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February 20 2012 2 20 /02 /February /2012 15:23

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Antimony trioxide production: The removal of most of the lead solution, acidification with hydrochloric acid, and oxidation with hydrogen peroxide formed a significant amount of antimony trioxide to fall out. The precipitate is filtered, dried, and photographed.

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Tungsten and molybdenum extraction: A halogen light bulb from a printer is broken and the molybdenum and tungsten extracted.

Tungsten and molybdenum reaction: Tungsten and molybdenum are individually placed in a moderately concentrated copper chloride solution. Mellor states that they both incompletely reduce a solution of copper(II). After a few hours no reduction is observed to occur. After 24 hours no reduction is observed to occur.

Lead zirconate titanate: My piece of PZT from a piezo element was placed in acetic acid to hopefully dissolve the lead and leave white zirconium and titanium dioxides behind. It appears to be turning a little whiter but that could be just wishful thinking, which it is after 24 hours.

Stainless steel corrosion: Copper chloride crystals rubbed on an 18/0 stainless steel spoon cause the formation of a brown mixture of copper and iron oxide. Stainless steel is not so stainless after all. 18/0 (18% chromium 0% nickel) seems to be lower quality than 18/10 (18% chromium 10% nickel).

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Antimony production: Antimony trichloride solution was reduced by zinc and the antimony collected in the past. Now, because the antimony was wet, it has some trioxide around it as a result of aerial oxidation.

Tetramminecopper(II) formation: Addition of a small amount of ammonia to a copper(II) chloride solution resulted in a copper(II) hydroxide precipitate. Addition of more results in a deep blue tetramminecopper(II) solution. Addition of hydrochloric acid reverses the process, with a little copper(II) hydroxide formed as an intermediate in the reaction.

Silver oxidation: A piece of silver wire is used as the anode in a 24V electrolysis apparatus with salt water electrolyte. The silver wire appeared to have turned whitish, showing the formation of a small amount of silver chloride. A passivation coating appears to have formed though, preventing the electrolysis from continuing. The picture below shows the wire. The bottom is the part that was anodized. On second glance, however, it appears that silver chloride was produced. Hydrochloric acid was added to the solution to dissolve the tiny amount of iron(III) hydroxide produced when the alligator clip was accidentally momentarily placed in the solution.  The remaining precipitate is decanted, washed, and filtered. It is a slightly creamy white.

 

Silver bromide formation: The silver chloride coated silver wire turned a little more yellow when dipped into sodium bromide solution. It is electrolyzed in this solution to see whether AgBr can be produced in the same manner. A small smell of bromine is observed. Other than the wire turning yellow, no silver bromide seems to have been produced. I’m not sure why silver chloride was produced last time. The left end has darkened due to exposure to light; silver bromide is more sensitive than silver chloride.

Galinstan oxidation: The partially oxidized remnants of the galinstan thermometer mixed with glass are placed in dilute hydrochloric acid. No dissolution appears to be occurring. The only explanation is that everything is oxide-coated or even completely oxidized.

Copper electrolysis: A bromine smell is produced when copper is electrolytically oxidized in sodium bromide solution. An infinitesimal green precipitate was formed. The current flow was quite high. Later on, a white precipitate of copper(I) bromide formed, which was oxidized by air to a greenish copper(II) oxybromide. Addition of hydrogen peroxide oxidized everything to copper(II) bromide, which had a brownish-green solution. Here is the copper(I) bromide, beginning to oxidize in the air.

Silver chloride production: Silver chloride is a very pale off-white color. It did not darken perceptibly after a few minutes in sunlight. It seems to be a heavy precipitate, which makes it likely AgCl. A significant amount was produced. It dissolves in aqueous ammonia to form a colorless solution.

 

Silver chloride reduction: Silver chloride was placed in aqueous ammonia to dissolve and zinc was added. However, the silver chloride does not seem to dissolve, even though it is supposedly very soluble in aqueous ammonia. Addition of HCl caused, among vigorous fizzing from the zinc, a spongy gray precipitate to form. This may be silver. [redacted] Some of the silver chloride dissolved.

Copper complexes: Copper(II) chloride is dissolved in hydrochloric acid to form the yellow-green tetrachlorocopper(II) complex. Sodium bromide is added. The crystals turn dark brown immediately, then dissolve to form a dark brown bromo copper complex which lightens to green when diluted.

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Silver chloride reduction: This is the extent of the “silver” that finally deposited on the bottom after being ceaselessly thrown about by the zinc’s hydrogen emission.

