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Make a Tritium Nuclear Battery or Radioisotope Photovoltaic Generator
updated
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Clips from old videos featured in this one:
Gold Chemical Resistance
youtu.be/ng6DGwiKWag
Platinum Chemical Resistance
youtu.be/fro-L5gSyh4
Platinum bar dissolving in Aqua Regia
youtu.be/APxL87X92t4
Dissolve Platinum with chlorine gas
youtu.be/JFNtP2N2Eho
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If you electrolyze water you generate hydroxide ions at the cathode, and hydronium ions at the anode. If you could some how split sodium bicarbonate, then mix the sodium ions with the hydroxide ions, you could make sodium hydroxide.
Of course "just" splitting ions completely glosses over the nuances and complexities of chemistry. But interestingly enough, a cationic exchange membrane like nafion essentially allows us to that by allowing cations to transfer through, but blocks anions.
To do this, all we do is get the nafion divided membrane cell we built in a previous video and insert it into a larger container of water and sodium bicarbonate. Using a titanium cathode and a cobalt oxide anode (although you can use nickel, platinum, or carbon), we make the sodium bicarbaonte solution the anolyte and use deionized water as the catholyte. Applying an electric current we separate the ions in sodium bicarbonate and pass the sodium through the membrane into the cathode side where they meet up with the hydroxide produced and create sodium hydroxide.
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Ever wish you could filter just one ion? Nafion is an ionic polymer or "ionomer" that has sulfonate functional groups as part of it's PTFE structure. These sulfonate groups make the nafion permeable to cations, very similar to cationic ion exchange resin. Cations can hop from sulfonate group to sulfonate group and transfer through the membrane. Anions are blocked.
So if we apply an electric field we can force cations through the membrane and separate them from anions.
In this video we make a single compartment membrane cell that we'll use in a future video to make sodium hydroxide from sodium bicarbonate.
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Related videos:
Ruthenium is invulnerable to aqua regia: youtu.be/H7Ng4sOVkns
Chemical resistance of platinum: youtu.be/fro-L5gSyh4
Dissolving platinum in aqua regia: youtu.be/APxL87X92t4
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Related videos:
Production of nitric acid by thermal decomposition of copper nitrate: youtu.be/hmB5x0LYfSE
Purification and concentration of nitric acid: youtu.be/88gbfCnrV8o
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But this is only a problem with fuming 100% nitric acid. The more common concentration of 70% does not set nitrile gloves on fire. Nonetheless for higher safety, vinyl gloves are recommended and if you can afford them, viton gloves.
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Normally to make nitric acid you react a nitrate salt with a strong acid like sulfuric acid. But what if we wanted to make it without any acids at all? Copper nitrate has the interesting property that if it's heated it will decompose into nitrogen dioxide and oxygen, two components needed for nitric acid. Best of all copper nitrate itself can be made with domestically available that don't require acid either.
First calcium ammonium nitrate is boiled with calcium hydroxide to produce pure calcium nitrate. This is done only to remove ammonia and not necessary if calcium nitrate can be obtained directly. Calcium ammonium nitrate is a fertilizer. The resulting calcium nitrate is reacted with copper sulfate which is available as a root killer. The resulting copper nitrate solution and calcium sulfate are filtered and the copper nitrate is boiled to remove most of the water until it starts to change color to green/blue.
The copper nitrate is then hooked up a distillation apparatus and heated until it decomposes. The nitrogen dioxide gas produced is lead into water to dissolve. The nitric acid produced is then purified by distillation. Yield is between 60%-80%
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I was exploring more nitric acid and wanted to see if calcium nitrate and sodium bisulfate would be viable. The rationale is that the reaction of calcium nitrate and sulfuric acid is well-known but almost never done directly since it produces insoluble calcium sulphate that solidifies into a rock in the flask. It has to be drilled out and risks break the flask. The traditional way to use calcium nitrate is the "wet process" where we first mix it with water and then add sulfuric acid. The calcium sulfate precipitates out and the dilute nitric acid is filtered and purified by distillation. This is slow and laborious so i was wondering if sodium bisulfate could be advantageous in producing a residue that didn't need to be drilled. This would save time and less risk of breaking glassware.
