new adventures in cyanide [Archive] - The Explosives and Weapons Forum

Polverone

April 21st, 2002, 08:09 PM

BACKGROUND

This weekend I had just enough free time to do a little chemical experimentation. I chose to try preparing a cyanide or ferrocyanide salt, something that I've repeatedly attempted without success in the past. In the past, I've taken guidance from Kurt "can't be trusted with Armstrong's" Saxon. I tried preparing ferrocyanides by heating a mixture of an alkali carbonate, powdered charcoal, and iron filings for as long and hot as I could. Alas, I couldn't heat it as much or as long as the Poor Man's James Bond told me to, since I only had a gas burner, not a charcoal furnace. And every time my preparation failed utterly.

I also began to suspect the directions in general. For example, there's no nitrogen source in the PMJB prep, apart from the air. Actual 19th century methods used materials already containing nitrogen - like leather scraps, dried blood, and horn - not charcoal. Also, once you had prepared the ferrocyanide and were converting it to cyanide by heating with additional carbonate, the PMJB advised using an open topped steel container for this stage. Yet the Kirk-Othmer encyclopedia mentions that hot cyanides are quickly oxidized to cyanates in the presence of oxygen and iron! The actual 19th century methods used iron vessels but kept them sealed from air.

EXPERIMENTAL PROCEDURE

Anyway, after meeting with these failures in practice and having doubts about the theoretical worth of the PMJB prep, I struck out in a new direction. I decided I would try using blood meal instead of charcoal. Blood meal is a light sandlike powder of dried slaughterhouse blood, readily available as an organic fertilizer. It contains considerable nitrogen, carbon, and iron. I also decided I would try using sodium hydroxide instead of carbonate, since I would already have plenty of carbon from the blood meal and NaOH has a much lower melting point (and would thus mix better with the blood meal).

I melted about 70 grams of NaOH in a stainless steel dish over my gas burner. Once it had all fused I started spooning in blood meal (I didn't measure this). Each time I added the blood there was vigorous bubbling and frothing. After a while bright yellow flames would sharply crackle/bubble to the surface. I only added 5 or 6 spoonfuls of blood meal and then shut off the heat. I let the mass cool in the bottom of the dish and then smacked it out onto a sheet of paper, broke it up into a few chunks, and added it to about 300 ml of water.

RESULTS

I let the chunks sit in the water for a couple of minutes, periodically swirling it. The water was warming up so I guessed a considerable amount of NaOH had survived unchanged. As the blackened crusty outer portion of the lumps fell away I could see that they appeared to be a mottled light yellow color, much like the potassium ferrocyanide I have purchased (although not quite as intensely colored).

So, thought I, time to test for the presence of ferrocyanide. I added a bit of ferric ammonium sulfate, which gives the lovely prussian blue in the presence of ferrocyanide, and... was horribly disappointed. The ferric ammonium sulfate seemed to turn a bit of a brighter orange color. There was no blue at all.

I figured I would clean out the vessel I'd done this in by adding some sulfuric acid, since there was obviously no ferrocyanide lurking about to harm me. As I poured the acid in, something startling happened. The liquid bubbled violently, and as more acid went in, it suddenly turned the telltale color of prussian blue! I hastily backed away from the hot, bubbling mix. The lumps of material were still dissolving in the water and acid. I nervously approached the vessel and cautiously wafted the air from the top of the jar toward my nose and inhaled. I definitely caught the odor of HCN. I repeated this test several times, with breaks in between, to make sure my nose hadn't been fooled. There was no mistake; HCN was being evolved.

ANALYSIS
Why didn't I instantly detect the ferrrocyanide when I added ferric ammonium sulfate? My guess is that the excess NaOH abstracted the sulfate from the iron compound so that there was no iron (III) in solution to precipitate prussian blue. When enough sulfuric acid had been added to overcome the NaOH then there was again soluble iron (III) which did react as expected. This characteristic precipitate and the odor of HCN evolved from the mixture have convinced me beyond all doubt that I did prepare sodium ferrocyanide.

After just one test I can confidently say that this method of preparing ferrocyanides is a cut above the one given in the PMJB. It still uses readily available, inexpensive materials but proceeds far more rapidly and at lower temperatures. This is especially important to individuals who cannot run a charcoal furnace overnight.

FUTURE WORK

I want to try this method again when I next have free time (ha ha). I want to try using a hotplate instead of a gas burner, since I am sure that the molten hydroxide is at least partially converted to carbonate on contact with CO2 from the burner. I would also like to try adding blood meal until no further reaction occurs, so that I could be reasonably confident of having just sodium ferrocyanide and insoluble impurities, which could be removed by filtration. I would also like to try other hydroxides (such as KOH) to see if there is any substantial difference. And, of course, I would like to try converting some ferrocyanide(s) to cyanide(s), but that is most definitely a topic unto itself.

Rhadon

April 22nd, 2002, 07:39 AM

I wanted to use this method, too. But since I'm a low budget chemist <img border="0" title="" alt="[Wink]" src="wink.gif" /> and don't have a bunsen burner und thus cannot reach the temperature required, I thought of another method which is both easier and not expensive: You can convert prussian blue, which I suppose everyone can get, to KCN or NaCN by reacting it with NaOH or KOH in an aqueous solution (prussian blue:NaOH = 1:1 by weight) and heating it.

EDIT: The equation for the first reaction should be
Fe4[Fe(CN)6]3 + 12 KOH ==> 3 K4[Fe(CN)6] + 2 Fe2O3 + 6 H2O

[ April 22, 2002, 12:36 PM: Message edited by: Rhadon ]

mongo blongo

April 22nd, 2002, 12:45 PM

Quote "I repeated this test several times, with breaks in between, to make sure my nose hadn't been fooled."
You must be crazy! If I thought HCN was being evolved I would run away and not return for at least a few days!

Rhadon

April 22nd, 2002, 01:42 PM

Yes, Mongo's right. This test cannot be recommended, at least not for everyone: Not everybody is able to smell the odour of HCN. If you are one of these guys...

vulture

April 22nd, 2002, 01:48 PM

Only 40% of the population can smell HCN....
If you smell the lethal concentration has been achieved IIRC...

Reacting blood with potash or KOH also works, that's because of it containing a ferrocyanide.

Polverone

April 22nd, 2002, 02:58 PM

I don't think I was *crazy* per se. I looked up the ld-50 of HCN in humans, converted milligrams to moles, moles to milliliters, and was able to visually evaluate the rate of gas evolution (bubbling) to estimate how much I was likely to inhale relative to the lethal concentration. It's not as if I stuck my nose in the jar and sucked up a lungful. It's possible I could have received a lethal dose without smelling it had I done this indoors, being exposed over a long period, but I was outside on a breezy day.

Rhadon, that is interesting about converting prussian blue to cyanides. I will definitely have to try that. You don't need a bunsen burner to get the necessary temperatures for this method. NaOH will melt from hotplate heat. Wait - scratch that - lab hotplates aren't cheap. Rather, you could use a denatured alcohol burner, which is very inexpensive and will easily reach the temperatures you need to melt NaOH.
I know I have a simple qualitative test method for HCN around somewhere, and I really would prefer using it to my nose. But I don't have all of the necessary reagents on hand.

Rhadon

April 22nd, 2002, 03:27 PM

<blockquote>quote:<hr />You don't need a bunsen burner to get the necessary temperatures for this method. NaOH will melt from hotplate heat<hr /></blockquote>To which method do you refer? To yours or to mine? For my method you don't need much heat at all, evaporating the water out of the ferrocyanide solution will do it since K4[Fe(CN)6] decomposes already at temperatures above 50° C.

Rhadon

April 22nd, 2002, 04:09 PM

@Polverone: Can you tell me about your cyanide test?

