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The Final Steps of Making Pyrimethamine (Daraprim)
updated
My previous videos on dissolving platinum:
youtu.be/APxL87X92t4
youtu.be/MlMj3VEYBMA
First we meticulously clean the beakers and condensing flask by first pyrolyzing them in an oven at 500 celsius for 24 hours. This destroys any residual organics. Then we boil dilute aqua regia in them to remove lingering inorganic residues. One troy ounce of platinum is then dissolved over 2 days using aqua regia in that beaker. Once it's dissolved it's boiled for another day to decompose any remaining nitric acid. The chloroplatinic acid solution is then evaporated down to less than 80mL and carefully pipetted into ampules. The ampules are then dried in mason jar desiccators over several weeks before finally being flame sealed. To ensure safety the ampules are soaked in sodium metabisulfite solution to remove any possible contamination of chloroplatinic acid and then labelled. They are vacuum sealed into plastic bags for shipping
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In this video we show how to get or extract thorium dioxide from commonly available thoriated Tungsten rods. Thoriated tungsten rods contain 2% thorium and are easily available online. They're among the easiest to get sources of radioactive materials other than smoke detectors. To extract the thorium, we need a way to remove the tungsten in the rods. Tungsten is resistant to acids but it is vulnerable to hydrogen peroxide. Although i prefer using electricity which is even cheaper than peroxide and also safer if handled correctly. For our 60g of thoriated tungsten rods we make our electrolyte consisting of 40g of sodium hydroxide in 200mL of water. We apply an electric current with the tungsten rods being our anodes. We can use any conductive metal for the cathodes but i'm using tungsten as well for convenience. We apply an electric current of 2amps with a maximum voltage of 6 volts. And that slowly dissolves the tungsten. I ran into the problem of the tungsten rods breaking in them middle due to uneven dissolution, so i used titanium tea infusers as anode baskets.
Eventually the tungsten dissolves into sodium tungstate and the thorium drops away as thorium dioxide powder. I tried to filter the powder but it passed through. I could use a finer filter but instead i just simply let the powder settle and decant it. Then i washed it a few times with water and decanted again. This then produced crude thorium dioxide powder. This is good enough for most purposes, but if you really want it cleaner you can remove leftover tungsten dust by stirring the thorium dioxide with hydrogen peroxide (5%), it will take a few days but it will dissolve the tungsten into tungstic acid. If you have sodium hydroxide in solution it will create soluble sodium tungstate that can be washed off.
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The process is rather simple, dissolve 300g of Calcium Ammonium Nitrate (A common fertilizer) in 1L of water and then dissolve 150g of Oxalic Acid dihydrate in 300mL of water with heating. Then mix the two. A white precipitate of calcium oxalate is formed. Filter this off and distill the filtrate. The distillate will be dilute nitric acid. Fractionally distill that to get azeotropic nitric acid. The yield is around 74%
Related videos:
Making Sulfuric Acid by Oxalate Precipitation: youtu.be/iDlFEV8bT3c
Make Potassium and Sodium Nitrate from Calcium Nitrate: youtu.be/RlonW4iJYrw
Purifying and upgrading nitric acid: youtu.be/88gbfCnrV8o
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Cesium - 137 is a radioactive isotope and one of the major components of nuclear fission waste. The various nuclear weapons tests and nuclear reactor accidents has spread detectable amounts all over the world. I obtained some blueberries that originally came from europe and have detectable cesium content. but i wanted to quantify it accurately so to perform the analysis i concentrated the caesium into a few grams of salt by "digesting" the blueberries with sulfuric acid. The acid completely destroys all organic matter and leaves behind the sulfate salts of any remaining inorganic elements including caesium. Using the built-in detection and analysis functions of my radiacode i was able to determine the activity was 150Bq. Since i started with a 60g sample, this meant the bulk activity was 2500Bq/kg. For comparison, the maximum allowed activity for food in most countries is 100Bq/kg, so the blueberries exceeded that by 25 times.