So i mixed 49g of calcium ammonium nitrate decahydrate with 150g of sodium bisulfate monohydrate and heated it directly in the "dry process" of making nitric acid. Nitric acid was distilled over and the yield was 85%. But more importantly the solid residue of sodium sulfate, sodium bisulfate and calcium sulfate was soluble. Upon addition of water it dissolved into a slurry that could easily be poured out. So i think the process is superior to using sulfuric acid as there is overall less labor involved.
For thoroughness i also tried the wet process by first dissolving the calcium nitrate in 50mL of water and adding sodium bisulfate. After distillation the yield was 95% but with 50mL of extra water diluting it. Personally i prefer higher concentration acid and don't mind the lower yields of the dry process.
Anyway. I was going to do additional nitric acid experiments but my hotplate failed.
Turns out the temperature sensor failed open and the safety limit of the hotplate refused to turn it on. It was a simple matter of finding the broken sensor and replacing it. The interesting note is that the hotplate uses a PT1000 RTD and it seemed the original was spot welded in. I didn't have spot welding capability so i used copper foil to crimp the connection.
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I actually try a few methods like dissolving them in water first and varying the amount of reagents. Overall the best method i found was to thoroughly mix 43g of sodium nitrate with 150g of sodium bisulfate and then directly distill off the nitric acid. Yield was about 95% nitric acid at 75% concentration.
To remove unsightly dissolved nitrogen dioxide, hydrogen peroxide, ammonia or urea may be added in small portions to react it away.
Related videos:
making sulfuric acid by the copper chloride process: youtu.be/l2AkVYxDSKc
Old video on making nitric acid (which sucks): youtu.be/2yE7v4wkuZU
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A reverse osmosis deionization system purifies water by first subjecting it to reverse osmosis to remove most of the minerals, and then passing it through a column of deionization resin to remove at leftovers. This resin has a very limited capacity and often represents the most expensive recurring cost of such systems. Normally they are discarded when spent, but can be regenerated chemically.
First a 15% solution of sodium hydroxide is prepared by mixing water and sodium hydroxide in a 3/17 ratio by mass. So for 170g of water, 30g of sodium hydroxide are added. This solution is added to spent deionization resin (80mL-200mL). The anion exchange resin component will float to the top while the cation exchange resin component sinks to the bottom. The solution also regenerates the anion exchange resin. The two resins are separate by pouring. The anion exchange resin is repeatedly washed with deionized water. The cation exchange resin is washed a few times with equal volumes of water and then regenerated by mixing with a equal volume of 5% hydrochloric acid (made by mixing 30% hydrochloric acid in a 1:4 ratio with water). After letting it sit for an hour, the cation exchange resin is filtered and also washed repeatedly with deionized water.
The two resins are now regenerated and can be recombined to make mixed-bed deionization resin.
#deionization #resin #regeneration
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Most sources of water that an amateur chemist may use (like tap water) contain dissolved salts. These salts usually consist of sodium, calcium, or magnesium carbonates, chlorides and sulfates. Water containing significant quantities of these minerals is often called "hard water". And they can be easily observed by letting a quantity of water evaporate completely. While these minerals are usually very low in concentration and inconsequential for most domestic purposes like drinking, cooking or bathing, they are a contaminant for performing chemistry. This can be particularly detrimental to sensitive experiments like analytical chemistry, crystal growing, or electrochemistry. So removal is preferred.
The historical technique for removing non-volatile mineral contaminants is distillation. For very small quantities distillation is cheap and effective as most amateur chemists already have distillation equipment. But for larger quantities, distillation is very energy intensive and expensive due to electricity costs. It's also extremely slow.
