Lab Notes - Failure in Making Sodium Nitrite
In this video i synthesize nitrosylsulfuric acid and isopropyl nitrite, and i tried to make sodium nitrite but i failed.
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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Make Potassium Permanganate
In this video, we explore the process of making potassium permanganate, a valuable oxidant with a striking purple color. Starting with 43g of manganese dioxide, often obtained from greensand filter media, and 25g of potassium chlorate, the chemicals are thoroughly mixed. A can made of iron is chosen as the reaction vessel due to its resistance to the highly corrosive mixture.
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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3 Ways to Make Sulfur Dioxide Gas
In this video, I'll be demonstrating three methods to produce sulfur dioxide gas. Sulfur dioxide, while undesirable on its own due to its toxicity and environmental impact, serves as a crucial precursor for various chemical processes, including the production of sulfuric acid. These methods have been showcased in previous videos, but I've compiled them here for easy reference.
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: https://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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Lab Equipment Repair: Broken Stirrer Encoder Disc in Hotplate Stirrer
In this video i repair the broken stirrer in my hotplate stirrer. Turns out the encoder disk snapped so to "fix" it i just glued it back in place.
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Lab notes - Making Potassium Permanganate
My lab notes of making potassium permanganate.
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 of permanganate.
So i thought maybe using manganese hydroxide was wrong. So 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 hate a redox active substance that assayed to 99% purity. The yield was 15.4g or about 19%.
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Make Potassium Chlorate from Bleach
In this video we show how to make potassium chlorate from bleach.
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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Hand in Hot Ice #shorts
I stick my hand into Hot Ice.
"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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Find the Concentration of Hydrogen Peroxide by Titration
In this video we find the concentration of hydrogen peroxide by titration using domestically available chemicals and equipment.
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 linger 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: https://youtu.be/227KdtAK1yU
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Make Sodium Oxalate - Primary Standard for Analytical Chemistry
In this video we make a sodium oxalate, a simple primary standard for the standardization of potassium permanganate titrant.
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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Lab Equipment: Rotary Evaporator or "Rotovap"
In this video we look at the Rotary Evaporator or "Rotovap" for quickly evaporating solvents from products under gentle heating and vacuum. These are used in professional labs for their high speed. But due to their high expense, amateurs almost never encounter them.
This particular unit was very graciously gifted by GWSI labs: https://www.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: https://www.youtube.com/watch?v=tYLlkTDstmo
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How Does Aqua Regia Dissolve Gold and Platinum?
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Clips from old videos featured in this one:
Gold Chemical Resistance
https://youtu.be/ng6DGwiKWag
Platinum Chemical Resistance
https://youtu.be/fro-L5gSyh4
Platinum bar dissolving in Aqua Regia
https://youtu.be/APxL87X92t4
Dissolve Platinum with chlorine gas
https://youtu.be/JFNtP2N2Eho
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Make Sodium Hydroxide by Electrolysis with a Nafion Membrane Cell
In this video we use a nafion membrane cell to make sodium hydroxide by electrolysis of sodium bicarbonate and separating and isolating the ions.
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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183
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Make a Nafion Divided Membrane Cell for Electrolysis
In this video we make a two compartment electrolysis cell divided with a Nafion membrane.
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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Lab Notes: Making Copper Sulfate and Electrobonding Wires
In this video we make copper sulfate in large quantities and also repair the sensors in my hotplate stirrer using electrochemical bonding, an alternative to soldering.
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Chemical Resistance of Palladium
In this video we explore the chemical resistance of palladium metal.
Related videos:
Ruthenium is invulnerable to aqua regia: https://youtu.be/H7Ng4sOVkns
Chemical resistance of platinum: https://youtu.be/fro-L5gSyh4
Dissolving platinum in aqua regia: https://youtu.be/APxL87X92t4
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Efficiently Recover Nitric Acid and Copper Metal From Copper Nitrate Wastes
In this video we Efficiently Recover Nitric Acid and Copper Metal From Copper Nitrate Wastes by reacting copper nitrate wastes with sulfuric acid to generate nitric acid and copper sulfate. Then we electrolyze the copper sulfate to recovery copper metal and sulfuric acid.
Related videos:
Production of nitric acid by thermal decomposition of copper nitrate: https://youtu.be/hmB5x0LYfSE
Purification and concentration of nitric acid: https://youtu.be/88gbfCnrV8o
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Nitric Acid Concentration and Purification (Azeotropic and Fuming)
In this video we purify and concentrate dilute nitric acid using a combination of fractional distillation and drying agents to produce azeotropic nitric acid and fuming nitric acid.
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DANGEROUS reaction of ACID and GLOVES
In this video we react fuming nitric acid with nitrile gloves and show that rather than being safe, nitrile gloves actually make fuming nitric acid even more dangerous.
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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Make Nitric Acid by Thermal Decomposition of Copper Nitrate
In this video we the thermal decomposition of copper to directly produce nitric acid without using any other acid.
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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Lab Notes - August 31st - Nitric Acid from Calcium Nitrate and My Hotplate Failed, Again.
Some lab notes for the month of august 2020
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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Make Nitric Acid from Sodium Bisulfate and Sodium Nitrate
In this video we Make Nitric Acid from Sodium Bisulfate and Sodium Nitrate.
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: https://youtu.be/l2AkVYxDSKc
Old video on making nitric acid (which sucks): https://youtu.be/2yE7v4wkuZU
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How to Regenerate Deionization Resin for Use in Reverse Osmosis Deionization Systems
In this video we show how to Regenerate Mixed-Bed Deionization Resin for Use in Reverse Osmosis Deionization systems.
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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Amateur Lab Equipment: Reverse Osmosis Deionization Systems for Purifying Water
In this video we discuss the components, usage, and science behind a Reverse Osmosis Deionization unit for purifying water.
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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Is Ruthenium Jewelry Dangerous?
In this video we explore whether ruthenium jewelry is safe by seeing how it reacts with the common household chemical bleach.
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: https://youtu.be/H7Ng4sOVkns
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Make a Chemical Garden From Cat Litter, Drain Opener, and Root Killer
In this video we're going to use silica in crystal cat litter, sodium hydroxide in drain opener, and copper sulfate in root killer to make the famous chemical garden experiment.
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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