I thought of a cyanide test myself. Here is an example [it isn't tested yet]:
I heat the substance that I suspect to be sodium cyanide with sulfur (NaCN + S --> NaSCN). The NaSCN is then added to a solution of an iron(III)-salt-compound (e.g. iron citrate or iron phosphate). If the substance really was NaCN, the color of the solution will change to red.

Polverone

April 22nd, 2002, 07:47 PM

Oh, the method I was thinking of for detecting cyanide was for detecting HCN, and was quite sensitive. I do not remember it off the top of my head but I will try to look it up again soon. I mentioned it because I realize that sniffing bubbling liquids is not the best method for detecting poisonous gases.

When I said the method did not require much heat I was referring to my own. Yours might indeed be better for a chemist who cannot use very much heat at all. But where I live I have never seen prussian blue for sale (I suppose I would have to go to an art store and get it as pigment?) while blood meal and NaOH are available in practically every grocery store/garden center.

It seems I did not read your first equation closely enough the first time. You are talking about preparing ferrocyanides from prussian blue, yes? When you say "For my method you don't need much heat at all, evaporating the water out of the ferrocyanide solution will do it since K4[Fe(CN)6] decomposes already at temperatures above 50° C." do you mean that you will get some KCN as the ferrocyanide decomposes? What are the decomposition products?

I am very interested in preparing cyanides, but I want A) high purity and B) no HCN used. I could easily make low purity cyanides by a variety of methods, or high purity cyanides by bubbling HCN through hydroxide solutions, but I do not like either of these methods. I need either a new method or some clever apparatus to safely obtain pure cyanides from my ferrocyanides.
Strictly speaking, being able to prepare sodium ferrocyanide didn't get me any closer to my cyanide goal since it is already easy to order ferrocyanides from photography and chemical suppliers. But it was satisfying to come up with a new method for making it from household items. I'm sure somebody's done this before, but I've never before seen any references or accounts of people preparing sodium ferrocyanide this way, just that frustrating method from the PMJB.

kingspaz

April 23rd, 2002, 05:57 PM

just a thought.
today in chemistry we learnt some stuff about polymers.
anyways, one of the polymers we looked at was polypropenenitrile (acrylic). it can also be looked as polyethene cyanide. containing the CN group.
we had to test for different plastics using flame tests. we where not however allowd to test acrylic because HCN would be released. i was just thinking maybe there could be a way to extract it by chemical means and collect it.

Rhadon

April 24th, 2002, 08:57 AM

<blockquote>quote:<hr />I suppose I would have to go to an art store and get it as pigment?) <hr /></blockquote>That's exactly the way I did it.

<blockquote>quote:<hr />When you say "For my method you don't need much heat at all, evaporating the water out of the ferrocyanide solution will do it since K4[Fe(CN)6] decomposes already at temperatures above 50° C." do you mean that you will get some KCN as the ferrocyanide decomposes? What are the decomposition products?<hr /></blockquote>The decomposition products are, as far as I know, KCN and iron carbide.

<blockquote>quote:<hr />I'm sure somebody's done this before, but I've never before seen any references or accounts of people preparing sodium ferrocyanide this way, just that frustrating method from the PMJB. <hr /></blockquote>I don't like PMJB so much... And I don't know anybody who used my method for making ferrocyanides except for myself :) I didn't read about it anywhere, but it must work that way. The reaction went exactly the way I 'predicted' it, thus I'm sure that my ideas were correct.

rikkitikkitavi

April 24th, 2002, 10:06 AM

hexamine (hexamethylentetramin, (CH2)6N4) ) decomposes above 200 C to ammonia and a resninous oil. Inreasing the temperature to 330 C
HCN, CH4, N2, H2 are the basically products.

At 800 C major decomposition product is HCN!

This is utilized in a patent(country germany ?) by Plischke and Zettl for producing HCN in 90 % yield from hexamine.

First vapourizing hexamine at 260 C then heating the vapours in a ceramic oven to 800-1200 C yielding HCN.

Unfortunately this is all I could dig out from my 40 cm pile of papers regarding chemicals... ,I can produce a reference to the patent but I be gone for R&R for a week from now.

/rickard

megalomania

April 24th, 2002, 02:42 PM

I do believe it is German patent 1076104 (DE1076104 at espacenet.com) and lets see if this link is valid... <a href="http://l2.espacenet.com/espacenet/viewer?PN=DE1076104&CY=gb&LG=en&DB=EPD" target="_blank">DE 1076104</a>

Now then, while I am on the subject, does anyone know how to convert these foreign pdf files into OCR'd text so they can be pasted into a translater to decode their mystic contents? I have a few dozen patents in many different languages and I do not want to type them all by hand <img border="0" title="" alt="[Frown]" src="frown.gif" />

[ April 24, 2002, 01:45 PM: Message edited by: megalomania ]

Polverone

April 24th, 2002, 04:38 PM

The text that follows was converted from the referenced German patent by

A) opening the PDF in Adobe Acrobat (not the free reader, the fullblown authoring package)
B) using the "export" menu to save all images in the PDF as TIFFs
C) opening the TIFF file in Finereader Pro, highlighting the body of the text, and OCRing it
D) copying the OCRed text into the demo web-translator at <a href="http://www.systransoft.com" target="_blank">www.systransoft.com</a>
E) copying the result here

I don't which of these mistakes are the fault of Finereader and which the fault of Systransoft. I would guess that some are definitely Finereader's (for example, it did not catch the very small subscript numbers) Anyway, here's the raw result:

The well-known reaction of splitting of simple amines is technically used only in the procedure for the production of prussic acid from molasses Dickschlempe after Reichar'dt and Bueb. A further technical utilization of the reaction of the 5 amine splitting failed because of the possibility of using amines which can be manufactured economically.
Other authors use among other things hexadecimal min for the production of blue-acid parasit 10 fight-average with yields of 15% HCN?N, related to assigned hexadecimal min nitrogen. In other patent specifications it is pointed out that by use of the chlorhydrate of Stickstoffbasen the yields at HCN en 15 can be improved.
To achieve against these specified and well-known statements found, dass it under observance of certain conditions is possible, from pure hexadecimal min one almost 100%ige conversion of the einge ao led hexadecimal min nitrogen to HCN?N. The reaction probably runs after the following principal equation:
Procedure for the production of prussic acid from Hexamethylentetramin
1200°C
4HCN+2CH,
25
by secondary reactions is reduced?die yield at H C N somewhat and developing methane with the dominant conditions more or less ther 30 mixes split.
The procedure can be operated in different manner.
1. Hexadecimal min is sublimated in a closed retort at temperatures between 160 and 270° C, preferably 35 with 260° C. Steams arrive into a superheater operated with 800 to 1200° C, in which the gap reaction takes place. The superheater is lined with ceramic material and can be structured after any of the well-known systems. 40 it is only necessary that for the achievement of a good yield steams are initiated directly into the zone of the high temperature. The gas is cooled under adherence to an optimal gas rate, which is dependent far away from the design of the superheater, 45 from the reaction zone, fast, separated ammonia from prussic acid in usual manner and supplied the remainder gas of the heating again. The reaction system is held under small negative pressure. 50
2. Hexadecimal min is supplied to a fission furnace consisting heated on 800 to 1200° C of ceramic material continuously by way of an air-lock. The developing reaction gases become by means of negative pressure
applicants:
VEB fermentation chemistry Dessau, Dessau, August Bebel August-Bebel-Str.QOa
Hans PUschke and walter Zettl, Dessau, were called as inventors
2
removed from the furnace and, as under l described, further regenerated.
3. Further found that it is possible, prussic acid from the components of the Hexamins, formaldehyde and ammonia to manufacture continuously without isolating the hexadecimal min only. The following procedure was prepared:
Formaldehyde steams, directly coming from the synthesis or won by evaporation of aqueous Formaldehydioesung as high a concentration as possible, are preheated on 250° C and likewise combined with ammonia in a heated reaction container, preheated on this temperature, after actually well-known way. The reaction container is in such a way trained that the two components are mixed intimately together by means of agitators or forced turbulence. The dosage from formaldehyde to ammonia takes place in the molar ratio 6:4 with a surplus of ammonia. The reaction temperature in the mixing vessel must amount to 230 ' to 270° C, so that the formed hexadecimal min leaves the reaction space in vaporous status and into the superheater or fission furnace, as under paragraph l described, thermally is split.
Conversions became prussic acid nitrogen, related to which, from 80 to 92% obtains assigned hexadecimal min nitrogen. With a 80°/oigen conversion about 525 kg prussic acid can be won from 11 hexadecimal min. Available procedure has the advantage, with a relatively simple system to manufacture on the basis of the products, formaldehyde and ammonia, prussic acid industrially manufactured in the industry in quite economic way.