Reverse Osmosis Deionization is now the standard for making purified water as such systems are much easier to purchase in the modern era. A basic system has a carbon prefilter that takes in water and neutralize the chlorine normally added to sterilize. This is done to ensure the chlorine cannot damage the reverse osmosis membrane. The water then proceeds to the membrane that consists of a rolled envelope of polyimide plastic. This membrane passes water, but resists the passage of minerals and salts. The wastewater that contains the leftover minerals is discarded, while the permeate water with most of the minerals removed is sent to a column of deionization resin. This resin is made of a special ionically charged plastic that swaps out mineral ions in the water for hydronium or hydroxide ions. Those ions neutralize to become water and the result is purified water with all the minerals removed. While not strictly necessary, purified water improves the quality and reproducibility of amateur chemistry experiments so a reverse osmosis system is a recommended addition to an established amateur lab.
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It's well known that ruthenium is a highly resilient metal capable of withstanding chemical attack by very corrosive acids like nitric acid, hydrochloric acid, sulfuric acid, aqua regia, etc. So it would be make sense to fashion jewelry out of such a resistant substance. But ruthenium is highly susceptible to attack by sodium hypochlorite. To test this we immerse a ruthenium plated ring into household bleach. Unfortunately the ruthenium plating very clearly dissolves off within minutes, producing sodium ruthenate and peruthenate salts as well as bubbles of ruthenium tetroxide gas.
Since these substances are highly toxic. And bleach is a commonly encountered substance in everyday life, it is recommended to discontinue use of ruthenium for jewelry.
Related videos:
Chemical resistance of Ruthenium: youtu.be/H7Ng4sOVkns
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#ruthenium #bleach #safety
Get 60g of silica gel based cat litter. This is often called "crystal cat litter". Add to it 30g of sodium hydroxide and 100mL of water. The reaction will get hot so be careful. This reaction forms sodium silicate. You may have to leave it overnight if it goes slowly. But few grains of leftover cat litter is acceptable.
Dilute the mixture by adding another 800mL of water. This cannot be added earlier as the mixture must be highly concentrated to successfully make sodium silicate.
Thoroughly mix the solution.
Now drop in a dozen large crystals of copper sulfate (around 1-2cm size). It's recommended to separate them for best looking results.
Over the course of two days the crystals will seem to sprout and grow as the reaction progresses.
What's happening is quite fascinating. As soon as you drop the crystals in, the surface of the copper sulfate dissolves but immediately reacts with the sodium silicate solution to form solid copper silicate. This coats the crystal so it's encased in a layer of copper silicate. But the silicate layer isn't perfectly impervious or rigid, water can still diffuse in. As it diffuses in it dissolves the copper sulfate underneath and forms a solution. This concentrated solution pushes out as the water continues to diffuse in and increases in pressure. The copper silicate membrane bulges out but eventually it can't contain the pressure and ruptures. The copper sulfate solution rushes out of the rupture and instantly reacts with sodium silicate solution to form another layer of copper silicate.
This layer is newer and weaker so as the pressure builds again it too will rupture and the process repeats. This gives the appearance of a growing structure. It grows upward because the density of the copper sulfate solution is lower than that of the sodium silicate.
Overall this looks like a growing stalagmite of copper silicate.
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The first method is merely boiling household ammonia solution that's domestically available from the local supermarket. The ammonia boiled out is lead into cold water where it can be dissolved. While this did work the yield was quite low at around 2.5g per 100mL of household ammonia solution. From the 600mL of ammonia solution used only about 15g was obtained.
The second method was to revisit the classic method to produce sodium nitrate from ammonium nitrate and sodium hydroxide by dissolving them both separately in water and then mixing them together and trying to boil out the ammonia. This worked terribly and i got almost no yield at all.
The third method that seemed to work the best was to react urea and sodium hydroxide in water. This reaction was well-behaved, steady and easily performed with domestically available chemicals. Starting from 200mL water, 90g urea and 120g sodium hydroxide, about 38.6g of ammonia was obtained.
I intend to use the ammonia in a future project to make nitric acid.
