zinc dissolved more slowly than is normal for hydrochloric acid of that concentration. It seems that some gallium was deposited on the zinc and is slowing down its reaction. The zinc, examined later, seems exceptionally brittle, and slightly differently colored. Did the gallium alloy with the zinc? Yes. The zinc alloy is exceptionally brittle. According to Wikipedia, gallium makes most metals brittle.

Manganese reactions: The magnesium dissolved almost complete, making some brown precipitate in the process. Because of the precipitate’s amount and its relative nonmagnetism, I believe that it is manganese metal contaminated with surface oxide and a little bit of iron. The zinc did not appear to reduce anything in the solution. The precipitate can be regarded as manganese metal.

Silver formation: A piece of cleaned copper metal is placed in the silver acetate solution. Some bubbling is observed, and the copper turns black immediately from silver deposition. The silver, though, is being dissolved as fast as it is being deposited. When the solution is agitated, black flecks of silver come off the copper and dissolve. It seems that the hydrogen peroxide did not decompose completely, and therefore no sizable quantity of silver will be precipitated until the hydrogen peroxide is exhausted. The copper gets a bluish-black look when a very thin film of silver is deposited. Copper(II) chloride is added because of its reputed peroxide catalyzing effect, but the silver chloride precipitated instead. The silver is quite dissolved by the process, as almost none remains.

Neodymium salt extraction: The neodymium magnet acetate is reacted with ammonia. A very light yellowish precipitate is formed, with most iron kept in the ferrous state by the zinc. Addition of air turns it greener. Dissolved oxygen was not present since the magnet dissolution replaced all of it by hydrogen. This precipitate is filtered and dried. I plan to follow the same process I followed with the mischmetal for iron removal. The magnet is of course covered with a thick layer of iron powder that does not dissolve as rapidly in the acetic acid as the neodymium and/or praseodymium.

 

 

Aluminium alloying: After the powder produced when galinstan alloys with aluminium is washed away, this is what remains. Keep galinstan off aluminium airplanes, please. This was about 50 mg of galinstan, and it wasn’t even done with attacking the aluminium.

Zinc gallium alloy: The side of the zinc alloy at a fracture point looks much more crystalline than a typical metal fracture. The second picture is just two of the broken pieces of alloy.

Galinstan cleanness: Galinstan is significantly oxidized on the surface by oxygen and water. This is all the more obvious because galinstan is a liquid and its oxides are solids. The difference between galinstan in dilute hydrochloric acid (for a few minutes) and in water (for a few hours) are obvious. The water-corroded bead is dull and spread out. It tends to stick more to surfaces. The clean bead is shiny, cohesive, and mobile.

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Neodymium salt production: The precipitate formed is dried in air. It becomes light yellow. This is then dissolved in hydrochloric acid. Zinc is added. Some decoloration of the iron(III) chloro complex is observed amid hydrogen production by zinc-acid reaction. The precipitate is visible below. This is much lighter than the dark-red mostly-iron precipitate formed when the magnet dissolves in hydrochloric acid. The solution turns colorless and is neutralized again with ammonia. Because of the use of an eyedropper containing a drop of FeCl3 solution, the resulting precipitate may have a significant contamination of iron. Once the precipitate is dried, it looks like the second picture. Not too much difference there.

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Neodymium salt dissolution: A final try is conducted. The precipitate is redissolved in HCl to give the telltale sign of iron, although only about 0.5% is present, based on the color. Zinc is added to the fairly concentrated solution to re-re-reduce the iron. The solution is still colored in the same way. There appears to be quite impure Nd in the magnet, so production from magnets does not appear to be a viable way.

Toothpaste reactions: Toothpaste is placed in water. Most of the chemicals in my toothpaste are soluble or miscible in water (sorbitol, water, silica, glycerin, sodium fluoride, sodium phosphate, sodium pyrophosphate, sodium hydroxide, etc.) I am thinking of filtering the solution and precipitating the fluoride with calcium chloride or magnesium sulfate solution. While sodium fluoride’s solubility is 40 g/L, magnesium fluoride’s solubility is 0.8 g/L, and calcium fluoride’s solubility is 0.1 g/L, making precipitation effective once the solution is concentrated. However, other phosphates may coprecipitate. However, the toothpaste forms a foamy colloid that is impossible to filter, so my toothpaste is not a good source of the fluoride ion.