Rhadon

April 24th, 2002, 09:22 PM

Mega, do you understand these machine translations <img border="0" title="" alt="[Eek!]" src="eek.gif" /> ?? Whenever I read translations made by computers I use to get headaches...

nbk2000

April 27th, 2002, 04:12 PM

When I experimented with HCN, I made test paper for detecting it by dipping a piece of copier paper into a water solution of iodine. The paper turns deep blue from the startch sizing reacting with the iodine.

When exposed to HCN, the blue color disappears. The faster it disappears, the stronger the HCN concentration.

My favorite test for liquified HCN purity was to have a roach in a flask. I'd add 1 (one) drop of the HCN solution to a one liter flask with an adult roach in it. The quicker the roach died, the greater the % of HCN in the test solution. Pure HCN will kill an adult roach in less than 40 seconds, with NO direct contact, only vapors.

Try using a mix of hydroxide and carbonate. The hydroxide lowers the m.p., the carbonate reacts with the iron and nitrogen to form the cyanide. No more than 25% hydroxide should be needed to provide a flux for the melt.

Rhadon

May 21st, 2002, 02:38 PM

Yesterday I realized that I did a mistake some time ago:
I proposed a cyanide test that involves reacting a substance (which is thought to be NaCN or KCN) with sulfur. My intent was to get NaSCN or KSCN, but this won't work because the thermal decomposition of NaSCN already takes place at 368° C which should be less than the reaction temperature of NaCN + S --> NaSCN.

[ May 21, 2002, 01:42 PM: Message edited by: Rhadon ]

Polverone

August 2nd, 2002, 12:36 AM

I have recently been able to experiment further, with encouraging results, pursuing a new route. First, I found a British patent, (710143), that relates a method of preparing cyanates from cyanuric acid. In the patent they are concerned about avoiding cyanide, but I am obviously NOT.

Quick summary of the patent: powdered alkali carbonates are mixed with powdered cyanuric acid and heated to about 520 C. If this is done in a carbon dioxide atmosphere, there is no detectable amount of cyanide formed. The reaction is carried out in a closed steel vessel at atmospheric pressure. Only about 2/3 of the stoichiometric amount of alkali carbonate should be used. If more carbonate is used, some remains unconverted to cyanate. If less is used, some ammonium carbonate and other products form.

I was using an open vessel so I used a slightly larger excess of cyanuric acid than the patent recommends, especially since I was planning on heating the mixture strongly enough to drive off any ammonium carbonate.

Here's how my latest experiment went:

I strongly heated sodium bicarbonate (obtained as baking soda) to produce sodium carbonate. I have sodium carbonate on hand but it is in the form of coarse granules containing some moisture, and I wanted a fine, anhydrous powder. I measured out 20 grams of the freshly prepared sodium carbonate and 27 grams of cyanuric acid granules. The granules were obtained as a swimming pool supply - "chlorine stabilizer, 100% cyanuric acid." I reduced the cyanuric acid to powder in a mortar and thoroughly mixed it with the carbonate. I also powdered 5 grams of charcoal and set it aside.

I poured the powder mix into a stainless steel dish, put the dish in a ring stand, and took the stand outside. I heated the dish with a large laboratory burner using propane as a fuel. Considerable "smoke" was given off as the mixture was heated. I don't know if this was volatilized cyanuric acid, ammonium carbonate, or a mixture of substances. It took about 10-15 minutes for the powder to completely melt down to a fluid. This occurred at a temperature so low that the reaction vessel was not glowing at all, so I am sure that the sodium carbonate (or at least a large proportion) was converted to cyanate. I then added the 5 grams of charcoal (somewhat in excess of what is theoretically needed to reduce cyanate to cyanide) and increased the heat by placing the burner closer to the vessel.

The charcoal powder does not readily mix with the molten salt, but it gradually absorbs and is wetted by the fluid to form a sort of paste. Gas evolution was fairly rapid at first, with lots of large bubbles forming and popping. As time went on the bubbles became fewer but the gases leaving the mix must have changed because the gas jets would ignite and burn with a sodium-yellow flame. I am unsure about this 2-phase gas evolution. What is the first gas that doesn't burn, and what is the second gas that does? I expected the reaction NaCNO + C = NaCN + CO, which could be the source of my flammable gas, but I'm not sure about the first part of the reaction.

The whole time this was going on, the liquid was slowly creeping up the sides of the vessel, forming interesting patterns. It was bubbling a bit on the metal. Near the top of the dish it was forming patterns that resembled toad skin. It was also turning white and infusible at the top - converted, I fear, back to sodium carbonate from my burner's carbon dioxide.

I continued the heating for 20-30 minutes after I added the charcoal. I wanted to heat it until all gas evolution ceased, but I wasn't sure how long that would take and didn't want to run out of propane. Plus, I feared that I would eventually be working counterproductively as CO2 converted my cyanide back to carbonate. Perhaps in future runs I should cover the dish with something to minimize CO2 intrusion.

I then withdrew heat and scraped the paste in the bottom into a lump while it was still hot (experience showed that it was very hard to remove if left as a uniform layer until cold). The lump, once it had cooled somewhat, was added to water. Stirring and heat, over the course of 1-2 hours, broke up the glassy lump and allowed me to filter the liquid to remove the charcoal.

The liquid was evaporated in a shallow dish over the course of a night. There is a faint cyanide odor to the granular masses I have, but I have no idea as to purity. This morning, again consulting the concise Kirk-Othmer, I learned that sodium cyanide can considerably hydrolyze to formate and ammonia above 50 C. Whoops! In the future I will use cooler water. That could definitely explain the strong ammonia scent over the dish in the later phases of evaporation. I thought it was just leftover cyanate hydrolizing and releasing that NH4.

These results seem fairly encouraging. I seem to have made sodium cyanide (of unknown purity, unfortunately) without a furnace, any special chemicals, or handling HCN gas. I don't know if I have enough propane left to do another run before refilling. I would really like to discover if the flammable-gas-evolution ever ceases, and if that also marks the complete conversion of cyanate to cyanide. I would like to try running the reaction at a higher temperature to see if the conversion is appreciably faster. I would also like - good lord would I like - to be able to perform a more sophisticated analysis on my end product to see what is really in it, and in what proportions. The dried powder/lumps I obtained have that HCN smell whenever I open the bottle again.

nbk2000

August 2nd, 2002, 09:07 AM

I am unsure about this 2-phase gas evolution. What is the first gas that doesn't burn, and what is the second gas that does?

I'd think that during the first part it would be CO2, then at higher temperature CO.

As for analysis, try adding concentrated sulphuric acid to a measured amount of what you got. Pass the resulting gases through a very cold condenser (but not freezing) to liquify out the HCN, and the remaining gas through lime water. Weigh out the precipitated CaCO3 and do the math. Subtract the CO2 produced from what you started with and the difference is the cyanide content.

Or, you could not worry about it and just convert all your fusion product into HCN, which is what it's best used for anyways. :)

You may wish to use a propane stove burner (available at most hardware stores) and enclose your crucible (assuming oil can) with a clay pot. This will keep in the heat, and keep out the air.