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Related videos:
Restoring Silver by electrochemistry: youtube.com/watch?v=57iwtmT4LNQ
Toning Silver by Anodization : youtube.com/watch?v=GajkqaSr01c
Make zinc powder: youtube.com/watch?v=3X9c6epL7HQ
Make silver powder: youtu.be/WRgSviGuEFY
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The process is pretty simple. Make a solution of 1g silver nitrate in 50mL water. Submerge an anode made of pure silver (i'm using silver coins) and a cathode of carbon. Connect the anode (silver) to the positive terminal of a variable power supply and connect the cathode (carbon) to the negative terminal. Apply a current and raise it until the cathode just starts to bubble hydrogen and then lower it about 25%. Magnetic stirring and a stir bar should be applied to constantly shred the silver dendrites as they grow.
Eventually the anode will be consumed and the solution is decanted to recover the silver powder. The silver powder is washed a few times with water and then dried by heating on the hot plate.
Related videos:
Restoring Silver by electrochemistry: youtube.com/watch?v=57iwtmT4LNQ
Toning Silver by Anodization : youtube.com/watch?v=GajkqaSr01c
Make zinc powder: youtube.com/watch?v=3X9c6epL7HQ
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Related videos:
The original video of making silver nitrate: youtube.com/watch?v=d6hPgGV_qAg
Very simple silver photography: youtube.com/watch?v=8e0-AbwBDYM
Silver conductive ink: youtube.com/watch?v=EBlqPS8boLI
Silver mirrors: youtube.com/watch?v=hUX_cpFWNso
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Related videos:
Pyrimethamine playlist: youtube.com/playlist?list=PLU79801KtVAUnKYktg8sXJUaEbHKxX5xx
Grignard reactions: youtu.be/EFQWD7-DCPI
Dean stark apparatus: youtube.com/watch?v=jxgpLp279Yc
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#Mothersday
Related videos:
Original video on how to make trimethyl orthoformate: youtu.be/TmUNTkP2nw0
How to make sodium: youtu.be/BsNoiFj3wlw
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Potassium Permanganate will directly react with various fuels like glycerol, PEG-based brake fluid, and antifreeze, to start fires. All you have to do is mix them.
For less reactive fuels like gasoline and mineral oil. It can be mixed and then a few drops of sulfuric acid added to create manganese heptoxide which is a powerful oxidant and will itself ignite most fuels.
Related videos:
The science of flaming brake fluid and pool chlorine: youtube.com/watch?v=SSNPtuAcTm0
I obtained my Potassium Permanganate here: amzn.to/2XAWxdB
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#PotassiumPermanganate
To do the demonstration: First get any soft drink can and using sandpaper, sand off the label. Then open the can and suspend it by the tab in 5% hydrochloric acid. The exact concentration is not critical. The can must be opened or it will rupture as the aluminum is removed.
over the course of an hour, the aluminum in the can will be attacked by the acid and dissolve away. This leaves behind the drink and also a very thin plastic liner inside the can. This liner protects the drink from leaching metals out of the can. Carefully lift the can to reveal the liner still holding the drink.
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#coke
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#sodium #Lithium
First, we get a flask and add in 14g of magnesium metal, this can be obtained from fire starters. Then we add in 20g of sodium hydroxide which is acquired from drain opener. Now the key catalyst is 1-2g of menthol crystals, these can easily be bought online. A magnetic stir bar should be added at this point. On top we add in 125mL of mineral oil, i recommend hypoallergenic baby oil. Finally, 3g of sodium metal is added to jump start the reaction and serve as a drying agent. If this cannot be obtained then the lithium hacked out of an AA energizer battery can be used.
The reaction mixture is connected to a gas bubbler and a thermometer is inserted. Magnetic stirring is applied and the contents kept suspended to prevent hot spots.
The mixture is heated to 120-130 celsius for 2 hours or until bubbling stops, whichever comes first. What's happening is the sodium or lithium metal jump start is reacting with any moisture present and destroying it. This is necessary to prevent damage to the glassware from the highly caustic reaction mixture at higher temperatures. If this damage is acceptable then the jump starter metal may be ignored.
After 2 hours or when the bubbling stops, heating is increased to 200 Celsius. Sodium metal is produced here as the magnesium reacts with sodium hydroxide to produce sodium, magnesium oxide, and hydrogen. Menthol serves as the catalyst, allowing this reaction to proceed in a controlled fashion at 200 Celsius. Other catalysts like tertiary alcohols or borneol may also be used.
