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

1-6 Use Control + F to find what you want in here

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.

1-7

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.

1-9

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.

1-10

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

1-2 Use Control + F to find what you want in here

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.

1-3

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).

1-4

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.

1-5

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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February 17 2012 6 17 /02 /February /2012 20:17

12-24 - Use Control + F to find what you want in here

Lead iodide reactions: Sodium hypochlorite oxidizes the surface of lead iodide crystals, but not the bulk, making them turn brown. They get darker over time, indicating more oxidation. PbI2 + 2 NaClO -> PbO2 + I2 + 2 NaCl

Rare earth extractions: The brown precipitate has fallen out of solution. It does not have the reddish tinge of iron(III) oxide, but it could just be a different form. However, iron(III) would have been reduced by the zinc, so it must be a lower-valence rare earth compound. The remaining solution is colorless. The brown precipitate redissolved for an unknown reason, turning the solution a pink-brown color. The solution gradually becomes colorless. The rare earth must have been oxidized.

Lead iodide reactions: The blackish precipitate is washed with water. The water is then removed and the precipitate acidified with hydrochloric acid. Chlorine gas is produced as the lead(IV) oxide oxidizes the hydrochloric acid, which then reacts with the iodine present to form a yellow solution of iodine monochloride in hydrochloric acid.

Lead chloride oxidation: When lead(II) chloride is treated with sodium hypochlorite, it turns brown. This appears to be the formation of a minute quantity of lead(IV) oxide.

12-25

Copper chloride crystallization: The evaporation is going well.

Mischmetal solution: It has turned light pink-orange.

Boron extraction: Some iron(III) oxide appeared to appeared from nowhere.

12-26

 [redacted]

Boron extraction: The boron/water mixture filters very slowly through ordinary paper, but hopefully the boron will stay on the surface of the paper. A boron spotted paper is better than no boron. Actually, a rather large amount of boron was collected by the paper and is slowly drying.

Mischmetal hydroxide: The mischmetal acetate solution was reacted with ammonia. A very light green precipitate was formed which gradually turned orange, then dark brown, at least in part of it.

Magnesium-copper chloride reaction: Magnesium turnings react fairly rapidly with copper(II) chloride, forming a mixed oxidation state complex. Aluminium tends to react more vigorously.

Iron separation from mischmetal: Hydrated iron(III) oxide dissolves in acetic acid to form basic iron(III) acetate, which appears soluble in dilute acetic acid. In the mischmetal dissolution, the iron appears to oxidize by air to iron(III) oxide, which dissolves in the acetic acid.

12-27

Cerium dioxide separation: Sodium carbonate was added to the mischmetal hydroxides because cerium dioxide was supposedly soluble in sodium carbonate. Hydrogen peroxide was added some time later. Acidification with hydrochloric acid destroyed the carbonate, while ammonia dropped no precipitate. Acidification of the remaining hydroxide with hydrochloric acid produced no sizable quantity of chlorine gas, showing that the cerium had not really oxidized to cerium dioxide. Next, the hydrochloric acid solution was diluted and magnesium shavings introduced into the solution. They dissolved rather quickly without reducing any of the iron. A piece of zinc is then added. No immediate reaction is observed other than slow hydrogen production. After a while, however, the iron is precipitated and the solution clears. The hydroxide precipitate as formed by ammonia has a light green color (praseodymium) as well as a slight color change in different light (neodymium). The separation of the rare earths from iron has succeeded! JThe hydroxide will probably turn more yellowish as the cerium(III) oxide oxidizes to cerium dioxide. Since lanthanum(III) oxide is more basic than cerium dioxide, it can be dissolved in ammonium chloride solution to furnish lanthanum chloride and ammonia gas (La(OH)3 + 3 NH4Cl -> 3NH3 + 3 H2O + LaCl3) while cerium as a more acidic member does not act in that manner. Even trivalent praseodymium, neodymium, samarium, etc. should not dissolve in ammonium salts in this way.

 

 

Wheel weight dissolution: Pieces of lead previously placed in concentrated hydrochloric acid have developed a rather impermeable coating of lead chloride. After a while, dissolution by acetic acid/hydrogen peroxide can continue, however.

12-28

Rare earth extraction: The mischmetal hydroxide has dried and shows no evidence of iron contamination to the naked eye. The oxidation of the cerium(III) has proceeded, turning it less greenish and more yellowish. This process should work well with isolating neodymium salts from neodymium magnet acetate. However, due to the historical similarity of the rare earths from each other, the ammonium chloride method was unsuccessful in isolating any lanthanum from the hydroxide mixture. The hydroxide mixture is then dissolved in acetic acid. The evidence of some formation of carbonate overnight is seen by the slight bubbling of the hydroxide as it slowly dissolves in the vinegar. The solution was then neutralized by ammonia until a sizable amount of hydroxide precipitated. This was filtered. The resulting solution was completely precipitated with ammonia. The color difference is obvious. One is a cerium-rich section, while the other is lanthanum-rich. They are not pure enough to be entered in the element collection, though, so they were discarded after production.

