First, a postscript from the previous blog entry, where I attempted to clean perc with Sodium Bisulfite, a reducing agent... following some suggestions from Tentacles and others, I proceeded a bit more methodically and was rewarded with success - perc that tests as clean as my commercial stuff! It simply required an acidic environment to liberate the SO3 gas, which dissolved immediately into solution, and reduced the stray chlorate. Future cleanups will use potassium metabisulfite so as to avo
Esters often have a fruity smell and are used in flavoring and perfume. Fischer esterification a type of esterification and the process of forming an ester by refluxing a carboxylic acid and an alcohol in the presence of an acid catalyst. Carboxylic acids are organic acids characterized by the presence of a carboxyl group. Carboxylic acids include formic acid, aceitc acid, benzoic acid, butyric acid, salicylic acid and anthranilic acid. An alcohol is any organic compound in which a hydroxyl grou
All of the work in the last few months has gone into the hopeful production of pyrotechnic grade potassium perchlorate. It is not difficult to make perchlorate... contaminated with chlorate and perhaps other unwanted hitchhikers. It is apparently difficult to make it pure. In a previous blog, I mentioned how well n-phenylanthranilic acid and sulfuric acid work in tandem to reveal chlorate contamination down to very low levels. I finally got to put these chemicals to use, and the results, as
Copper benzoate is used in pyrotechnics to create a blue flame. This is desirable because the blue spectrum is often difficult to achieve and a good blue star is the mark of an accomplished pyro. The formula for copper benzoate blue is 82/18 ammonium perchlorate/copper benzoate. Overview of synthesis: Step 1: synthesis of benzoic acid via hydrolysis of sodium benzoate Step 2: synthesis of copper carbonate Step 3: synthesis of copper benzoate Step 1: synthesis of benzoic acid via hydroly
OK this is my first blog post. I plan on posting a variety of entries on how to synthesize various compounds that have interesting chemical properties or have uses in pyrotechnics. However to carry out these procedures it is necessary to have a basic knowledge of chemistry and lab safety. Most I'm sure have forgotten their high schools chemistry courses unless they are currently enrolled so this will be a basic review of most of the information need to preform these yourself or make your own com
This is going to be a fairly brief blog entry. I still have not tried either of the recently plated LD (Lead Dioxide) anodes to create perchlorate, but I hope to soon. I'd like to make a few more while the setup is in place, and vary some of the parameters a bit. I've always been a fan of microscopy, and decided to take a look at the better of the two anodes under a stereo microscope. To take pictures, I have two options - I can set up a camera in one of the eyepieces, and use a small noteb
So I'm really pissed, so this is going to be pretty short. While playing with the pictures, or before, during, and after I ended up deleting about half of them in a second with out recovery. I had pictures of the motor, the nice nozzle, and the fusing technique, and a side-by-side of 3 types of Ti. Mainly, the motor blew. Guess slightly slowed whistle is ok but not goex bp. Instant boom. Blew burning chunks of Ti all over the place. In the process of stopping out some fires, I found some
Thanks to some inspiration from Rosco Bodine at SMDB, among others, I have successfully hacked a $10 crock pot and turned it into a precision heating bath capable of holding +/- 1 degree C. Background: I have been using expensive polypropylene tanks to do the bulk of the work, and an immersion heater provides the heat. The immersion heater is an industrial cartridge heater encased in copper pipe, soldered shut at the business end. It works... but the Cu is not always compatible with the bat
So for the life of me I can't figure out what happened to my camera over the weekend. Its been misplaced somewhere. So until I find it I'm not moving any farther on this project. Though the only thing left to do is light it . The pressing went very well. The Ti actually release easier that clay does. Looks like a shiny gray nozzle. The Ti seems to be about 4-5 times more volumetric compared to clay when it comes to amount put in for a given amount of nozzle. Were I would use about 2-2
I am always experimenting with miscellaneous things, testing new ideas, and just overall doing random things that are never documented, recorded in any way, or sometimes not pictured or video taped at all. The results are usually stored in my head for further use. After being inspired after looking through Swedes work, I decided I would make me up a random experiments "blog". I suppose I can use this as a type of documenting what I've done or will be doing. I really hate the word "blog". I
It has been a long road, but I now have two anodes plated... one of them looking fairly sad, while the other looks excellent. The weather has NOT cooperated, and in addition to the physical discomfort (cold!), there are process issues as well. Jugs of distilled water are ice cold, and the hot bath (60 to 70 degrees C) must really struggle to maintain heat. Evaporation from the bath is at a ferocious rate. Anyway, I am getting ahead of myself. I've spent probably a month preparing for this