Heating is continued until bubbling stops, about 30-40 hours in the case of menthol. After cooling, the sodium can be boiled in dioxane to separate excess magnesium. Alternatively, the sodium can be remelted into an ingot, and the excess magnesium cut away as it tends to settle at the bottom.
Approx yield is 10.9g or 94%
Related videos:
Make sodium metal with domestic chemicals (thermochemical dioxane process): youtube.com/watch?v=jCrFFVVcPUI
Make dioxane: youtube.com/watch?v=9Zzrn-61XAY
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#Sodium #Menthol
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#sodium
For the anode, carbon, platinum or mixed metal oxide works best. For the cathode, almost any metal can be used but titanium is preferred.
The electrodes are simply inserted into a solution of potassium chloride salt and a current is passed through. The anode is the positive connection while the cathode is the negative connection. The current should be adjusted to match the surface of the electrode. For carbon that's around 40ma/cm^2, for platinum 300ma/cm^2, for mixed metal oxide 200ma/cm^2. You can use less current for lower heating and wear but the production will take longer.
The electrolysis must be kept in a well ventilated area since it produces hydrogen gas as well as small amounts of chlorine gas.
As the reaction progresses the potassium chlorate will precipitate our and the potassium chloride will be depleted. This has the overall effect of lowering the solution concentration. Every so often the salts must be topped up. Saturated potassium chloride solution has a density of 1.16g/mL. I recommend adding more potassium chloride salt when the density drifts below 1.1g/mL
I ran my cell for 40 days but you can run for as long as you like. But i recommend stopping and processing your reaction before your electrodes are more than 30% submerged in solid potassium potassium chlorate.
Simply remove the electrodes and filter the cell contents to obtain large crystals of potassium chlorate. For greater yield you can boil the supernatant to disproportionate the potassium hypochlorite and squeeze out a few more percent of product. This is optional though and not necessary if you intend to reuse the solution in future runs.
If you wish to have finer crystals of potassium chlorate, you can recrystallize the potassium chlorate from boiling water at a ratio of 60g of potassium chlorate per 100mL of water.
total yield for my runs at 2A current for 40 days is 705g or 48%.
Related videos:
Making potassium chlorate from bleach: youtube.com/watch?v=JtxQT7aVDeg
Fake platinum electrode:
youtube.com/watch?v=uDQuP4oCOgo
Chemists lights a barbecue with potassium chlorate:
youtube.com/watch?v=eRtaPlEcEUU
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Where i got my Platinum anodes:
amazon.ca/TWL-Platinized-Titanium-1-Inch-4-Inch/dp/B00JKXKTZO
Recent reviews and commentors suggest the platinum anodes in the above link may have been replaced with fake ones. If you do buy them, test them right away and return immediately if they are.
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Thanks for 10 great years.
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#sodium
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#sodium
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#sodium
Related Videos:
"Hydrogenation: transform liquid oil into solid fat" by applied science: youtu.be/oqdDWA9-DSY
"Making Margarine: Edible Chem" by Nilered: youtu.be/drIm8_1CvjQ
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#sodium #nickel
Related Videos:
Using grignards to make tertiary alcohols: youtube.com/watch?v=EFQWD7-DCPI
Previous lab notes on making sodium involving tea tree oil: youtube.com/watch?v=v7o3ZfX0BQc
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#sodium #4-Terpineol #TeaTreeOil
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If you want to buy the model kits featured at the end of the video. You can purchase them at:
realatoms.com
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Tea tree oil is found to have lackluster but still promising potential as a catalyst.
Related Videos:
Using grignards to make tertiary alcohols: youtube.com/watch?v=EFQWD7-DCPI
Using 7-hexyl-7-tridecanol to test if sodium production was even possible: youtube.com/watch?v=D4vDwQ4TyIc
Previous lab notes on making sodium: youtube.com/watch?v=juWlrKdsjm4
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Slow heating with aluminum powder proved very effective. But lithium metal was determined to work best.