 

Chemicals from household substances: I began to rewrite this document.

Why I do home chemistry: I wrote a paper on why I perform chemistry at home and why it may be good for you too.

12-29

Lead carbonate production: The lead dissolution in hydrogen peroxide/acetic acid went as planned. The lead solution was pipetted off and neutralized with sodium bicarbonate to form lead carbonate. The precipitate was very heavy. After a washing with water, it was filtered on a tissue from which only a little escaped.

 

Yttrium production: The supposedly yttrium-nickel alloy ground electrode of a spark plug was placed in vinegar to dissolve the yttrium. No immediate reaction is observed, possibly because of a protective coating formed by the nickel, making it impervious to acetic acid. After over an hour, no bubbles are observed to have formed. Yttrium-nickel alloy is impervious to acetic acid.

Antimony production: The black residue from the lead dissolution was dissolved in hydrochloric acid and hydrogen peroxide added. A white precipitate dotted with black dirt (random insoluble junk) was formed. The white precipitate was washed with water to remove the [redacted] and filtered. Hydrochloric acid was then added to the precipitate in the filter paper. It redissolved and fell through the paper into another container, where it hydrolyzed a little as it hit some water. Zinc was added and a moderately vigorous reaction with the acidic solution ensued. Black flecks of antimony were precipitated simultaneously, insoluble in the acidic solution. The antimony was washed with water, dried, and photographed.

Vanadium production: A chrome-vanadium steel screwdriver bit is immersed in hydrochloric acid. The solution turns yellow and small amounts of hydrogen are produced, typical of iron dissolution. After a while, the solution turns nearly colorless and small amounts of insoluble black precipitate are formed. It is difficult to tell whether the precipitate is magnetic as the screwdriver bit is strongly magnetic, but the precipitate does not appear to be magnetic.

Lead production: The previously formed lead carbonate is redissolved in excess acetic acid and zinc is added. A black spongy precipitate, amid the fizzing, begins to form on the zinc. This precipitate is pure spongy lead metal. Some lead carbonate is visible on the bottom of the container in this picture. Once the lead sponge is compressed it becomes much smaller with release of water, just like a real sponge.

 

Nickel reactions: A nickel spark plug ground electrode is placed in a mixture of 30% hydrochloric acid and 3% hydrogen peroxide in the ratio 1:3. Dissolution begins slowly, with a green layer of nickel(II) chloride floating out of the electrode, and continues steadily.

12-30

Vanadium production: More precipitate has formed overnight. It should consist of just carbon and vanadium flecks; no tungsten or molybdenum should be present.

Copper chloride crystallization: The copper chloride appears to be just about crystallized. When a stainless steel knife is inserted into it, it begins corroding immediately, reducing the copper to the very dark mixed oxidation state complex, which gets reoxidized by atmospheric oxygen in the acidic condition.

Nickel reactions: The nickel solution is darkening but very slowly.

Lead dissolution: Here is a picture of the elements insoluble in acetic acid/hydrogen peroxide. These are all of the elements other than lead in the wheel weight pieces.

Copper comproportionation: Copper is placed in an acidic solution of copper(II) chloride. Immediately, the solution begins turning dark at the bottom. After a while, the solution ceases becoming darker. When water is added, it lightens up again instead of precipitating the copper(I) chloride crystals.

Vanadium production: The residue, which mostly appears very light (amorphous carbon), was washed with water. It is nonmagnetic, showing that no iron has been left behind. Since vanadium is 3 times denser than carbon, a drying and then dropping into water should make the vanadium fall to the bottom while the carbon is stuck on the top by surface tension. However, there is not enough vanadium to do this.

Lead sulfate production: The lead solution from the lead dissolution was reacted with magnesium sulfate to produce insoluble heavy powder of lead sulfate. The precipitate was washed with water, filtered, and dried. Like most but not all lead compounds, it is white.

Wheel weight dissolution: The black residue was washed with water and acidified with hydrochloric acid. Not much happened, although undoubtedly the tin was dissolving. Addition of hydrogen peroxide rapidly cleared the black suspension, causing fine crystals [redacted]  to fall down and collect in the bottom. [redacted] Adding water to this mixture did not hydrolyze any antimony. All of the other times the antimony was readily hydrolyzed, but here, a significant amount of sodium bicarbonate was needed to just make a cloudy solution. This has more of the behavior of tin than antimony. I’m not sure why this is. Repetition with new lead is deserved. It is strange that the cutting open of the lead pieces reveals no shine of metal inside, only a dull gray interior.