Alchemist

August 2nd, 2002, 11:22 AM

From Rhodium's sight;

-------------------------------------------------------------------------------
Synthesis of Sodium Cyanide
-------------------------------------------------------------------------------

WARNING! SODIUM CYANIDE IS HIGHLY TOXIC!

Do not attempt this synthesis without adequate ventilation!

Put 420 g of K4[Fe(CN)6]3 (potassium ferrocyanide(II) trihydrate, FW 422) in
a 2 l RB flask. In 1 l chemical glass pour 600 ml of cold water and _carefully_
add 200 ml of conc H2SO4. Pour this hot soln to ferrocyanide, join to the neck
of flask 40 cm glass tube (1-1.5 cm diameter) as deflegmator & condenser, attach
silicon rubber hose and place the end (of hose, of course) in 181 ml 45% NaOH
soln. After 10-min heating at boiling water bath, a strong gas evolution begins;
be careful, do it only under good fume hood. From time to time stir NaOH soln
in receiver flask (this soln may heated up to 80°C, this is doesn't matter -
don't cool). After 1-1:10 reaction complete, no more gas evolution observed.
Voila, you get near 260-280 ml 40% NaCN soln.

PS. Don't poll blue-green residue in sewer system; you sewer pipes will be
covered with this viscous mixture, sure. Carefully pour it (under hood!!!) in
1-liter glass jar and bury it. In uninhabited place, please.

-------------------------------------------------------------------------------
Catastrophe:

Easy Cyanide Synth

In any General Chem book they always some example in the synth of a cyanide.
Here's what mine says...

BaO + 3C + N2 ----> Ba(CN)2 + CO
HEAT

Cyanides can be made by the action of carbon and nitrogen on metallic oxides.
The mixture is heated to a red heat and is usually done in a stream of N2. But
this reaction really doesn't help us much, because we want Sodium/Potassium
Cyanide, but we don't have the proper oxides, right? Well, what's another
metallic oxide? Hmmmmmm maybe Iron Oxide? That's right good old RUST! Here's
what you should do...

First, here's some stuff you'll need:

Iron Oxide (rust)
Carbon (ummmmm, Charcoal!)
Sodium/Potassium Carbonate (Pool neutralizer)
Nitrogen (well the Earth's atmosphere is 70% N2, so that should be fine)
Crucible (you should get one of these, but I guess you can use a tin can)
Bunsen burner (propane blowtorch)

Here's how it works:
1. First we convert the carbonate to the ferrocyanide.
2. Then we convert the ferrocyanide into the cyanide.

Ferrocyanide:
Take 5 parts(by weight) of rust and 10 parts(by weight) of charcoal and 10
parts(by weight) of Sodium Carbonate (make sure they're powdered up real nice)
and mix them together good. Fire up a crucible to red heat, then pour the mix
in. Now everything should kinda fuse together and redden, and every once in
awhile you'll see purplish flames shoot up from the mixture. Stir with a fork
until the flaming stops. Turn everything off and let cool. Chip the mixture into
a large amount of HOT water and stir vigorously. Filter off the unreacted carbon
and mostly unabsorbed iron. Evaporate water to leave the powdered ferrocyanide.

Cyanide:
The ferrocyanide is converted to the cyanide by mixing 8 parts of the
ferrocyanide with 3 parts of the carbonate. Pour the mixture into the red hot
crucible. The powder will melt and bubble and there will be a solid portion and
a liquid portion. When the bubbling stops, pour the liquid portion onto a hard
surface (marble countertop). It will solidfy on the surface and should be broken
up and stored in a container. This will be your cyanide, and should be
relatively pure. There are other ways of making the cyanide from the ferro, look
at rhodiums page. It is a real good idea to have a supply of sodium thiosulphate
or amyl/butyl nitrite handy as cyanide poisoning can occur easily. Oh and do it
OUTDOORS!!! I don't think I need to tell you the fumes are toxic!

The synth does have some complications. For me, sometimes I get it and sometimes
I just don't. I really don't know why, any ideas?

Refs:
General Chemistry; Linus Pauling, 1970

-------------------------------------------------------------------------------

nbk2000

August 2nd, 2002, 01:12 PM

Thamks for posting info that he obviously already knows. :rolleyes:

BTW, Polverone, is there an online british patent database that you're using? I've tried using the esp@ce.net site that the offical British patent site directs a person to, but it doesn't go back past 1977, and is rather poorly designed too.

Or are you using university library resources for this?

Also, since cyanuric chloride is a trimeric form of cyanogen chloride, might it be possible to depolymerize the inert cyanuric into the toxic cyanogen?

[ August 02, 2002, 01:47 PM: Message edited by: nbk2000 ]

Polverone

August 2nd, 2002, 04:43 PM

<blockquote>quote:<hr />Catastrophe:

Easy Cyanide Synth ....<hr /></blockquote>I've looked at that synth before. Since I've been posting on the Hive a bit lately I've also mentioned that it is, as written, a mixture of ingenuity, wishful thinking, and BS. I think "Catastrophe" has an appropriate name. He obviously has never attempted this himself. He gets "purple flames" from sodium carbonate? Methinks he ripped off someone else's description of making ferrocyanides and substituted Na2CO3 for K2CO3 without ever trying it himself. He makes it sound like you can make the ferrocyanide in a few minutes using a bunsen burner and a few chemicals, and you just can't. I should know. Even Kurt Saxon's method, which I am rather skeptical of, has the decency to warn you that you will need a charcoal furnace of sorts and a long reaction time.

And you know what? I encountered another journal article, from the early 20th century, talking about the purity of 19th century potassium/sodium cyanide. It appears that cyanides obtained by such methods (which Kurt Saxon's and Catastrophe's are based upon) were very rarely more than 40% pure. That's good enough for leaching gold or killing things, I guess, but it's pretty lousy if you want to use your NaCN/KCN in syntheses.

I did my patent search on esp@acenet - the patent I discovered relating to cyanate production was issued in the 1950s, so the database must at least sometimes go back earlier than 1977. Cyanuric acid is the trimer of cyanic acid, so if it depolymerizes you only get the relatively harmless cyanic acid. I'm assuming this is how the method I found works, although the authors admit that they're not sure exactly how the reaction proceeds. I'm thinking of trying another reaction run using a little charcoal barbecue as my heat source, since charcoal will get hotter and cost less than burning all that propane. I don't think I'll be analyzing my NaCN with a cold trap and acids real soon. After all, the whole point of my dogged research has been to avoid the generation of HCN except in situ during a synthesis.

NBK, I know you've done some cyanide experimentation before. Do you think you might be able to try this method so that I might compare results with somebody? Assuming you already have a heat source, you can get the materials you need for under $10.

nbk2000

August 2nd, 2002, 07:05 PM

I'd certainly like to, but my situation at present precludes it. :(

However, I can give some advice.

When I did have cyanide (commercially bought) and was making HCN from it, I found an easy way to make test papers to detect the presence and (relative) strength. I'd take photocopier paper and cut it into pH test strip sized pieces. Then I'd dip it in iodine water. It'd turn deep purple, practically black. This was the starch paper sizing reacting with the iodine.

On exposure to HCN, wet or dry, it would rapidly decolorize, leaving the paper with just a faint stain of its former color. Liquid HCN would instantly decolorize. Holding the paper over a vial of the pure stuff would decolorize in a second or two. A drop in a liter flask would take about 10 seconds. That same drop would kill an adult roach in the flask in under 40 seconds, with no direct contact, just the vapor. <img border="0" title="" alt="[Eek!]" src="eek.gif" />

Also, it may be profitable to add some NaOH to your carbonate to act as a flux to lower the melt temperature so you don't have to heat it as high to get the reaction started. I don't know, but perhaps adding rust to the melt acts as a catalyst (as it's known for being) to combine the nitrogen with the carbon?

