An aluminium frame is visible, supporting several connected pieces of chemistry equipment. At the left, there is a tube containing a clear solution, with a tube leading to a clear tube heated by a gas flame, with another tube leading to a clear bottle, which has a tube leading to a bubbling orange solution.

A Miniature Ostwald Reactor To Make Nitric Acid

Modern fertilizer manufacturing uses the Haber-Bosch and Ostwald processes to fix aerial nitrogen as ammonia, then oxidize the ammonia to nitric acid. Having already created a Haber-Bosch reactor for ammonia production, [Markus Bindhammer] took the obvious next step and created an Ostwald reactor to make nitric acid.

[Markus]’s first step was to build a sturdy frame for his apparatus, since most inexpensive lab stands are light and tip over easily – not a good trait in the best of times, but particularly undesirable when working with nitrogen dioxide and nitric acid. Instead, [Markus] built a frame out of aluminium extrusion, T-nuts, threaded rods, pipe clamps, and a few cut pieces of aluminium.

Once the frame was built, [Markus] mounted a section of quartz glass tubing above a gas burner intended for camping, and connected the output of the quartz tube to a gas washing bottle. The high-temperature resistant quartz tube held a mixture of alumina and platinum wool (as we’ve seen him use before), which acted as a catalyst for the oxidation of ammonia. The input to the tube was connected to a container of ammonia solution, and the output of the gas washing bottle fed into a solution of universal pH indicator. A vacuum ejector pulled a mixture of air and ammonia vapors through the whole system, and a copper wool flashback arrestor kept that mixture from having explosive side reactions.

After [Markus] started up the ejector and lit the burner, it still took a few hours of experimentation to get the conditions right. The issue seems to be that even with catalysis, ammonia won’t oxidize to nitrogen oxides at too low a temperature, and nitrogen oxides break down to nitrogen and oxygen at too high a temperature. Eventually, though, he managed to get the flow rate right and was rewarded with the tell-tale brown fumes of nitrogen dioxide in the gas washing bottle. The universal indicator also turned red, further confirming that he had made nitric acid.

Thanks to the platinum catalyst, this reactor does have the advantage of not relying on high voltages to make nitric acid. Of course, you’ll still need get ammonia somehow.

Fixing A Fatal Genetic Defect In Babies With A Bit Of Genetic Modification

Genetic defects are exceedingly common, which is not surprising considering just how many cells make up our bodies, including our reproductive cells. While most of these defects have no or only minor effects, some range from serious to fatal. One of these defects is in the CPS1 gene, with those affected facing a shortened lifespan along with intensive treatments and a liver transplant as the only real solution. This may now be changing, after the first successful genetic treatment of an infant with CPS1 deficiency.

Carbamoyl phosphate synthetase I (CPS1) is an enzyme that is crucial for breaking down the ammonia that is formed when proteins are broken down. If the body doesn’t produce enough of this enzyme in the liver, ammonia will accumulate in the blood, eventually reaching levels where it will affect primarily the nervous system. As an autosomal recessive metabolic disorder it requires both parents to be carriers, with the severity depending on the exact mutation.

In the case of the affected infant, KJ Muldoon, the CPS1 deficiency was severe with only a low-protein diet and ammonia-lowering (nitrogen scavenging) medication keeping the child alive while a search for a donor liver had begun. It is in this context that in a few months time a CRISPR-Cas9 therapy was developed that so far appears to fixing the faulty genes in the liver cells.

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Benchtop Haber-Bosch Makes Ammonia At Home

Humans weren’t the first organisms on this planet to figure out how to turn the abundance of nitrogen in the atmosphere into a chemically useful form; that honor goes to some microbes that learned how to make the most of the primordial soup they called home. But to our credit, once [Messrs. Haber and Bosch] figured out how to make ammonia from thin air, we really went gangbusters on it, to the tune of 8 million tons per year of the stuff.