Nickel reactions: The ammonia turned the nickel solution bluish, but precipitated hardly any hydroxide. When sodium bicarbonate was added, however, a large amount of nickel carbonate precipitated. This was filtered and washed with water. Addition of a large excess of ammonia formed a blue ammine complex.

[redacted]

12-31

Nickel carbonate: It is taking a while to dry, showing that some deliquescence even after washing is present.

[redacted]

Nickel complex and oxidation: Nickel forms a yellow-green chloro complex with excess hydrochloric acid. Nickel carbonate dissolves slowly in acetic acid to form a green solution of nickel acetate. From the amount of bubbling it appears that more hydroxide than carbonate formed. Addition of sodium hypochlorite does not oxidize the nickel(II) to nickel(III), probably because the solution is too acidic.

Antimony trioxide extraction: Lead from a new wheel weight is dissolved in acetic acid/hydrogen peroxide. Some oxidation of the non-lead elements is accomplished by the hydrogen peroxide alone, as evidenced by a whitish film of oxidation products floating above the elemental powders.

Sodium bromide oxidation: Manganese dioxide powder, about 10% pure and contaminated with carbon, ammonium and zinc chlorides, and lower manganese oxides, was added to a solution of sodium bromide acidified with acetic acid. No immediate reaction occurred. Returning after a few hours, the solution is light yellow and smells of halogens.

Hydroxide                Chloride

La          Ce

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February 14 2012 3 14 /02 /February /2012 16:00

12-17 - Use Control + F to find what you want in here

Magnet dissolution: The solution has turned the same color as the mischmetal solutions have. The color does not noticeably change when exposed to fluorescent light versus sunlight. Is this the result of iron?

Cadmium production: The filtered solution is green(?). Upon zinc reduction, a few magnetic particles appear to form, but they could just be junk on the zinc. Later, some very weakly magnetic particles form (cadmium), which dissolve slowly in the green solution. Some nickel was produced as well.  Further on, more cadmium appears to have precipitated; the zinc has become coated with a black nonmagnetic substance.

 

 

Nickel dissolution: Upon placement of the NiOOH cathode in HCl, a little fizzing was produced, along with a very lightly colored solution. It appears that no nickel was dissolved. The “cadmium” produced more green than the “nickel”.

12-18

Magnet dissolution: Overnight, some insoluble matter has formed in the magnet – acetic acid mixture. A large amount of iron filings are attracted to the magnet, probably as the result of preferential neodymium oxidation. The solution appears to have dissolved quite some iron.

12-19

Mischmetal reactions: The mischmetal solution turned very light yellow when ascorbic acid was added, showing that a highly colored complex of iron(III) was present. Upon addition of sodium bicarbonate, an extremely dark purple iron(II) ascorbate complex (seen with another iron exploration) was formed. It appears red upon transmitted light. It oxidizes to brown in air.

 

 

 

Threshold frequency experiment: A glow-(green)-in-the-dark object was placed in the dark until its glow diminished to a steady level. It was then exposed to equal quantities of red and white light. The red did not have any noticeable effect since just about all of its emitted photons were below green, which is the threshold frequency. The white did have a noticeable effect. From left to right: Beginning, Red, and White.

12-20

Magnet dissolution: Inclusion of air meant that the residual iron was oxidized rapidly. A small amount of the bright red iron(III) acetate complex was formed, but mostly iron(III) hydroxide was formed. If air is excluded, this might be a good way to extract neodymium from their magnets, but as long as air is present, the rusting process gets its way.

Tissue chlorate: The bleach-soaked tissue had dried onto the container and was peeled off in shreds and squeezed together. It seems quite heavy, as if there is a significant amount of chloride and chlorate present.

Cobalt chloride and zinc: Although some hydrogen is being produced, no cobalt is made at first. After a couple hours, however, microscopic cobalt pieces are made. The amount of cobalt gradually increases, as evidenced by a magnet sweep.

Magnetic metals: Iron, cobalt, and nickel are videotaped. The iron is an electromagnet core; the cobalt is produced by magnesium reduction; and the nickel is a 5 cent Canadian coin.

Copper(II) chloride production. A mixture of about 5:1 ratio of 3% hydrogen peroxide to 31.45% hydrochloric acid dissolves copper well, resulting in a green solution. The copper partially dissolves in the solution again, forming a black mixed oxidation state complex which is oxidized by the air during evaporation.

 

12-21

Nicad battery reactions: The “nickel” crystallized with white crystals after HCl was sprinkled on the electrode, while the “cadmium” began forming wet-looking crystals on the surface of the fluid after significant evaporation. Neither seemed deliquescent, which makes it a puzzle worthy to leave in the past. ;)

Metal determination for CO detector: The metal does not appear to dissolve in the basic solution produced when lithium reacts with water, but neither does the aluminium foil, so it could still be Al.

Mini fireplace: A 2B pencil when heated by its internal lead emits smoke at the ends as they get hot first. Unfortunately, the power supply burnt its fuse.

