LabLulz: a DIY melting point apparatus

If you’ve ever taken an organic chemistry lab class, you’ve probably done a melting point determination. That’s when you take a small sample of a solid, heat it up, and make note of the temperature at which it melts. This can be used to identify an unknown, but it is often used to assay purity. This is because impurities tend to make solids melt over a range of temperatures rather than at a single point, and because they tend to lower the melting point overall. There are fancy instruments you can buy which will measure melting points, but they’re so simple that I decided to make my own.

One way to do it is to use a Thiele tube, but I didn’t have one of those lying around. So I reached for my volumetric flask, filled it with mineral oil, and set it on a hot plate. Then, I put a tiny bit of the chemical vanillin into a capillary tube; this is my sample to test. I rubber-banded the capillary tube to a thermometer, such that the sample was next to the bulb. I set up a stand and clamped the thermometer in place, suspended in the mineral oil.

This would have worked, except that the samples used are typically so small that they are difficult to see with the naked eye. So I grabbed my USB microscope and clamped it in place, focused on the sample.

With my apparatus assembled, I turned up the heat and sat back to watch. Sure enough, between 80 and 82 degrees C. My copy of the Merck Index actually gives two melting point ranges for this compound, 80-81 and 81-83 degrees, which is a little confusing but seems to confirm that my melting point apparatus works as expected. Sweet!

LabLulz: this microscope is the bee’s knees!

Figure A: The knee of a bee

I recently bought a 80-800x USB microscope. It has really good quality for less than $40, and I’ve been using it to get up close and personal with crystals, dead bugs, and gross parts of my anatomy. Feast your eyes!

A wasp, with a bizarre, insectile tonguemouththing. Proboscis. Weird.

One of my moles. Maybe it’s time I get it looked at, hm?

I wasn’t too thrilled to find out that I had warts, but they grow on you.

Iridescence in a bead of thermite residue.

Copper sulfate blocks

Feathers of copper acetate

Copper acetate closeup

I hope to get some polarizing filters and videotape the growth of chiral crystals, like sugar or vitamin C. Stay tuned…

LabLulz: densitometry of hydrogen purr-oxide

Today in LabLulz, I’m going to walk through a recent preparation I did in my chemistry lab: increasing and measuring the concentration of hydrogen peroxide.

WARNING: This procedure involves heat and the end product is a powerful oxidizer. Don’t get burned and don’t get it on yourself – wear gloves, splash-resistant goggles, and an apron. I had a spill of ~15%, all over everything, including myself. It was okay, but only because I followed safety protocols. I didn’t have the apron though, and I had to get pantsless.

Hydrogen peroxide is an interesting substance; it’s formula is H2O2, meaning that it is composed of two hydrogen atoms bonded to two oxygen atoms.

Figure 1. Behold, the hydrogen peroxide molecule!

It is a powerful oxidizer, decaying into water and free oxygen. This is because the bond between the two oxygen atoms, called the peroxide bond, is unstable. Some substances which contain the peroxide bond are even explosive, like triacetonetriperoxide. Because it’s an explosive precursor, and somewhat dangerous on its own, concentrated hydrogen peroxide can be difficult to come by. The weak 3% solution found in drugstores is all that is available to DIYers, hobbyists, and other scientists outside of the mainstream chemical supply chain.

Fortunately, it is relatively trivial to increase the concentration from 3% to around 30%. There are several tutorials on the subject at YouTube (TheChemLife; zhmapper, nerdalert226) so I’m going to focus on measuring the concentration of the end product, a procedure which the videos tend to treat very qualitatively. I hope this tutorial will be informative and useful, even outside of punklabs; the process is easily generalized and density is important in many fields, including medicine and winemaking.

The concentrating procedure is pretty simple: pour about 500 mL of the 3% solution into a beaker and heat it, forcing the excess water to evaporate until there is a tenth as much liquid left (peroxide boils at 150 C, compared to 100 C for water.) There are only a couple of tricky points: the liquid must NOT boil, only steam – if it starts boiling, the peroxide will decay. Bits of dust and dirt will also cause disintegration, so the equipment must be kept very clean and free from scratches.

Okay, so after a few hours, I have about 50 mL of liquid. I drop a bit into a solution of corn starch and potassium iodide, and the mixture turns black, a positive test for oxidizers. I add a squirt to some sulfuric acid and copper wire, and the metal wire begins bubbling and the solution begins to turn blue with copper sulfate*. This reaction is faster and more vigorous than when I try it with the 3% solution, so I’ve clearly succeeded in increasing the concentration, but to what level? To answer that question, I’m going to measure the density of the solution.

dont forget the crystals

Magnesium sulfate crystals, clingin’ to a petri dish. Chillin’.

Another quick lab snap. These are some nice crystals I grew. I was washing an earlier, less photogenic crystal garden with alcohol, and catching the runoff in a petri dish. I let it evaporate and was greeted with this happy little accident! The crystals are magnesium sulfate, available as Epsom salt at most pharmacies.

haxor hijinx: a DIY hotplate

I have, once again, found myself at the helm of a DIY lab, this one with a chemical wetlab focus. I’m sure this will provide lots of material in the future; right now, I want to share a protip I came up with the other night. I have been using soda can alcohol stoves for heat, but this isn’t always appropriate. You can’t heat flammable mixtures, and they leave soot on my glassware. But I don’t have a hotplate yet! What’s a gutterpunk labnerd to do?

Don’t forget the boiling chips!

It’s won’t spin a stir bar, but a clothes iron will do fine as a hotplate! You can see that I’ve secured this one to the lab bench with wood and a clamp for extra stability.