While it’s not likely that [benchtop take on the Haber-Bosch process demonstrated by [Marb’s lab] will turn out more than the barest fraction of that, it’s still pretty cool to see the ammonia-making process executed in such an up close and personal way. The industrial version of Haber-Bosch uses heat, pressure, and catalysts to overcome the objections of diatomic  nitrogen to splitting apart and forming NH3; [Marb]’s version does much the same, albeit at tamer pressures.

[Marb]’s process starts with hydrogen made by dripping sulfuric acid onto zinc strips and drying it through a bed of silica gel. The dried hydrogen then makes its way into a quartz glass reaction tube, which is heated by a modified camp stove. Directly above the flame is a ceramic boat filled with catalyst, which is a mixture of aluminum oxide and iron powder; does that sound like the recipe for thermite to anyone else?

A vial of Berthelot’s reagent, which [Marb] used in his recent blood ammonia assay, indicates when ammonia is produced. To start a run, [Marb] first purges the apparatus with nitrogen, to prevent any hydrogen-related catastrophes. After starting the hydrogen generator and flaring off the excess, he heats up the catalyst bed and starts pushing pure nitrogen through the chamber. In short order the Berthelot reagent starts turning dark blue, indicating the production of ammonia.

It’s a great demonstration of the process, but what we like about it is the fantastic tips about building lab apparatus on the cheap. Particularly the idea of using hardware store pipe clamps to secure glassware; the mold-it-yourself silicone stoppers were cool too.

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Integrated Micro Lab Keeps Track Of Ammonia In The Blood

We’ve all got our health-related crosses to bear, and even if you’re currently healthy, it’s only a matter of time before entropy catches up to you. For [Markus Bindhammer], it caught up to him in a big way: liver disease, specifically cirrhosis. The disease has a lot of consequences, none of which are pleasant, like abnormally high ammonia concentration in the blood. So naturally, [Markus] built an ammonia analyzer to monitor his blood.

Measuring the amount of ammonia in blood isn’t as straightforward as you think. Yes, there are a few cheap MEMS-based sensors, but they tend to be good only for qualitative measurements, and other solid-state sensors that are more quantitative tend to be pretty expensive since they’re mostly intended for industrial applications. [Marb]’s approach is based on the so-called Berthelot method, which uses a two-part reagent. In the presence of ammonia (or more precisely, ammonium ions), the reagent generates a dark blue-green species that absorbs light strongly at 660 nm. Measuring the absorbance at that wavelength gives an approximation of the ammonia concentration.

[Marb]’s implementation of this process uses a two-stage reactor. The first stage heats and stirs the sample in a glass tube using a simple cartridge heater from a 3D printer head and a stirrer made from a stepper motor with a magnetic arm. Heating the sample volatilizes any ammonia in it, which mixes with room air pumped into the chamber by a small compressor. The ammonia-laden air moves to the second chamber containing the Berthelot reagent, stirred by another stepper-powered stir plate. A glass frit diffuses the gas into the reagent, and a 660-nm laser and photodiode detect any color change. The video below shows the design and construction of the micro lab along with some test runs.

We wish [Markus] well in his journey, of course, especially since he’s been an active part of our community for years. His chemistry-related projects run the gamut from a homebrew gas chromatograph to chemical flip flops, with a lot more to boot.

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Fighting The Scourge Of “Screwdriver Mange”

We’ve all got our favorite hand tools, and while the selection criteria are usually pretty subjective, it usually boils down to a combination of looks and feel. In our opinion, the king of both these categories when it comes to screwdrivers is those clear, hard acetate plastic handles, which are a joy to use — at least until the plastic starts to degrade and exude a characteristically funky aroma.

But perhaps we can change that if these experiments on screwdriver “mange” hold up. That’s [357magdad]’s unappealing but accurate description of the chemical changes that eventually occur in the strong, hard, crystal-clear handles of your favorite screwdrivers. The polymer used for these handles is cellulose acetate butyrate, or CAB, which is mostly the same cellulose acetate that replaced the more explode-y cellulose nitrate in things like pool balls and movie film, except with some of the acetate groups replaced with a little butyric acid. The polymer is fine at first, but add a little UV light and over time the outer layer of CAB decomposes into a white flaky cellulose residue while the butyric acid volatilizes, creating the characteristic odor of vomitus. Lovely.