Copper bromide production: Cleaned copper is placed in hydrogen peroxide to which sodium bromide is added. I hope copper(II) oxybromide will be produced. However, no coloration is observed.

Silver dissolution: Silver is again added to a mixture of hydrogen peroxide and acetic acid. However, this silver was not previously activated by electrolytic oxidation. No dissolution is occurring. The silver was removed and then electrolytically oxidized in sodium chloride solution. It was placed again in peroxide. This time the catalytic separation was swift. Acetic acid was then added. The decomposition slows considerably and the cloudiness appears.

Gallium extraction: The brittle zinc-gallium alloy is dissolved in hydrochloric acid. No gallium is left.

Bromide mess: Lead is electrolytically oxidized in sodium bromide solution. Pale white lead(II) bromide is produced by reaction of the bromine water with the lead. The reaction is not instant and smell of bromine is produced. Iron is electrolytically oxidized as well. Black carbon falls off as the iron dissolves to form most likely iron(II) bromide. Eventually, the solution gets basic enough that iron(II) hydroxide begins precipitating. With more oxidation, iron(III) bromide is produced, which hydrolyzes to iron(III) oxybromide, darker than iron(II) hydroxide. When copper is electrolytically oxidized, first white copper(I) bromide is produced.  Later, more bromine oxidizes it to copper(II) bromide, which is soluble. The first picture is the iron oxybromide, second is the copper(I) bromide, and the third is the lead(II) bromide.

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Silver dissolution: After the silver dissolves in acetic acid/hydrogen peroxide mixture, there is always a residue. My silver is supposed to be 99.9% pure, so why is there a residue? It also seems that silver has a protective coating impermeable to the mixture. Nascent chlorine removes this layer, allowing silver to dissolve or react.

Silver halide production: Silver acetate solution was reacted with sodium chloride, sodium bromide, and sodium iodide. All three precipitated their insoluble silver halide. The silver chloride is pure white; silver bromide is slightly off white; while silver iodide is definitely yellowish. The sodium iodide was made by reduction of tincture of iodine with ascorbic acid. Excess ascorbic acid later reduced the silver iodide to silver metal. The silver chloride also appears to be turning a little gray. Silver bromide, precipitated separately and filtered, shows the yellowish color better.

 

 

Silver reactions: Silver acetate solution is reacted with solid calcium hydroxide. A grayish precipitate is formed, probably a mixture of calcium hydroxide with a little silver oxide. The precipitate is placed in excess water to allow much of the calcium hydroxide to dissolve. The precipitate that falls out is pipetted out and placed on a tissue.

Silver halide light exposure: The silver halides change upon exposure to light. The silver chloride seems most affected, while the silver iodide (flakes alongside the black puddle) seems least affected.

Silver reduction: Silver acetate solution is reacted with ascorbic acid, which instantly reduces it to gray silver powder.

Silver carbonate: When the silver acetate solution is reacted with sodium carbonate, it forms white silver carbonate which quickly turns gray as some of it converts to silver(I) oxide. The precipitate appears very fine and is not caught by a tissue, unlike silver(I) oxide. Mellor states that excess sodium carbonate will convert some of it into silver(I) oxide, so that appears to be what happened.

Gold dissolution/Iodine production: Gold is placed in a hydrogen peroxide/hydrochloric acid mixture. No dissolution occurs. Tincture of iodine is added. The triiodide is oxidized to elemental iodine, which dissolves in the alcohol present to form a brown solution. Supposedly iodine can dissolve gold. Some iodine has precipitated(!), while change regarding the gold is imperceptible. Regarding the iodine; it seems that the alcohol is either oxidized by the peroxide or insufficient to dissolve all of the iodine. After such a waste of iodine tincture by electrolysis, I have found a much simpler way to produce iodine for the element collection.

Sodium hydroxide production: Sodium carbonate is shaken with calcium hydroxide in aqueous solution in an attempt to form sodium hydroxide. The pH is only about 11, which means I only made a dilute sodium carbonate solution after wasting almost all of my calcium hydroxide. No reaction occurred.

More oxygen

 

 

Less oxygen

AgI                                                                         AgBr                                      AgCl

             NaI                                            NaBr                                      NaCl

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Published by LanthanumK - in Experiments
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