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Potassium nitrates and sodium nitrates are sought after for their uses in... umm.. fertilizer.... as well as for making alternative aqua regia. I've previously shown how to make them from ammonium nitrate, but ammonium nitrate is getting harder and harder to find as stricter regulations are enacted. Fortunately it seems calcium nitrate is widely available as fertilizer and has much less restrictions. I could easily buy it online from various e-commerce vendors.
Calcium nitrate by itself is usable to make nitric acid directly, but potassium nitrate or sodium nitrate themselves are specifically desired, then it can be converted. To do so, Calcium nitrate is first identified by looking at its NPK value to determine the exact form and the molar nitrate equivalent is found. That quantity is then reacted with equivalent amount of alkali, like potassium hydroxide or sodium carbonate, and then filtered. The filtrate contains the corresponding alkali nitrate that can then be dried or crystalized.
For potassium nitrate specifically. Potassium chloride may be reacted with calcium nitrate and the solution heated until dissolved. Then filtered and allowed to cool and the potassium nitrate directly crystalizes out. This is filtered and retained. Although it is rather impure and needs to be recrystallized again for best purity.
Related videos:
Make nitric acid from calcium nitrate and sodium bisulfate: youtu.be/Xa2OMNaHn_Y
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The idea is rather simple, oxalic acid produces insoluble metal oxalates with a lot of metal salts. But in doing so, the salt anions are left behind in solution and become their respective acids. So a metal sulfate can be converted into sulfuric acid by removing the metal ions with oxalic acid. The conversion isn't perfect, but it's good enough to give better than 50% yield under the right circumstances.
300g of Iron (II) sulfate heptahydrate was mixed with 1L of water and stirred until dissolved. Then 200g of oxalic acid with heated with 300mL of water until dissolved. The two liquids are mixed and iron oxalate precipitates out. This can be filtered but for improved yield, i found leaving it out in the sun to photolyze any dissolved Iron (III) oxalate for 8 hours increased yields by 10%. After filtration the filtrate is boiled down until it starts to crystalize and then cooled and filtered again before the filtrate is distilled at high temperature to get sulfuric acid. Effective yield was around 67%.
I wasn't able to get Magnesium sulfate or copper sulfate to work. I think magnesium sulfate just doesn't work, but copper sulfate produces ultrafine copper oxalate that can't be filtered.
Related videos:
Purification of Sulfuric Acid by Distillation: youtu.be/0Gb9rM9BJ8I
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Previous videos:
Purification of Sulfuric Acid by Distillation Revisited: youtu.be/0Gb9rM9BJ8I
Lab notes - Making Oleum - Success (part 1): youtu.be/wB2zzm8VP9Y
Lab notes - Making Oleum - 20% yield improvement: This Video
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Turns out, it's not too expensive. Oxygen can be made entirely artificially by electrolyzing water. So most of the cost is the electricity to do so. Factoring in additional costs of water and maintenance, it costs approximately 45-50 cents per day to breathe.
Edited by Ciggy Snake, check out his channel at: youtube.com/@UCHgAcJ_wd5qQ3-qPO15oOkg
Stock photo from freepik.com
music from: youtube.com/watch?v=sQPDe1mU31s
Turns out it is possible to do it with just a ceramic hotplate, sulfuric acid, and sodium bisulfate. Along with standard laboratory glassware. But so far the yield is around 13%. I'm trying to optimize it.
The procedure is simply heat the sodium bisulfate on the ceramic hotplate and pyrolyze it until it becomes sodium pyrosulfate. Then let it cool and add in sulfuric acid. Distilling it again yields sulfur trioxide.
Previous methods require much higher temperatures to pyrolyze the sodium pyrosulfate directly.
Related videos:
Purification of Sulfuric Acid by Distillation Revisited: youtu.be/0Gb9rM9BJ8I
Lab notes - Making Oleum - Success (part 1): This Video
Lab notes - Making Oleum - 20% yield improvement (Part 2): youtu.be/hUyJ6CibhSg
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I start by highlighting the inherent dangers associated with handling sulfuric acid and stress the importance of safety precautions, including wearing protective clothing and performing the procedure in a well-ventilated area or fume hood.