In the video below, [357magdad] takes a look at different concoctions that all allegedly cure the mange. TL, DW; it was a dunk in household ammonia that performed the best, well ahead of other common agents like vinegar and bleach. The ammonia — or more precisely, ammonium hydroxide — works very quickly on the cellulose residue, dissolving it readily and leaving the handle mange-free and looking nearly new after some light scrubbing. None of the other agents came close, although acetone did manage to clear up the mange a bit, at the cost of softening the underlying CAB in a process that’s probably similar to acetone smoothing ABS prints.

As for the funky smell, well, the results were less encouraging. Nothing really got rid of the pukey smell, even a roll in baking soda. We suspect there won’t be much for that, since humans can detect it down to 10 parts per million. Consider it the price to pay for a nice-looking screwdriver that feels so good in your hand. Continue reading “Fighting The Scourge Of “Screwdriver Mange””

How To Refrigerate With Urine

It’s often said that the best science experiments are the ones which do not require any special devices or ingredients, which makes the use of what naturally comes out of one’s body clearly one of the winners. It’s also the beginning of yet another [Hyperspace Pirate] chemistry video that’s both fascinating and unforgettable — this time introducing a considerable collection of urine, and the many uses of the urea in it, including its use for refrigeration.

The respective cooling effect of a variety of compounds in solution. (Credit: Hyperspace Pirate)
The respective cooling effect of a variety of compounds in solution. (Credit: Hyperspace Pirate)

As icky as this may sound, it doesn’t even rank in the top ten of quaint things people have historically done with urine, so extracting urea from it is rather benign. This is performed by adding sodium hydroxide to the starting component after heating, which creates gaseous ammonia (NH3) which was then condensed into its liquid (dissolved) form. In order to create the target compound – being ammonium nitrate – nitric acid (HNO3) had to be created first.

For this the older, but cheaper and easier Birkeland-Eyde process was used. This uses high-voltage electrical arcs to break down the nitrogen and oxygen in the air and cause the formation of nitric oxide (NO), that subsequently reacts with atmospheric oxygen to form nitrogen dioxide (NO2). Running the NO2 through water then creates the desired HNO3, which can be combined with the ammonia solution to create ammonium nitrate. The resulting solution was then evaporated into solid ammonium nitrate, to use it in an aluminium cooling cylinder, with freshly added water.

This is the simplest way to use the cooling effect of such solutions (pictured), but the benefit of ammonium nitrate over the original urea seems minimal. The low efficiency of this cooling approach means that the next use of urine will involve a much more efficient vapor-absorption cycle, which we’re sure everyone is squeezing their legs together for in anticipation.

We’ve been covering the refrigeration experiments [Hyperspace Pirate] has been conducting for some time now. If you’re into the science of making things cold check out how seashells can be turned into dry ice, or what goes into building a home cryocooler.

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Japan Wants To Decarbonize With The Help Of Ammonia

With climate change concerns front of mind, the world is desperate to get to net-zero carbon output as soon as possible. While direct electrification is becoming popular for regular passenger cars, it’s not yet practical for more energy-intensive applications like aircraft or intercontinental shipping. Thus, the hunt has been on for cleaner replacements for conventional fossil fuels.

Hydrogen is the most commonly cited, desirable for the fact that it burns very cleanly. Its only main combustion product is water, though its combustion can generate some nitrogen oxides when burned with air. However, hydrogen is yet to catch on en-masse, due largely to issues around transport, storage, and production.

This could all change, however, with the help of one garden-variety chemical: ammonia. Ammonia is now coming to the fore as an alternative solution. It’s often been cited as a potential way to store and transport hydrogen in an alternative chemical form, since its formula consists of one nitrogen atom and three hydrogen atoms.However, more recently, ammonia is being considered as a fuel in its own right.

Let’s take a look at how this common cleaning product could be part of a new energy revolution.

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