Sodium bromide electrolysis: Sodium bromide is dissolved in water and the solution electrolyzed at 24V with a carbon anode and iron cathode. Pictures below are of the progress of the electrolysis. The fourth picture is much lighter since the colorless NaOH-containing side was mixed with the orange bromine-containing side, and a chemical reaction occurred, which formed hypobromite and bromide. If the solution gets warmed enough, the hypobromite will disproportionate into bromate and bromide.

Galinstan oxidation: Galinstan seems very resistant to attack by hydrochloric acid. A little was dissolved after about 40 hours as evidenced by a small amount of precipitate which formed when the solution was neutralized with ammonia. A blob of galinstan seems to have obtained a clear surface from the acid bath. Instead of dissolving the galinstan and leaving the junk behind, it dissolved the junk and left the galinstan behind! What dissolved was probably the gallium oxide coating on the glass to prevent the galinstan from sticking.

Galinstan freezing: Galinstan is placed in the coldest part of a food freezer. The surface appears to have formed some crystals, while the bulk remains liquid. It appears that galinstan can freeze, although it probably exhibited supercooling to some extent.

Galinstan oxidation: The galinstan bead is placed in hydrochloric acid. It slowly dissolves. Two impurities latched onto the bead dissolve faster than the bead itself. Once it was placed in hydrochloric acid, it lost all of its droopiness and behaves more like a mercury bead.

Galinstan oxidation continued: Most of my small amount of lithium is reacted with water to create a basic solution. The galinstan bead is placed in the solution. It dissolves extremely slowly. Occasionally a bubble grows on the bead and then leaves. However, if this keeps up, a solution of lithium gallate will be obtained. The residue will become solid once all of the gallium has left, which I do not think will happen.

Sodium bromide electrolysis: The end result is a concentrated solution of bromine bleach, which contains sodium hypobromite. I would estimate about 15% concentration based on the color. This is made in the identical way a solution of chlorine bleach would be made, but using sodium bromide instead of sodium chloride as the starting point.

Bromine bleach treatment: Because oxygen gas was beginning to form and the bromine bleach beginning its path back to ordinary sodium bromide, I heated some water and dropped the bleach-filled container into the hot water bath. Quite a bit of oxygen was given off, and the solution appears to have become lighter. The amount of oxygen given off is negligible, however, when the amount of oxygen remaining in the solution is considered. Net reaction for synthesis: NaBr + H2O -> H2 + NaBrO decomposition: 2 NaBrO -> 2 NaBr + O2 (undesired reaction) disproportionation: 3 NaBrO -> 2 NaBr + NaBrO3 (desired reaction)

Neodymium magnet dissolution: Neodymium magnet, along with zinc metal, is placed in 5% acetic acid solution. It turns brownish after a while, indicating iron(III). The zinc is covered with precipitated iron, oxidizing to brown iron oxide.

LED dissolution: The phosphor from a burnt-out LED is placed in hydrochloric acid/hydrogen peroxide. No reaction is observed to occur.

Manganese reactions: The MnOOH from a CR2016 coin cell is placed in hydrochloric acid. The reaction starts very slowly. The solution, as always, is colored black. Later it clears up to a bright yellow, indicating some dissolved iron. When diluted, it becomes almost colorless. The acidic character seems to have almost disappeared. Zinc has almost no visible reaction with the diluted solution, while magnesium putters away, producing hydrogen and some iron, as evidenced by a magnet.

Silver dissolution: Silver is placed in a 2:1 mix of hydrogen peroxide/acetic acid. Catalytic decomposition of the peroxide is observed. Supposedly some silver will dissolve. The solution turned cloudy as if there was some chloride ion present, which is probably true. The cloudiness is coming off the silver, a good sign that dissolution is occurring. Catalytic decomposition seems to have slowed to a minimum.

Galinstan dissolution: It appears to have stopped (LiOH dissolution). At least the galinstan bead is reusable; if it does not dissolve in one reagent, it can dissolve in another. Zinc was added to the “lithium gallate” solution. Some galinstan was also placed on aluminium; maybe only the gallium alloys while the indium and tin remain behind as a solid. The noise produced by the gallium amalgamating and oxidizing the aluminium is captured by camera. Galinstan loses its ball formation in water. Addition of water to the aluminium amalgam caused fizzing. The aluminium needs scratching or tearing to be able to amalgamate quickly; otherwise, the process is very slow or nonexistent. A hole formed through the foil. Here are some pictures of the progressive amalgamation without water. This is what produced the crackling sound.

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Published by LanthanumK - in Experiments
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