I would have imagined long ago that I would have made a lead dioxide plating attempt by now, but the more I read, the more useful information that I am able to gather... and the more reagents and hardware I seem to require. The print resources and other descriptions are rarely simple "home chemist" solutions. Usually, they are patents, and the patent office is not going to award a new patent to a scientist who plates a tiny MMO anode in a 1 liter beaker - they are going for the biggest, best,
VERSION III of "Lead Dioxide for Dummies!" Fellows, this is the LAST update of this document at this blog, but the document itself will see continued editing and work as the research progresses, so feel free to download it in a few weeks (months? perhaps) when it is complete. Here, the document ends rather abruptly at the pre-plating stage. It will eventually include an actual plating procedure, but that will be a new blog entry, full of photos and hopefully quite interesting. I will
With the huge harvest from T-Cell Junior (over 4 kg dry potassium chlorate) I now have about 15 pounds of this oxidizer, and I am ready to move on to the Lead dioxide experiments that really got me interested in the (per)chlorate process in the first place. There is a particular U.S. patent (4038170) that goes into tremendous detail on plating this substance, which is an ideal material for the electrochemical oxidation of chlorate to perchlorate, with one glaring problem... it doesn't stick wor
This is going to be the LAST "Harvest" blog I do, because it is getting repetitious. This one is worth detailing a bit because it has gone up to a scale where new and different techniques are required to successfully gather and clean the chlorate crop. It will also show portions of the T-Cell that succeeded, and failed, spectacularly. Subsequent blog entries will deal more with specifics, and with perchlorate conversion. I've got enough KClO3 to feed a perchlorate cell for a long time! Fro
The last three days have been very, very busy for me with regards to this project. I had hoped to have the system running Monday. Instead, it was Wednesday before I finally had everything put together, and ready to plug in. The odd thing is this - I don't have any pictures of the entire system once it was running! Just individual pictures, snippets here and there. The lead-up to this was pretty lengthy, work-intensive, and frankly, expensive. One of the reasons I waited was the delivery
I've finally got some days off, and on Monday, 3 Nov 2008, I'm going to launch this monster! With the end in sight, I've started final plumbing, anode work, and what is turning into an amazing amount of pneumatic tubing for agitation AND venting. I've got two sealed containers... both of them need to be vented, and both of them need to be agitated, or stirred, for proper function. Thanks to TheSidewinder, I can now pretty much flood this blog with photos! Photos are always more interestin
This is going to be a boring blog entry... the main purpose is to show that yes, the project is still underway, and progress is being made. The scope and complexity of this project has really grown. I'm looking at a potential rat's nest of tubes, wires, cables, etc, many of which, if they leak, could be disastrous. I think of myself as an organized guy. My wife would call me obsessed with order, and she's probably right. My chemicals are incredibly tidy, labeled with a Dymo "Letra-tag", an
It's been too long since my last blog. Most of the stuff I've been doing hasn't been worthy of note. Even worse, I couldn't find my camera! I've been using a Sony CD Mavica for years, and it has a great lense that does good macro work. Scouring the house for days, I was totally frustrated. Then, for some odd reason, I entered my teenage son's room, despite the mess. Young APC'ers, enlighten me, why does a teen not mind living in filth? It baffles me. How can your soul find peace when sur
Before this thing can get wet, there are a lot of fiddly things to take care of, one of the primary being a secure, well-sealed anode. In a previous blog, I mentioned how chemically resistant hardened "Sculpey" type clays are to the electrolyte in a (per)chlorate cell. These clays come in a variety of shades, brand names, firmness, etc. When I first thought about this, I bought three or four small samples from a local art and craft store. Of the samples, Fimo soft polymer clay was the easies
If you haven't been reading this blog, you may want to go back a few days to put it all into context. The entries are coming fast and furious! I've had a few days off from work, so I was able to put some focused effort into this beast. The placement of the electrodes really had me stymied. The cathode is necessarily massive... two 25mm wide titanium strips had to enter a 4" cylinder, AND it had to be air and water-tight. Ditto for the anode, although its shank was much smaller. In additio
I knew the electrodes would be a PITA and I have been putting the task off a bit. Today I decided to apply a bit of effort and get this critical task done. One think I learned from previous runs is that pure titanium is a crappy conductor. It works, but not as good as copper, and tends to heat quite a bit if the amperage is high. The typical titanium cathode from suppliers like Nothstar has a 1/2" X 1/16" shank, and above 20 amps, will heat badly; enough to boil water. I decided to try a
As usual, I underestimated the time and effort such a new system would entail. The good news - it is coming along very well, and I do enjoy this sort of hands-on work, so rather than being a chore, it is enjoyable. While the T-Cell is underway, I decided to run a last chlorate batch in my old acrylic tower cell. Three distinct purposes: Acquire another kilo of stock Take detailed notes on voltage, time, and chloride ion concentration Test my roll of Tygon tubing for chemical compatibilit