Related Videos:
Previous lab notes on making sodium: youtube.com/watch?v=av4zfDV5Mng
Previous very crappy video on getting lithium from an energizer battery: youtube.com/watch?v=BliWUHSOalU
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It turns out water might be the primary trigger for the glassware degradation. So the sodium hydroxide was stirred with molten sodium for a few hours to thoroughly react away all the water and dry it out. Then the sodium production react was performed as usual.
This time the glassware survived the reaction without visible damage. An additional bonus was the yield was considerably higher at 96%. It seems the glassware destruction introduced impurities that considerably lowered yield. Elimination of the destruction pathway allowed all the reactants to be used.
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Previous lab notes on making sodium: youtube.com/watch?v=Rra3N-kaGhg
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Hydrobromic acid is the bromine analogue of hydrochloric acid. While too expensive to use as much as hydrochloric acid, it's often used when the bromine element itself is needed. For example a major use is the synthesis of organobromine compounds like the ones we used in our grignard reactions.
To make it, we start with 400mL of water and add to it 250g of sodium bromide. Sodium bromide is available as a bromine source for swimming pools. To this we add 200mL of sulfuric acid, I got mine from drain opener.
The mixture is stirred until everything is dissolved and then cooled to freezing to crystallize out the byproduct sulfates and bisulfates.
The filtrate is then distilled until half the volume has been transferred and then allowed to cool. More crystals should crash out. This is filtered again and the filtrate is again distilled.
The distillate is then fractionally distilled to obtain constant boiling acid at around 124-126 celsius.
If the acid is yellow or orange, this indicates bromine formation. To remove it sulfur is added (1g per 100mL) and then distilled. The bromine-free distillate will have colloidal sulfur in it so it can be refluxed for an hour to drive the sulfur into the column.
Alternatively sodium metabisulfite can be added in small amounts until clear. Then distilled again to leave behind the sodium bisulfates.
Related videos
make hydrobromic acid: youtube.com/watch?v=C3n4Xqfb9qk
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Most cat litter is made from clay but "crystal" cat litter or "silica" cat litter is made from silica gel. Silica gel is amorphous silicon dioxide made by aqueous chemistry is very easy to convert into other silicon compounds.
The process is quite straightforward: 60g of silica gel based cat litter is mixed with 100mL of water. Then 80g of sodium hydroxide is slowly added to dissolve the silica gel. What's produced is a solution of sodium silicate.
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The Dean Stark Apparatus: youtube.com/watch?v=jxgpLp279Yc
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Basically, i've been optimizing sodium production. So far i can get it up to 60-70% yield just with cleaner techniques.
I've been making more hydrobromic acid and have and improved method of making it using sulfuric acid, and purifying it using sulfur or sodium metabisulfite.
i've also have a new piece of lab equipment called the clevenger apparatus.
--------------------
In this video we make dimethyl dioxane from propylene glycol based antifreeze.
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Related videos:
Making sodium by the thermochemical dioxane process: youtube.com/watch?v=jCrFFVVcPUI
"Progress report: Theory test": youtube.com/watch?v=D4vDwQ4TyIc
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After many failures i decided to go to other end of the spectrum and try an experiment constructed under ideal conditions that would have far greater chances of working. While it would be thousands of times more expensive to make sodium this way, it would nonetheless prove or disprove whether it was possible. If it failed, it would show it was impossible or just very hard and thus not worth pursuing with my limited time.
To do it, 10mL of 7-hexyl-7-tridecanol were placed in a flask with 0.5g sodium metal (to jump start the reaction). A reflux condenser was fitted over the flask and the contents heated until the sodium melted and dissolved. 3g of magnesium metal was added and heated for another 30 minutes. 4g of sodium hydroxide was added and heated for three hours. Tiny spheres of sodium formed as alcohol catalyzed the reaction of sodium hydroxide and magnesium metal.
This was a success. And thus proves that we can make sodium this way and thus it's worth to keep trying for cheaper conditions.
Related videos:
How to make tertiary alcohols by the grignard reaction: youtube.com/watch?v=EFQWD7-DCPI
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