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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