I explain why obtaining purified sulfuric acid is essential for certain chemistry experiments and discuss common sources of impure sulfuric acid, such as drain cleaner or battery acid. I then detail the equipment needed for the distillation process and share improvements I've made, like using a ceramic hotplate stirrer and PTFE pipe threading tape for sealing joints.
Throughout the video, I emphasize safety measures, such as using a containment bin to mitigate potential glassware failure and avoiding direct contact with boiling sulfuric acid. I provide tips for recognizing when pure sulfuric acid begins to distill over and explain the challenges of achieving concentrations higher than 98%.
Additionally, I address safety protocols for handling spills or accidents involving sulfuric acid, including neutralization procedures and the importance of protective gear. I also discuss the chemical properties of sulfuric acid and its various applications in chemistry.
Overall, this video serves as a comprehensive guide to safely purifying sulfuric acid for laboratory use while highlighting the risks involved and the precautions necessary to mitigate them.
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In this video we review the radiacode 103, a handheld gamma ray spectrometer. We also as explore basic aspects of gamma ray spectroscopy.
Geiger counters measure radiation, and they're easy to buy online. But all they do is measure how much radiation there is. The Radiacode is a gamma spectrometer and can measure the energy of each individual gamma photon hitting it. When plotted on a histogram this gives a spectrum of gamma ray energy. This is tremendously useful because each radioisotope has a characteristic gamma ray spectrum that can be used to identify it.
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The operating principle is that sulfuric acid would react with potassium chlorate and sugar to catch fire. So to turn it into a match, the sulfuric acid was stored in a glass capsule that was broken and mixed with potassium chlorate and sugar. This would ignite and set fire to the paper roll it was packaged in.
Related video: Lighting Matches with Acid - youtu.be/oc3U2P9PlXY
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Typically, amateur chemists use sodium nitrite, hydrochloric acid, and isopropyl alcohol for this process, but sodium nitrite is becoming harder to obtain. This sodium nitrite-free pathway goes through nitrosylsulfuric acid which can be made using more easily obtained fuming nitric acid and sulfur dioxide.
To make fuming nitric acid from you can use this video: youtu.be/88gbfCnrV8o
How to make sulfur dioxide: youtu.be/2AFKlLSwUZ4
To begin, we dry 400mL of 99% isopropyl alcohol using molecular sieves 3A (that itself was previously dried at 200 Celsius). In a separate flask, we mix 63g of fuming nitric acid with 150mL of glacial acetic acid, keeping the mixture cool in an ice bath.
To make glacial acetic acid, i refer you to Nile Red: youtube.com/watch?v=8iG_qnkF08Y
or Amateur chemistry:
youtube.com/watch?v=FOb4R5_LK-I
Meanwhile, a sulfur dioxide is injected from a sulfur dioxide generator into our nitric acid mixture forming nitrosylsulfuric acid.
After the reaction, the nitrosylsulfuric acid precipitates out. It's filtered and i got a Yield of 117g or 91%. Due to its instability, it must be used promptly. It's slowly combined with chilled isopropanol, creating isopropyl nitrite. Careful addition and temperature control are crucial to prevent decomposition.
After the reaction, we add ice and make up the volume to 1L to separate the isopropyl nitrite. A separatory funnel is used to recover the lighter organic phase of isopropyl nitrite. The final yield is 56g or about 63% based on nitric acid, with an adjusted yield of 69% based on nitrosylsulfuric acid quantity.
While this method may not match the ease of sodium nitrite-based processes, it serves as a valuable alternative for those facing sodium nitrite availability challenges.
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To make it, 60g of potassium chlorate are mixed with 30g of iron metal powder and 2g of calcium oxide. The powders are thoroughly mixed and initiated by direct flames or a sparkler. The reaction burns the iron powder and generates enough heat to decompose the remaining potassium chlorate into oxygen and potassium chloride. Such devices are used often in air craft, submarines, mining operations, and even space craft.