Alnico magnet extraction: An old dB meter contained an alnico magnet, as evidenced by its lack of fracture when struck.

Capacitor boom: Capacitors when run on relatively high AC voltage tend to vent their electrolyte somewhat dramatically, although not explosively.

Tissue chlorate: The tissue did not seem to burn any more rapidly than normal. There are several potential reasons: 1) the tissue was crumpled up; 2) there was not enough chlorate to provide the oxygen to ignite the inside; 3) the excess of sodium chloride could have a dampening effect on the combustion; 4) the tissue has fire-retardant chemicals in it.

Hydrogen ignition: Zinc was reacted with HCl and the hydrogen produced was ignited by a spark. However, the wood piece attached to the sparking mechanism became moist with the foaming and the spark no longer worked after a few seconds. A repeat experiment worked much better, with the zinc forming massive hydrogen bubbles which ignited wonderfully.

12-22

Magnetism experiment: Various materials were floated on an aluminium foil boat (shown to have practically no magnetism because of impurities) and placed close to a powerful magnet. Their response was documented and compared to recorded responses. Diamagnetic materials repel a magnet, while paramagnetic materials attract a magnet.

The two anomalies were because the carbon rod was probably tainted with iron impurities, and the molybdenum was encased in diamagnetic quartz glass.

Wheel weight dissolution: Wheel weights have begun dissolving in a 1:1 mixture of 5% acetic acid and 3% hydrogen peroxide. If any of the other elements have oxidized in this environment, the white oxides are invisible in the black forest of[redacted] puffy powder that accumulated.

 

Boron extraction: A neodymium magnet was dissolved in HCl for the sole purpose of obtaining boron powder.

Hydrogen ignition: Hydrogen was ignited [redacted].

Hydrogen peroxide concentration: Hydrogen peroxide is cooled in freezer in an attempt to concentrate it for no reason. Some crystals form and are removed. The residual liquid is frozen further.

Lead iodide: Lead acetate, acetic acid, and ascorbic acid are reacted with tincture of iodine. Lead iodide is precipitated. A small amount of lead iodide is dissolved in hot water and a crystallization attempt failed.

12-23

Lead iodide production: A measly, but still significant amount of lead(II) iodide was found on the filter paper. The crystallization experiment may be repeated with the yellow residue on the paper.

Magnet dissolution: A sizable amount of boron was formed by the magnet’s dissolution. The acid solution was washed away very carefully and replaced with water, which was mostly pipetted off. The rest of the water will evaporate, leaving boron powder in the container.

Lead halides: Lead bromide was precipitated by reaction of the lead acetate solution with a saturated aqueous solution of sodium bromide (produced by dissolving NaBr in hot water). Lead chloride was produced by reaction with hydrochloric acid. Lead bromide appears a tiny bit more off white than the chloride, but not much different.

 

[redacted]

Lead iodide production: The lead iodide appears to have turned yellow-brown over time.

[redacted]

Rare earth extractions: Cerium does not appear to oxidize in acetic acid solution spontaneously. Because of the tiny amount of iron in the previous solution (1% or so) it did not precipitate separately from the rest of the rare earth metals. A rerun is attempted with dilute acetic acid and quick removal of the ferrocerium to prevent aerial oxidation of the iron. Upon addition of hydrogen peroxide, the light pink solution turned yellow, just like cerium is supposed to. When sodium bicarbonate is added, however, the yellow does not lighten but instead partially precipitates as an orange precipitate. Neither is reduced by ascorbic acid. Reacidification with hydrochloric acid then activates the ascorbic acid, which reduces it to a relatively colorless solution.

 

 

 

Rare earth extractions: Ferrocerium is added to 2% acetic acid with zinc to suppress the oxidation of iron. Hopefully, the iron(II) will become reduced by the zinc back to elemental iron. The solution appears brownish and changes color slightly between fluorescent and incandescent light. Samarium(II) is a possibility, as well as a combination of several rare earth salts.

Cd

Bottom                                               Top

Material

Experimental Magnetism

Recorded Magnetism

Aluminium

?

Attracted

Zinc

Repelled

Repelled

Bismuth

Repelled

Repelled

Battery junk

Attracted

?

Lead titanate zirconate

Attracted

?

Iron pyrite

Attracted

?

Silver

Repelled

Repelled

Lead/tin(?) foil

Attracted

Lead repelled, tin attracted

Tin/Antimony blob

Attracted

Antimony repelled, tin attracted

Hafnium

Attracted

Attracted

Magnesium

Attracted

Attracted

Gold

Repelled

Repelled

Copper

Repelled

Repelled

Lithium

Attracted

Attracted

Carbon

Attracted

Repelled

Molybdenum

Repelled

Attracted

Sodium chloride

Repelled

Repelled

Lead chloride

Original      After hydrogen peroxide

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February 9 2012 5 09 /02 /February /2012 19:18

This is the public version of the diary of my personal chemistry experiments. The removal of personal and other sensitive information is marked with “[redacted]”. Use Control + F to find what you want in here.