Covering your crucible to keep out oxygen would be a good idea. A flat piece of steel with a pinhole drilled in it to vent the gases (like cooking wood to charcoal) should do the trick. And keeping the crucible surrounded in an invert clay potter should increase the maximum temp your burner can achieve by several hundred degrees by reducing radiant heat lose and reflecting the heat back inwards.

And since your in a cooking mood :) , what about cooking WP from ammonium phosphate and carbon? Ammonium salts have very low disassociation temps.

Polverone

August 2nd, 2002, 07:29 PM

<blockquote>quote:<hr />And since your in a cooking mood [Smile] , what about cooking WP from ammonium phosphate and carbon? Ammonium salts have very low disassociation temps.<hr /></blockquote>Funny that you should mention that. I tried it months ago. I made two attempts. My reaction vessel was a piece of steel pipe capped at one end. The other end had a screw-on nipple with a piece of copper tubing inserted in the hole, and the joint carefully sealed with furnace cement. I got a lot of unpleasant gasses to evolve, but nothing that I could recognize as phosphorus (I had the venting end of the copper tube dipped in water to condense whatever might come off). I was only able to get the pipe up to a dull red heat in any case. In the later stages of my first attempt I got some flammable gas/vapor near the end that may have contained phosphorus but I couldn't capture it because I had already removed the nipple/tube assembly and was trying to clean out the pipe by letting the reactants flow out under heat.

I haven't tried again because cleaning the pipe was/is a real PITA. After heating, the ammonium phosphate/charcoal mixture was a hard, glassy mass. Water would hardly touch it, even with extended soaking. I had to hammer/chisel out practically all of the remaining reactants. It was slow, labor intensive, and messy.

If I ever build myself a nice little charcoal furnace with forced air feed I will definitely try again. I'm not going to give it another shot with my current setup, though. I might also try absorbing phosphoric acid on charcoal and heating that, since H3PO4 doesn't readily volatilize but just turns into weird polyphosphoric acids at high temps.

Pu239 Stuchtiger

August 3rd, 2002, 05:37 AM

Mr Cool

August 3rd, 2002, 07:30 AM

"The ammonium phosphate will just disassociate into ammonia and phosphoric acid."

Then:

2 H3PO4 + 5 C --> 3 H2O + 5 CO + 2 P

Although it would have to be contained.

[ August 03, 2002, 06:32 AM: Message edited by: Mr Cool ]

nbk2000

August 3rd, 2002, 08:17 AM

Hence the need for carbon, to combine with the oxygen and free up the phosphorous.

vulture

August 3rd, 2002, 04:49 PM

Industrial processes use Ca5[F/(PO4)3] in combination with carbon and Sand (SiO2) to form CaSiO3, which has a relatively low melting point. Well, that is if you consider 1500C as low heat... :mad:

Why don't you use CaC2 instead of carbon, it's a much more powerful reductant, it can even reduce MgO.

Polverone

August 3rd, 2002, 07:38 PM

Oooh, I like that idea Vulture! And here's another gem.

Donald J. Haarmann was kind enough to post this on Usenet in sci.chem as part of a very long post on thermites and Goldschmidt reactions:

<blockquote>quote:<hr />
Aluminium as a Reducing Agent, &c.
L. Franck. Chem. Zeit. 1898, 22, [25], 236-245.
In:- The Journal Of The Society Of Chemical Industry. 17, [6], 612-613.
June 30,1898

Action of Aluminium on Phosphorus Compounds—Phosphorus vapour when led over powdered aluminium, heated to a dull red beat in a current of hydrogen, combines with it with incandescence, forming a dark greyish-black unfused mass, which is decomposed in contact with moist (normal) air, forming PH3, and leaving a greyish-white powder. It is decomposed also by water, aluminium also by water, aluminium hydroxide and a brownish-black residue being left ; and by acids and alkalis, which dissolve it almost completely with evolution of PH3. The compound remains unaltered when heated in air.

At more or less elevated temperatures, all phosphoric, acid compounds (meta-, pyro-, and ortho-salts alike) are decomposed by aluminium. Metaphosphates, however, undergo the most complete change, according to the equation—

6NaP03 + 15AI = 6NaAl02 + 2Al203 + Al5P3 + P3

The addition of silica effects the release of the remaining phosphorus, thus :—

6NaPO3 + 10AI + 3Si02 = 3Na2Si03 + 5Al203 + 3P2

Calcium and magnesium salts are as efficacious as those of sodium, but the superphosphates of commerce are not available for the production of phosphorus in this manner. If, however, bone ash be decomposed by hydrochloric acid instead of by sulphuric acid, a material suitable for the purpose is obtained.

Hence phosphorus may be produced, with almost quantitative completeness of yield, at relatively low temperatures...
<hr /></blockquote>Now the real question is: what is meant by a "relatively low temperature?" One of these days I may just have to find out!

rjche

August 3rd, 2002, 10:13 PM

having read the thread from end to end, a question arises...

Since potassium ferrocyanide is same as ferricyanide, except ferro has four potassiums and ferri has only 3,...

yet all the references above stick to ferro for the conversion...

does anyone know of a reason why the ferri would not as well work?

A practical question since there is a quart jar of K ferri sitting on the lab shelf, but narry a speck of K ferro.

By the way the common blacksmith use of the stuff is to case harden steel, by heating steel dull red and sticking it in the ferro or ferri cyanide, and reheating to melt the coating and decompose it to drive probably both C the N into the steel. It made very tough implements which would hold a fine edge.

Polverone

August 4th, 2002, 01:28 AM

I *think* that the only reason ferro is mentioned all the time is because people are following or building off of historical procedures. Historically, the ferrocyanide was produced and it took extra effort to convert it to ferricyanide - wasteful effort if it's just going to be an intermediate. There are certainly more places that one can buy the ferricyanide than the ferrocyanide because of ferricyanide's use in photography.

nbk2000

August 4th, 2002, 04:10 AM

Both ferro and ferri will produce cyanide, correct?

Machiavelli

August 4th, 2002, 08:16 AM

The main difference between K4[Fe(CN)6] and K3[Fe(CN)6] is that the first one is much more stable because the Fe2+ forms a komplex with an electron octet while Fe3+ can't do that, well at least with HCl you won't get HCN from K4, I'm not sure about K3.

PrimoPyro

August 6th, 2002, 10:02 PM

No one has even mentioned the reaction of chloroform, ammonia, and sodium hydroxide yet. Has no one done this?

CHCl3 + NH3 + 4NaOH --> NaCN + 3NaCl + 4H2O

I believe the process involves the sodium hydroxide causing the chloroform to racicalize to dichlorocarbene which adds to the ammonia and more NaOH to form a geminal aminedial, which spontaneously dehydrates to an iminal which further dehydrates to the cyanide ion.

This process is used industrially to prepare polar organic isonitrile salts. What the hell they are used for is beyond me, but they start with an organic amine and use chloroform and NaOH. Since the R function of the organic amine translates to the R function of the isonitrile, when R = H you start with ammonia and end up with isocyanide HN+C- which spontaneously rearranges to the MUCH more stable cyanide HCN.

Also, phosphates can be reduced to elemental phosphorus with catalytic hydrogen around 750C (upper limit) and lower down to around 350C.

PrimoPyro

[ August 06, 2002, 09:04 PM: Message edited by: PrimoPyro ]

simply RED

September 4th, 2002, 02:48 AM

Why not we make the things easier!
1. buy K3[Fe(CN)6] as much as you want from the chem suplier!
2. dissolve the ferocyanide in water and add KOH
K3[Fe(CN)6] + 3KOH = 6KCN + Fe(OH)3(p)
immediately Fe(OH)3 precipitate falls, decant the liquit and evaporate the water. pure KCN will be left!
This method is described in the book: "inorganic chemical reactions" by Elena Kirkova. I never tried it so far.
By the way:
3Ca(CN)2 + 2H3PO4 =} Ca3(PO4)2(p) + 6HCN
this makes a good wepon, just put the cyanide and the acid in separated ampules and put the ampules (test tubes) near 200g urea nitrate. for example 200g UN and 3kg ampules.