Smarter Everyday on a submarine: youtube.com/watch?v=g3Ud6mHdhlQ&t=620s
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Inside of them is a water activated exothermic chemical reaction. The most common one is magnesium iron alloy and salt. When water is activated it produces magnesium hydroxide and plenty of heat. Less common mixtures include sodium hydroxide and aluminum, magnesium metal and sodium bisulfate, aluminum and calcium hydroxide, and calcium oxide alone with water.
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My original goal was to make sodium nitrite. Sodium nitrite sets itself apart from the more common sodium nitrate by having one less oxygen atom, which makes it quite unstable under various conditions. This particular challenge intrigued me, and I thought I'd give it a try, even though I knew it's notoriously tricky for amateur chemists like me to produce.
I wanted to develop a low-temperature method, which involved several chemical reactions. I began by crafting nitrosylsulfuric acid from fuming nitric acid and sulfur dioxide.
Having successfully created nitrosylsulfuric acid, I moved on to the next stage: generating isopropyl nitrite. The idea was to eventually use this compound to produce sodium nitrite. The formation of isopropyl nitrite was quite intricate and required careful temperature control to keep the reagents and products stable.
I attempted to break down isopropyl nitrite into sodium nitrite using sodium hydroxide and methanol but this failed. I ended up with the decomposition of isopropyl nitrite instead.
But at least i found a way to make isopropyl nitrite without starting with nitrites.
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All reagents are mixed long with 40mL of water and 60g of potassium hydroxide. The can is placed in a furnace and heated to 400 degrees Celsius for several hours. This step involves the oxidation of manganese dioxide to potassium manganate by potassium chlorate, with potassium hydroxide providing essential potassium ions and alkaline conditions.
Once cooled and soaked in water, the solid chunks of potassium manganate are retrieved. To convert potassium manganate into potassium permanganate, chlorine gas is used. A chlorine generator comprising 45g of trichloroisocyanuric acid in 100mL water and 75mL of 30% hydrochloric acid is employed to produce chlorine gas, which is then introduced into the potassium manganate flask. The reaction results in potassium permanganate with potassium chloride as a byproduct.
Once the reaction is complete, the mixture is vacuum-filtered and then chilled to separate potassium permanganate from potassium chloride and hypochlorite. The potassium permanganate crystals are beautiful black needles.
The final yield is approximately 30.7g or 39%, adjusted to 52% considering the purity of the manganese dioxide used. Both crystallizations of potassium permanganate are found to be 99% pure with a 1% margin of error, confirmed through titration.
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I wanted recreate the test tube thunderstorm on a larger scale, adding sound for a more immersive experience. The setup involved using a glass funnel to carefully pour sulfuric acid into ethanol and form a layer of it in the bottom. Sprinkling potassium permanganate into the mix led to the formation of manganese heptoxide that reacted with ethanol and produced display of small explosions, accompanied by popping sounds and flashes of light.
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I wanted recreate the test tube thunderstorm on a larger scale, adding sound for a more immersive experience. The setup involved using a glass funnel to carefully pour sulfuric acid into ethanol and form a layer of it in the bottom. Sprinkling potassium permanganate into the mix led to the formation of manganese heptoxide that reacted with ethanol and produced display of small explosions, accompanied by popping sounds and flashes of light.
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Method 1: Burning Sulfur
The most cost-effective approach involves burning sulfur. Elemental sulfur, often used in gardening and pest control, is readily available. By burning it and capturing the resulting sulfur dioxide, we can utilize it for various reactions. A gas capture setup is essential, comprising a metal funnel over the burning sulfur, connected to a coil of copper tubing to cool the gas, and finally linked to a reaction flask using plastic tubing. Vacuum assistance is used to pull the gas into the apparatus, eliminating the need for a sealed combustion chamber.