Past

Tin oxidation: tin is heated on an element (heating element), creating some smoke and white tin(IV) oxide.

Lead oxidation: lead is heated on an element, creating some smoke and yellow lead(II) oxide

Magnesium ignition: Magnesium rod ignited in a candle, though with difficulty. Further attempts to ignite magnesium ribbon using candle were unsuccessful. Magnesium ribbon ignited easily when heated on an element. The residue is white magnesium oxide, and the flame is almost pure white and bright enough to hurt eyes.

Lead iodide formation: tincture of iodine was reduced by ascorbic acid to make an iodide solution. Lead was dissolved in acetic acid/hydrogen peroxide, leaving a residue of (likely) antimony and tin. These solutions were mixed to precipitate a bright yellow precipitate of lead iodide.

Iodide formation: Tincture of iodine was reduced by ascorbic acid to make an iodide solution. The iodide is colorless and partially consists of sodium iodide.

Lead chloride formation: Lead chloride was not formed by reacting sodium chloride with the previously prepared lead acetate solution because the Pb(Ac)2 was too dilute. Reaction with hydrochloric acid precipitated the white chloride, however.

Lead bromide formation: An attempt to synthesize lead bromide by the reaction of the previously mentioned Pb(Ac)2 solution with sodium bromide was unsuccessful.

Magnesium dissolution in acetic acid: magnesium dissolves relatively slowly in 5% acetic acid, liberating hydrogen. Zinc, by comparison, underwent no reaction in about 10 minutes, although it has been previously shown to undergo a reaction upon standing.

Copper(II) chloride aluminium reaction: Copper(II) chloride was reacted with aluminium foil shreds to form hydrogen, aluminium hydroxide, copper, and aluminium(III) chloride in a violent reaction.

Galinstan coating removal: When galinstan is properly applied to aluminium foil, it dissolves the protective layer, making it susceptible to aerial and aqueous oxidation. Flaking of aluminium oxide was observed coming from the point of application of the galinstan. The galinstan-coating aluminium also reacted with water, creating hydrogen gas, aluminium hydroxide, and re-precipitating the galinstan as liquid metal beads.

Lithium air reaction: Lithium was put in a closed bag where a limited amount of air was available. It first blackened and then decomposed into a white oxide/carbonate layer. Apparently, either the bag had too much air or the seal was not working as very little nitride was produced. Only the faintest smell of ammonia was present after combination of the oxide/carbonate with water.

Carbon monoxide detector dismantlement: The fuel cell in a CO electrochemical sensor was disassembled. A canister containing an unknown electrolyte (not sulfuric acid) was present, as well as several Teflon sheets found to be impregnated with platinum. The material of the canister is yet to be determined, as it is slightly magnetic. (Later determined to be nickel-plated aluminium.)

12-3

Lead sulfate formation: The previously mentioned Pb(Ac)2 solution reacted with magnesium sulfate to form a white precipitate of lead sulfate.

Ammonium chloride smoke: Tissues were soaked with ammonia and hydrochloric acid and brought near each other. The vapors combined to create a white smoke of ammonium chloride, which was slightly noxious.

Carbon monoxide detector electrochemical cell electrolyte test: According to Wikipedia, most contain sulfuric acid. Mine did not appear to contain it, as a pH test showed a neutral pH. Hardly any residue was left behind after evaporation.

12-8

NdFeB magnet dissolution: A neodymium magnet is dissolved in HCl. The reaction is moderately rapid, with the solution turning yellow-green.

12-9

NdFeB magnet dissolution: The solution has turned a red-green color, from the combined colors of neodymium and iron (possibly praseodymium) chloride. Upon evaporation with hair dryer, it fumed strongly but eventually crystallized as greenish crystals, which continue to release excess HCl. The boron powder was insoluble in HCl and precipitated, but was accidentally lost. The crystals show a tint of red when photographed in non-fluorescent light as a result of the neodymium.


Triiodide electrolysis: An attempt to produce iodine by electrolytically oxidizing triiodide was conducted. The attempt was successful at 5V; the reduced occurrence of oxygen gas helped prevent the carbon anode from erosion. Additional triiodide was added as the iodine yield was less than desired, although the solution was practically colorless. The iodine was filtered. Because of the lack of heating with 5V electrolysis, the alcohol (which did not evaporate extensively) began dissolving the iodine as soon as the electrolysis stopped. The experiment was repeated using 24V, with which the iodine is produced rapidly (10 minutes) and there is much heating of the solution. Iodine can be differentiated from carbon impurities by its sheen; carbon has no reflection capabilities.