Polverone

September 4th, 2002, 03:57 PM

For many (most?) of us, potassium ferricyanide is not available at local retail outlets. Otherwise your method sounds good. I have tried this with the ferrocyanide, but it was too stable to precipitate anything; ferricyanide must be more amenable. I do think your cyanide-bomb idea is a little heavy on the urea nitrate.

Rhadon

September 4th, 2002, 05:25 PM

Potassium ferricyanide can be made by potassium ferrocyanide and H2O2. I don't know if some HCN will be created during this process, though.

Mr Cool

September 6th, 2002, 02:18 PM

Ooh, and chloroform can be made very easily from acetone and a hypochlorite! I like the look of that synth, Primo. OTC cyanide :D

Polverone

September 8th, 2002, 02:44 AM

<blockquote>quote:<hr /> Potassium ferricyanide can be made by potassium ferrocyanide and H2O2. I don't know if some HCN will be created during this process, though.<hr /></blockquote>What are the conditions? K ferrocyanide + 20% H2O2 + gentle heat gave nothing (well, gave unchanged ferrocyanide).

the_unbound

September 8th, 2002, 07:10 AM

There is a cheaper way to produce HCN without using ferrocyanide or other expensive stuff. Only lime nitrogen, sodium chloride and carbon is needed

Ullmann:
"Black cyanide" (also called "Aerobrand Cyanide") is produced commercially in large quantities by heating crude calcium cyanamide (fertilzer: lime nitrogen / Kalkstickstoff (german) as with carbon, in electric furnaces above 1000 °C and in the presence of sodium chloride [144] . The reaction product is a dark-colored mixture of Ca (CN)2 , NaCN, CaCl2 , NaCl, and excess carbon [145] ; the cyanide content corresponds to about 42 – 44 % NaCN.[142] I. G. Farben, DE 529 506, 1928 (C. Schumann, R. Fick) ; DE 529 575, 1928 (R. Fick).

A electric frunace works fine, however a torch will work, too.

That’s the old good way, which was already used to produce the ZyklonB

Mr Cool

September 8th, 2002, 07:25 AM

That method's OK if you can get lime nitrogen fertiliser, but I've never seen it in England. I believe it's quite common in some places though.
I'm making some methylamine*HCl at the moment, I want to try making acetonitrile with the CHCl3 method but I might have a go at NaCN, too.

Rhadon

September 16th, 2002, 08:35 PM

Polverone, I don't know about the conditions. I just found the information by chance when I was looking through "Römpp" in order to find something that had to do with the ferrocyanide / ferricyanide discussion. But it doesn't mention any details.

OUAGADOUGOU

October 18th, 2002, 11:20 AM

Sorry for restarting this discussion, but I was thinking, what about
the conventional industrial synthesis of alcali isocianates from urea?
e.g. 2 OC(NH2)2 + Na2CO3 -> 2 NaNCO + 2NH3 + CO2 + H2O
Unfortunately I don`t know much about the temperature requirements of the reaction. I remember seeng something like 200 C for this. But I`m not sure at all. It would be great if anyone could check the required temperature. If it would be as low as I recall than this would be a wery easy vay of producing isocianates and then reducing them to cyanides.
Many appologies for my bad spelling!

Boob Raider

October 18th, 2002, 08:49 PM

Check this out .... A quote from a ferrocyanide safety project report that came up when I was looking for the solubility of Na-Ferrocyanide on Ask Jeeves
"The Ferrocyanide Safety Project was initiated as a result of concern raised about the safe storage of ferrocyanide waste intermixed with oxidants, such as nitrate and nitrite salts, in Hanford Site single-shell tanks (SSTs). In the laboratory, such mixtures can be made to undergo uncontrolled or explosive reactions by heating dry reagents to over 200EC. In 1987, an Environmental Impact Statement (EIS), published by the U.S. Department of Energy (DOE), Final Environmental Impact Statement, Disposal of Hanford Defense High*Level Transuranic and Tank Waste, Hanford Site, Richland, Washington, included an environmental impact analysis of potential explosions involving ferrocyanide*nitrate mixtures. The EIS postulated that an explosion could occur during mechanical retrieval of saltcake or sludge from a ferrocyanide waste tank, and concluded that this worst*case accident could create enough energy to release radioactive material to the atmosphere through ventilation openings, exposing persons offsite to a short*term radiation dose of approximately 200 mrem."

Polverone

October 19th, 2002, 04:46 AM

Urea is certainly a viable precursor to cyanides as well, via cyanate. I chose to use cyanuric acid because it is available in smaller quantities and is of greater purity than fertilizer-grade urea.

From W.G. Palmer's Experimental Inorganic Chemistry:

<blockquote>quote:<hr />
Potassium Cyanate, KCNO

Reaction between potassium carbonate and urea in a fused mixture may be regarded as proceeding in two stages:

CO(NH2)2 -> NH4NCO, 2NH4NCO + K2CO3 = 2 NH3 + CO2 + 2 KNCO + H2O.

Since a good yield of cyanate depends very much on efficiently mixed reactants, it is advantageous to replace the deliquescent carbonate by its equivalent of the bicarbonate KHCO3.

Powder in a dry mortar 16 g (1.3 mol) of urea crystals. Add in portions 20 g (1 mol) of potassium bicarbonate, and mix the latter as intimately as possible with the powdered urea. Transfer the mixture to a porcelain basin, which is then heated (in the draught cupboard) with a free flame, the temperature being gradually raised until the contents of the basin are just fused. A brisk effervescence then develops, but after only a short time rather abruptly ceases.
<hr /></blockquote>I've omitted the purity test and purification instructions because they aren't really important for cyanate that's immediately going to be reduced to cyanide.

nbk2000

October 19th, 2002, 06:00 AM

I assume that'll be discussed next?

Polverone

October 19th, 2002, 03:26 PM

The next step (reduction of cyanate to cyanide) has already been discussed above. I haven't done any significant new work with that. A few weeks ago I thought I had come with an idea for the ultimate OTC KCN synthesis: heat potassium hydrogen tartrate (cream of tartar) until it decomposes. This leaves a fluffy mass of carbon intimately mixed with potassium carbonate. Continue to apply heat and add urea. This should yield potassium cyanate, still intimately mixed with carbon. Apply strong heat and wait for reduction to complete... When cool, extract the KCN with cool water or alcohol and let it evaporate at room temperature (heating the mix will cause hydrolysis and loss of KCN).

Unfortunately, this method didn't really seem to work. The material I obtained after extraction crystallized in needles, not cubes (as KCN should). A second run using somewhat longer heating seemed to yield a mixture of cubical and needlelike crystals. I still need to do more experimentation but I'm very busy with school right now and probably will be for the next several months.

Alchemist

October 19th, 2002, 09:29 PM

Hello Polverone,

is it possible to get that book, W.G. Palmer's Experimental Inorganic Chemistry, on the FTP when it's back online? Thanks!!!

Polverone

October 19th, 2002, 09:58 PM

Sorry,

I haven't scanned it, and I doubt that I'll be able to any time soon (i.e. in the next 6 months) due to the amount of work I have to do for school.

Polverone

October 27th, 2002, 04:25 PM

SUCCESS!

I have finally prepared NaCN of reasonable purity from readily available materials without exotic techniques or use of HCN gas.

How did I do it?