Link to aspirator vacuum pump: youtu.be/tYLlkTDstmo
Method 2: Sulfuric Acid Decomposition
This method involves adding elemental sulfur to concentrated sulfuric acid within a sealed distillation setup. The sulfuric acid decomposes the sulfur to produce sulfur dioxide and water. While this approach yields relatively pure sulfur dioxide, it is slow and inefficient for amateur chemists. Moreover, the risk of dealing with boiling hot sulfuric acid makes it impractical for most.
Method 3: Sodium Metabisulfite Acidification
The most convenient yet costly method involves sodium metabisulfite and hydrochloric acid. A generator is set up with water, sodium metabisulfite, and hydrochloric acid. Upon opening a valve, the hydrochloric acid reacts with the sodium metabisulfite to instantly produce sulfur dioxide gas. This method offers convenience, immediate gas production, and purity, making it preferable for many applications. Sodium metabisulfite, found online and used in food preservation, is readily available for purchase.
In summary, these three methods provide options for generating sulfur dioxide gas, each with its advantages and drawbacks. The choice of method depends on factors like cost, convenience, purity, and safety considerations for specific applications.
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First i tried reacting manganese hydroxide, potassium chlorate and potassium hydroxide by mixing them together and heating to 300 celsius. I got green stuff that i think was potassium manganate so i oxidized it further to permanganate using chlorine gas. It turned the proper purple color but when i crystallized it the result was crystals of potassium chlorate with a little permanganate mixed in.
So that was failure and i repeated the experiment again at 400 celsius thinking i just needed more heat. But it still failed and produced only small quantites of permanganate.
So i thought maybe using manganese hydroxide was wrong. I repeated the experiment but using manganese dioxide this time. I produced a much more intense color of green manganate and purple permanganate and when i crystalized it i produced the proper black crystals of potassium permanganate. To make certain it was correct, i titrated using sodium oxalate and confirmed that i had a redox active substance that assayed to 99% purity. The yield was 15.4g or about 19%.
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To do this we boil down sodium hypochlorite to convert it into sodium chloride and sodium chlorate. While that's happening, in a separate container we dissolve an excess of potassium chloride in water to create a saturated solution. Continue boiling the bleach until sodium chloride crystals begin to form. Note the volume and boil off half of it.Sodium chlorate has higher solubility than sodium chloride, so boiling removes more sodium chloride, improving the yield. Stop heating and let the solution cool to room temperature. Filter out the sodium chloride crystals to retain the filtrate containing sodium chlorate and sodium chloride. Mix the filtrate with an equal volume of the saturated potassium chlorate solution to produce potassium chlorate, which precipitates out. Filter and collect the solid potassium chlorate.
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"Hot Ice" is Sodium Acetate trihydrate. It has a melting point of 58 celsius but can be easily super cooled well below that and still remain liquid. If initiated by solid crystals of sodium acetate it will rapidly crystalize in bulk.
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Hydrogen peroxide is titrated using potassium permanganate solution that was standardized with sodium oxalate. The titration is performed in a solution of sodium bisulfate to provide the acidic protons needed to run the reaction. Sodium oxalate is titrated with the potassium permanganate at 70 Celsius until a lingering pink or brown color is observed. The amount titrated is used to determine the actual concentration of the potassium permanganate.
Once the concentration is known, hydrogen peroxide is titrated with potassium permanganate until a lingering pink color is observed. Using the known concentration of permanganate the concentration of the hydrogen peroxide can be determined.
Related videos:
Making Sodium Oxalate: youtu.be/227KdtAK1yU
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The reaction is pretty simple. 120g of oxalic acid is dissolved in 300mL of boiling water and mixed with 80g of sodium hydroxide dissolved in 200mL of water. The sodium oxalate precipitates out and is allowed to cool. It is filtered and dried.
Sodium oxalate will be used in an upcoming video to standardize potassium permanganate solution that will in turn be used to titrate hydrogen peroxide.
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This particular unit was very graciously gifted by GWSI labs: gwsilabs.com
The vacuum is provided by powerful aspirator vacuum pump and the concept is explored in our own video on an amateur version of the same system: youtube.com/watch?v=tYLlkTDstmo
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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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