NdFeB magnet dissolution: An Nd magnet is again dissolved in HCl, with an attempt being made to separate boron upon reaction completion. The (II) oxidation state of iron may be taken advantage of in order to separate most of the iron from the neodymium chloride. I got HCl acid in my hair from the earlier drying experience.

12-10

Iodine production: iodine can also be separated from carbon by its evaporation rate; my iodine disappeared overnight, despite near-freezing temperatures, leaving dirty filter paper behind.

NdFeB magnet dissolution: Is it NdFeB? There is not B precipitate. However, a magnetic precipitate shown to be nickel or cobalt (nickel is much more likely) by its very slow dissolution in HCl was formed, probably from the corrosion-resistant coating. On later examination, boron in an almost colloidal form had fallen to the bottom of the container. This ultrafine powder mostly passes right through a tissue and so cannot be collected and dried in small quantities. Upon dissolution of a large magnet, a measurable amount of boron dust may be collected.

NdFeB magnet work: The acidic chloride solution was neutralized with sodium carbonate to create a white precipitate that turned brown, similar to manganese. Upon addition of hydrogen peroxide, violent fizzing occurred and a dark red flocculent precipitate appeared to form. The pH was around 7. Some HCl was added to raise the pH to around 2. The dark red precipitate dissolved to form a deep dark red solution whose identity is unknown. Upon addition of more HCl, it lightened to a yellow solution, looking just like an iron(III) chloride complex. When a base is added, a bright red-brown precipitate is formed. The pH was changed to about 4 and the solution filtered. Other than a little iron that leaked through the filter paper, no soluble rare earth metal ion passed through the paper as evidenced by a lack of precipitation when ammonia is added to the filtrate.

Cobalt production: A dilute aqueous solution of cobalt(II) chloride in hydrochloric acid was electrolyzed with a carbon anode and a brass cathode. Practically no cobalt was produced (as evidenced by a magnet sweep), probably because of the dilution.

12-12

Iodine production: Triiodide is reduced with ascorbic acid. Due to an unfortunate accident, an iron solution contaminated the iodide, but it should still be usable. The plan is to evaporate the alcohol, then oxidize the iodide directly to iodine.

NdFeB magnet work: Other than some of the precipitate falling into the iodide solution, nothing happened. A slight color change is noticed when the precipitate is photographed in fluorescent vs. xenon light, but it seems as if I do not have the resources to extract the neodymium. In that attitude, the precipitate was disposed of.

Lead dissolution: I poured off most of the lead solution and added hydrochloric acid to the residue. Lead(II) chloride precipitated, which dissolved in additional acid. The gray precipitate dissolved without much hesitation in a way that made it seem like tin. A test with copper(II) chloride can be used to determine if tin(II) is present. Triiodide seems to have been reduced by the solution.

12-13

Cobalt production: Reduction of acidic cobalt(II) chloride solution by magnesium metal produced, along with vigorous bubbling, pure cobalt metal, as evidenced by its magnetism.

Lithium chloride production: Lithium hydroxide prepared by reacting lithium with water had absorbed carbon dioxide through the container lid gaps and turned into lithium carbonate. This was placed in hydrochloric acid. It dissolved to form a colorless solution of lithium chloride. This can be used to make a flame test.

Magnesium iodide work: Magnesium metal was placed in dilute triiodide solution to determine if reduction would take place. No reduction happened, even after acidification with acetic acid. Reduction of the acid and/or water was only observed, with hydrogen being produced.

Magnesium reduction of magnet chloride: Iron was produced, as evidenced by the magnetism of the magnesium piece. However, the iron dissolved as fast as it was formed in the acidic solution. After the acidity declined, more iron was precipitated, however. Eventually, the iron started oxidizing to iron(III) hydroxide.

Mischmetal separation: After grinding of mischmetal, a black powder remained. It appears to be a magnetic oxide. The rare earth oxides cannot be separated from the iron oxide, unless it is the metal after all. The metal is slightly magnetic itself, so that is a possibility.

Mischmetal reactions: Mischmetal reacts very slowly with hot water, similar to magnesium. When some acetic acid is added, dissolution begins occurring, despite the extreme dilution of the acetic acid (1%). The rare earths are preferentially oxidized, as evidenced by a magnet. Upon addition of bleach, a yellowish-white precipitate is formed, looking a lot like cerium(IV) oxide. Upon addition of acetic acid, it re-dissolves to form a yellow solution.

12-14

Iodine extraction: The almost evaporated solution of iodide mixed with ascorbic acid was electrolyzed. Because the iodine was being reduced as fast as it was being oxidized, bleach was added to speed up the reaction. An instant precipitate of iodine formed, along with much heat. The iodine was then re-dissolved, and the solution became green. The green appears to be an oxidation product of ascorbic acid by bleach. Little bleach was present according to a hydrochloric acid test. When the solution was reduced with additional ascorbic acid, it formed blue-gray iodine crystals as an intermediate; the miniscule quantity is shown on the filter paper below. Most of them immediately dissolved to make brown triiodide, which was reduced to colorless iodide. The oxidation state of iodine in the clear solution upon oxidation of bleach is yet to be reported. The colorless iodide is electrolyzed.