Basically, I again prepared sodium cyanate and reduced it with charcoal at high temperatures (see earlier messages in this thread). However, this time I used a small charcoal fire in a barbeque as my heat source instead of a gas burner, so I was able to maintain a higher temperature for a longer time. I heated a mixture that started out as 50 g cyanuric acid, 50 g NaHCO3, and 10 g powdered grapevine charcoal (you'll notice that this was a large excess of cyanuric acid and charcoal - probably not necessary) for 3 hours in an empty soupcan that I lightly sealed with a tapering stainless steel dish placed in the mouth of the can to exclude air and CO2 from the fire. After about an hour at a red-orange heat it appeared that the reduction was complete. No more flammable gases were coming off. However, I left it there for an additional two hours because my fire was still going strong and I figured it couldn't hurt. After removing the can and letting it cool, I smashed the hardened mass of charcoal and salts from the bottom, crushed it, and added it to room temperature water, occasionally swirling it over a period of 2 hours. I filtered out the charcoal and am currently evaporating the solution in a shallow glass pan.

How do I know it's NaCN?

It smells mildly of HCN. Its solution has the slippery feel of a strong base. It gives a lovely prussian blue with an acidified mixture of Fe(II) and Fe(III) salts. It forms cubical crystals resembling table salt when drops of it dry slowly ; NaCN has this crystal structure, NaCNO and Na2CO3 don't. Its solution doesn't smell of ammonia when dried on a hotplate (NaCNO hydrolyzes to release ammonia). However, it does contain some Na2CO3: it gives a white precipitate with Ba(NO3)2 solution. I would guess this is partially due to the solution's long exposure to air. It is taking days for it to dry at ambient temperature, and I didn't want to heat the solution for fear of excessive hydrolysis. Really, I should have removed most of the water under reduced pressure, or in a dessicator, but I don't have either handy at the moment. Perhaps another, faster-evaporating solvent could be used for extracting the NaCN in the future?

Anyway, this is the real deal, the best way I've ever heard of or found to make modest quantities of cyanide salts simply, cheaply, and effectively. I hope somebody finds it useful.

[ October 27, 2002, 03:53 PM: Message edited by: Polverone ]

Mr Cool

October 28th, 2002, 09:28 AM

I'm about to try urea -> cyanate -> cyanide, I'll let you know the results by the end of the day.

<blockquote>quote:<hr />Powder in a dry mortar 16 g (1.3 mol) of urea crystals. Add in portions 20 g (1 mol) of potassium bicarbonate...<hr /></blockquote>What the fuck? The molar ratios are the same if you use the molar ratios as given or the masses, but that's still a rather big error...

Anyway, I'll report my results later, stay tuned...

nbk2000

October 29th, 2002, 04:27 AM

I'd be interested in trying it out once a reliable process has been worked out.

I've got a 10,000BTU propane burner because the power goes out during the winters here so I have to have a way to cook food and heat water when the power goes out for days at a time (RTPB: Plan for failure.)

Would dried urine work as a source of urea? Or would the phosphate interfere? The local gardening places don't stock it for some reason.

Polverone, the non-flammable gas is likely CO2 coming from carbonate decomposition, turning into flammable CO once the reduction nears completion.

Since my goal would be HCN production, any process that produced that without having to make the intermediate CN salt would be welcomed, thought I realize most people try to avoid producing HCN. I've already worked with it though, so I'm not scared of it.

[ October 29, 2002, 03:32 AM: Message edited by: nbk2000 ]

Mr Cool

October 29th, 2002, 08:22 AM

It worked!
16g of urea, 16g of NaHCO3 and 5g of charcoal were ball milled for half an hour, to form an intimately mixed dark grey powder.
The mixture was heated at around 150*C with stirring until the reaction had stopped (lots of ammonia is given off, so do it outside!), as indicated by the effervescence susbsiding. The pasty mixture was stirred as it cooled to break it up.
The black, gravel-like substance remaining was put into an iron crucible with a narrow neck (used to be a CO2 canister), and placed in a very hot (bright yellow) fire. I used a coal fire, fed with air at about 400*C from a paint stripping gun. After a short amount of time a flammable gas was produced (CO), and heating was stopped 10 minutes after this gas was no longer produced. Charcoal was poured into the crucible, which was then left to cool, with the charcoal hopefully excluding most air.

The residue was extracted with cold water and filtered, leaving a clear, colourless, strongly alkaline solution. A drop put into citric acid solution produces HCN smell :)
I've made some CuSO4, so I'll do the prussian blue test too.

NBK: there may not be any fertilisers which state urea on the front, but have you checked the analysis on the sides of the packs? Cheap lawn food normally contains "46% ureic nitrogen", meaning it's pure urea.

[ October 29, 2002, 07:25 AM: Message edited by: Mr Cool ]

nbk2000

November 1st, 2002, 12:10 AM

Some other solvents that NaCN is soluble in:

95% ETHANOL : 5-10 mg/mL @ 20 C
AMMONIA (I'm assuming anhydrous, though maybe 30% will work?) : Freely Soluble

It's not soluble in acetone, toluene, or alcohol(methanol?).

So, lots of denatured alcohol (anhydrous) will wash out the cyanide without hydrolysis, then distill off the alcohol to recover, leaving dry cyanide.

Are you using charcoal briquettes for your carbon? Those things are loaded with all kinds of extra crap like clay. I've looked at activated carbon in the fish tank section of Wal-Mart. It's about $5 for 4 ounces, but that's pure carbon. Any cheaper sources of pure carbon available that you may know of?

Also, off topic a bit, cyanide is used to dissolve gold as we know. But did you know that urea does the same thing? And is actually better than cyanide at doing so? Thing is that the urea solution has to be over 40C to do so, and is more expensive than cyanide.

[ October 31, 2002, 11:15 PM: Message edited by: nbk2000 ]

Mr Cool

November 1st, 2002, 08:02 AM

I never knew that urea would do that, but I suppose any complex-forming compound would, like all amines (except tertiary), cyanides, etc.
I'm using barbeque charcoal, but not the kind that's like powder stuck together into uniform lumps. This is just lumps of pure charcoal, so they look like lumps of shiny black wood. I use it for my BP too, and it works OK. Much better than making your own willow charcoal, because it seems almost as good for a lot less effort.

jimwig

November 4th, 2002, 05:42 PM

there are quite a few German (especially chemical) terms that do not translate to English. so the method seemed to work rather well.

even my English/German chemical translation book doesn't contain a lot of these words/expressions.

megalomania

December 17th, 2002, 02:20 PM

I have been running ideas through my head the past few days because of my newest explosive prep, PL-1. This explosive requires the use of cuanuric chloride, which is itself prepared from hydrogen cyanide. One possible alternative is to use a close derivative, cyanuric acid. While the direct conversion of cyanuric acid to cyanuric chloride seems impossible, I have been mulling possible uses for the stuff.

Cyanuric acid, or its isomer isocyanuric acid, can be found OTC as a pool chemical. It is some kind of bacteria fighter I believe, if I am wrong/right on this I am sure someone will say something. Anyway, if a perfectly dried sample of cyanuric acid is distilled, and the vapors led into an ice cooled collection flask, a considerable quantity of a liquid substance called cyanic acid can be collected. The presence of water in the distillation converts the stuff to ammonium carbonate, which is why the crystals must be dry beforehand.
A modification to this distillation is to instead bubble the cyanic acid into a solution of potassium hydroxide. The acid will be converted to the salt potassium cyanate, KCNO. If potassium cyanate is mixed with charcoal and ignited in a closed crucible it can be reduced to potassium cyanide, KCN. I presume the same could be done with sodium hydroxide to make sodium cyanate, and then sodium cyanide.
It is also possible to prepare cyanuric acid from urea by distilling it dry. Ammonia is given off and eventually impure cyanuric acid forms. This can be purified by adding it to a small amount of sulfuric and gently heating while nitric acid is slowly added until the liquid becomes colorless. The works is diluted with water and allowed to cool whereupon crystals of cyanuric acid precipitate. Another way is to distill urea while passing chlorine or HCl gas over it. Dissolving in water can separate the cyanuric acid from ammonium chloride, the cyanuric acid does not dissolve of course.