12-15

Iodine production: Iodine blew away. Found a week later in the hedge.

Mischmetal reactions: Another piece of mischmetal is dissolved in acetic acid. A slow reaction was observed in a highly dilute bleach(?) solution. The magnetic precipitate that formed was dissolved in additional acetic acid. The solution is not coloring and the precipitate remains magnetic despite thinning, evidence that the iron is not dissolving in the diluted acetic acid solution. Instead, the precipitate appears to be a magnetic iron-lanthanide mixture with more iron than before.

Magnesium and zinc dissolution: Magnesium and zinc were placed in hydrochloric acid and videotaped doing their thing.

12-16

Mischmetal reactions: The iron-lanthanide hypothesis expressed before is true. The mischmetal acetate solution darkened considerably overnight, while the one with the more recent dissolution remains practically colorless. Below are pictures of before and after standing.

Magnet dissolution: An NdFeB magnet is placed in acetic acid, with hopes that the iron will not dissolve and the resulting solution will not be so caustic. It dissolves very slowly, producing hydrogen and an almost colorless solution.

Battery dissection: The NiCd battery came apart without much trouble. The cadmium appears to be in a fine compacted powder form, not an electrode form. The nickel electrode shows some evidence of green nickel(II) hydroxide at certain locations. The electrolyte papers (seen with the Ni roll) are placed in water to dissolve the KOH and then neutralized with HCl to form KCl. The original solution had a pH of >10. The final solution is soaked into the porch through a hole on the bottom of the container and ate away the paint KFortunately the spot is small enough. A successful math lab project is visible in the background of this photo.

 

 

 

 

Mischmetal reactions: I evaporated the solution of mischmetal acetate to a small puddle by a blow dryer, which crystallized upon cooling. The crystals appear syrupy, as there is probably acetic acid left in them. After placing in the freezer, they remain syrupy. Upon dissolving in water, they are completely soluble, showing that no insoluble oxy-acetate has formed. It appears that the solution has gotten a little darker again, although not much darker.

Cadmium production: The “cadmium” anode from the nickel-cadmium battery was placed in diluted HCl. Chlorine(!) was evolved, and black slime filled the solution. No hydrogen seems to be produced.

Cd

Ni

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July 8 2011 6 08 /07 /July /2011 14:14

Warning: Thionyl chloride is one of the only easily obtainable chemicals that rates a 4--Extreme Risk on the NFPA diamond for health. Do not bring it in the house in anything but a strong, sealed container. Noxious fumes are created in this experiment.

 

You will need:

 

Lithium-thionyl chloride battery (I obtained mine from an EZpass device in the woods)

Water

Drill

Pliers

Very very sealed container

 

Remove as much from the lithium-thionyl chloride battery as you can. These things are built very strongly so a drill is needed. After you remove all the extra stuff from the battery, you should see a carbon rod sticking out on one side. Drill it out. As you drill, you will see smoke and smell sulfur. This is the thionyl chloride around the carbon rod reacting wih the water in the air; it is not fire. After a nice hole is drilled, remove your smoking drill bit. Then, place the battery hole down in the sealed container and let the thionyl chloride drip out. The container may cloud up. You may have to squeeze the battery to get significant amounts of thionyl chloride out. Now you have thionyl chloride. It can be used for producing the anhydrous forms of several metal compounds. It also reacts vigorously with water. Place a drop of it in water. Bubbles of sulfur dioxide will leave, along with some HCl fumes. Both of these gases are very annoying to the nasal passages. Do what you want with the rest of the thionyl chloride.

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July 7 2011 5 07 /07 /July /2011 15:00

Warning: Copper and zinc salts are slightly to moderately toxic. Do not ingest them. Hydrochloric acid is corrosive.

 

You will need:

Brass

Ascorbic acid or sodium metabisulfite

Sodium bicarbonate

Carbon rod

 

Electrolytically oxidize the brass in sodium bicarbonate solution with a carbon cathode. Green copper carbonate and white zinc carbonate are formed. Filter and dissolve the precipitate in HCl. A dark green solution is formed. Add sodium bicarbonate until the pH of the solution is around 2 or 3. Then add ascorbic acid or sodium metabisulfite. White copper(I) chloride will precipitate. Filter. Now you have a copper(I) chloride precipitate and a zinc chloride solution. You have separated brass.

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July 6 2011 4 06 /07 /July /2011 13:52

Warning: Hydrochloric acid is corrosive. The resulting metal chlorides are toxic or carcinogenic.

 

You will need:

 

Alnico magnet

Hydrochloric acid

3% or more concentrated Hydrogen peroxide

Sodium bicarbonate

Sodium hypochlorite

Ammonia, concentrated

Sodium hydroxide

 

Alnico magnets are made of an iron-aluminium-nickel-cobalt alloy. The process for separating them is detailed here.

 

Add hydrogen peroxide to concentrated hydrochloric acid in a 1:1 ratio. Add the alnico magnet. Bubbling is observed and a colored solution is formed. This solution contains these components:

 

Iron(III) chloride, yellow

Nickel(II) chloride, green

Cobalt(II) chloride, blue (in this HCl concentration)

Aluminium(III) chloride, colorless

 

Here are some properties of the chlorides:

 

Iron(III) chloride: Forms alkali-insoluble hydroxide, is not oxidized by bleach, hydroxide does not dissolve in ammonia

Nickel(II) chloride: Forms alkali-insoluble (at normal temperatures) hydroxide, is not oxidized by bleach, hydroxide dissolves in ammonia

Cobalt(II) chloride: Forms alkali-soluble hydroxide, is oxidized by bleach, hydroxide dissolves in ammonia

Aluminium(III) chloride: Forms alkali-soluble hydroxide, is not oxidized by bleach, hydroxide does not dissolve in ammonia

 

Based on these properties, a separation mechanism is thought out:

 

Add sodium bicarbonate to reduce the pH to around 2.

Add excess sodium hydroxide. Cobalt and aluminium dissolve, while nickel and iron remain behind. Filter.

Acidify the cobalt and aluminium solution to neutral and then add excess ammonia. A cobalt ammine complex will form and the aluminium hydroxide will precipitate. Filter and separate.

Add excess ammonia to the nickel and iron precipitate. Nickel should dissolve as the nickel ammine complex. Filter and separate.

 

Results:

 

Nickel(II) ammine chloride, blue solution

Iron(III) oxide, brown precipitate

Cobalt(III) ammine complex, orange solution

Aluminium hydroxide, white precipitate

 

You have successfully separated an alnico magnet.

 

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July 5 2011 3 05 /07 /July /2011 13:19

Warning: Cobalt compounds are toxic and potentially carcinogenic. Do not ingest or inhale them. Bleach fumes may be a problem. The procedures that release chlorine should be done under a fume hood or outdoors.

 

You will need:

Test tube

Cobalt(II) chloride

Bleach (sodium hypochlorite solution)  

Sodium carbonate

Source of heat

Ammonia

Hydrogen peroxide

 

 

Dissolve the cobalt(II) chloride in some water. You will see the burgundy color of cobalt aqua ions. Add bleach. It instantly turns brown-black and cobalt(III) oxide precipitates.  Some chlorine is produced. Filter and dry the cobalt(III) oxide. This oxidation state is only stable in the presence of certain ligands and in a basic state. Acidify the precipitate with hydrochloric acid. Chlorine is released and a cobalt(II) ion is formed. Depending on the amount of excess hydrochloric acid, the color of the resulting solution can be red, blue, or green.

 

Cobalt-III--oxide--1-.JPG

 

Dissolve more cobalt(II) chloride in water and precipitate it with sodium carbonate. Filter and dry the cobalt carbonate produced and heat it. It decomposes to black cobalt(II,III) oxide when heated. It also becomes calcined, making it insoluble in acid. I placed the resulting substance in HCl and it only produced a tiny amount of cobalt(II) chloride before the acid evaporated.

 

Cobalt-II-III--oxide.JPG

 

Dissolve more cobalt(II) chloride in water. Add ammonia. A blue precipitate of cobalt(II) hydroxide will form. This is only one form of cobalt(II) hydroxide, but that is beside the point. Then add some hydrogen peroxide. The solution will turn greenish, then brown as cobalt(III) hydroxide precipitates. The precipitate will be light, fluffy, and insignificant, almost like aluminium hydroxide.

 

DSCF0297.JPG

 

Do this reaction outside. Dissolve more cobalt(II) chloride in water to produce a concentrated solution. Use a carbon anode and an iron cathode. A vigorous electrolysis will result in the formation of a brownish-green precipitate of probably cobalt(II) oxide.

 

Cobalt-II--oxide-2.JPG

 

 

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July 4 2011 2 04 /07 /July /2011 13:41

Warning: This experiment deals with corrosive substances and toxic fumes. Work outside or in a fume hood.

 

You will need:

 

Sulfur chloride mixture

Water

Sulfur

 

The sulfur chloride mixture created in a previous experiment should be orange or red. Add some sulfur to it when warm. The sulfur should dissolve and react with the red sulfur dichloride to make yellow disulfur dichloride. This sulfur chloride is more stable. Disulfur dichloride dissolves sulfur as well. Add disulfur dichloride to water. A yellow solid is formed, along with release of sulfur dioxide gas and hydrogen chloride fumes.

 

 

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