What does everyone think about the utility of using OTC cyanuric acid or urea to obtain some cyanides?

megalomania

December 17th, 2002, 05:45 PM

Pardon me, I feel the fool. I just read some of this thread above and it discusses much that I just posted about. I was just trying to snag an existing thread... I guess I am not the only one to have unearthed this particular bit of information.

Boob Raider

April 10th, 2003, 01:50 AM

Hey Polverone .... I tried to cook Blood meal in NaOH, but I only get a multicolored sludge and some dissolved blood, and some bubbling and NH3. I don't get a Na Ferro cyanide color.
Oh BTW Na ferrocyanide decomposes at ~485*C to form NaCN, Fe, N2 and C. A lot of loss of -CN as C and N2.

Marvin

April 10th, 2003, 09:46 AM

Think excess fused NaOH, possibly with a little extra charcoal, and very hot. Sodium cyanide is what forms in the melt, it doesnt convert to ferrocyanide until you add water/acid to the cold product (just until OH is neutralised! it will still be alkaline while free NaCN is still present), as Polverone found out experimentally and is mentioned in one or two of my older books. Use an iron container, but not thin metal, expect it to be attacked somewhat by the melt, and keep air away from the contents. The yellow ferrocyanide 'Yellow prussate of potash' was normally isolated by fractional crystalisation, rather than converted to prussian blue, unless this was specifically required. Ferric chloride is sold for etching circuit boards so you should have no problem doing the test to see if you have actually form ferrocyanide. Ferrous sulphate wont work, in case its not clear from the posts above.

Conversion to ferricyanide is described as follows for anyone interested, 'Red prussiate of potash', ...is slowly prepaired by slowly passing chlorine in, with agitation, to a somewhat cold dilute solution of potassium ferrocyanide until the liquid aquires a deep redish green colour and ceases to precipitate ferric salt. The solution is evaporated until a skin forms on the surface then filtered and left to cool. Purified by fractional crystalisation. Its decomposed by excess of chlorine. Its 'air stable'.

Ferro/ferricyanides are rather safer than uncomplexed cyanides, Id consider trying these before free cyanides anyday, though the melt/acidification steps are potentally just as hazardous.

Mussprat, which you can read for yourself on Polverones site has an improved method for potassium ferrocyanide from blood, by adding potash, saltpeter, iron acetate and charcoal, volume 2 under Iron.

Polverone

April 10th, 2003, 02:54 PM

Boob Raider, I wouldn't bother with the blood meal + NaOH method. The raw materials are more expensive than for my NaCN method, it stinks horribly, it needs constant babysitting as you add the blood meal... yech!

Marvin was right about using an excess of NaOH and keeping it plenty hot, though I never added any charcoal in my few attempts with blood meal. My main problem - as mentioned elsewhere - was the horrible frothing of the mixture as the blood meal decomposed. That and the stink and the impurity of the product and the all-around horridness of the method.

Unless you have a slaughterhouse whose products are going to waste, I really suggest you try the Na2CO3/(urea/cyanuric acid) method.

If you need an especially pure cyanide, see Muspratt on hydrocyanic acid. HCN is quite volatile but has a BP much higher than that of CO2. Therefore one can add a dilute non-volatile acid to crude cyanide at low temperature, wait for fizzing to stop, then distill the HCN into NaOH solution. But of course this would be hazardous and required only if you needed really pure material.

vurr

April 28th, 2003, 06:56 PM

using "electromelting" or HCOOK (mp: 160 C)
http://www.roguesci.org/theforum/showthread.php?s=&threadid=1546
http://www.roguesci.org/theforum/showthread.php?s=&threadid=1548

nbk2000

May 18th, 2003, 02:25 AM

Well, now that we all know how to make cyanide, it might be instructive to see what might happen to you if you ever cross paths with the piggies and they find out you have it.

Below is a copy of a local newspaper article that tells of just such an encounter. I've added commentary in italiacs where appropriate.

In what federal authorities are calling the first case of its kind in Kansas City, an area chemist is facing chemical weapons charges for allegedly possessing potassium cyanide.

Hessam S. Ghane, 53, a naturalized citizen from Iran, is charged in a federal indictment unsealed Monday. Authorities allegedly found 177 grams of the poisonous powdered substance at his Independence home — enough to harm as many as 1,000 people.

He's an iranian, so he must be planning to kill americans, but if he was black, he'd be a mis-understood minority. And since when has 177 grams of KCN managed to kill, let alone harm, 1K people? They imply intent to harm, even though there's no indication of such intended use.

The indictment alleges that Ghane "did knowingly stockpile, retain and possess.. .a toxic chemical not intended by the defendant to be used for a peaceful purpose."

What did he intend to do with it? Unless they can show hostile intent, then it automatically must be peaceful, under the constitutional assumption of innocence till proven otherwise

Potassium cyanide can be fatal if swallowed, inhaled or absorbed by the skin.

Same can be said of water, so what's this prove?

Federal officials did not elaborate on how Ghane came to possess the chemical or on its intended use but said he was thought to have acted alone and was not part of any terrorist activity.

He probably got it from Aldrich. And they won't "elaborate" because there IS NO terrorist intent, but they can't say that fact publicly, not when innuendo is enough to imply otherwise.

There are no allegations of any specific plan to use the chemical, but it is illegal to possess it said Todd Graves, U.S. attorney for the Western District of Missouri, at a news conference.

Pure bullshit! KCN isn't illegal for an individual to possess under the CWC. It IS controlled in the multi-ton quantity because of its use in manufacturing Tabun, a nerve gas.

Ghane is in federal custody and is scheduled for a bond hearing Tuesday. If convicted, he could face up to life in prison and up to $250,000 fines.

If they give him life, then good luck trying to squeeze a quarter mil out of him, what with the BOP pays for inmate labor! :p

Because this matter is the subject of a grand jury investigation," Graves said, "we are not at liberty to provide additional information about the case."

Because it'd then be obvious that the whole case is bullshit P.R. by an AG looking to get in on the "Terrorist" bandwagon, even if he has to create a "terrorist" threat himself.

But he said that there was no longer any threat to the public. Was there ever? Ghane was charged under a 5-year-old federal law that lists potassium cyanide among the substances prohibited under the international Chemical Weapons Convention.

The investigation began Feb. 4 after an incident at Ghane's residence. Police went there after receiving calls that Ghane was "distraught."

His hamster died...CALL THE POLICE! HE'S A DISTRAUGHT TERRORIST! ;)

"Once we got there, we recognized that we had certain issues, and we secured the area and called in the FBI," Independence Police Capt. Gregg Wilkinson said at the news conference.

"We found a raghead with a jar of white powder in the basement...CALL THE FBI!"

Police had gone to Ghane's home on several occasions in the past, Wilkinson said, but he did not elaborate.

Why not? Let me guess..."National Security"?

Federal authorities said Ghane is a chemist who holds a doctoral degree and formerly worked for the U.S. Army Corps of Engineers. He also taught chemistry at Maple Woods Community College in 1996 and 1997. Calls to the college were not returned Friday.

Strange...he's an honest-to-God fuckin' professional chemist who's worked for the military and taught it in college...what the fuck would he be doing with chemicals in his apartment?! :rolleyes:

According to court records, the corps fired Ghane in 1993 after his former girlfriend called his workplace and said he had threatened a co-worker and said he would blow up a federal office building.

RTPB "Never trust anyone, especially a women". 'nuff said

Ghane sued the corps, records show, alleging that racial discrimination was at the root of his firing and that his superiors had stereotyped him as a "crazed Iranian." In response, corps officials cited numerous instances of subpar work performance.

Too bad he wasn't a nigger, then he'd have won millions, but sand-nigger don't count in mizzora

The 8th U.S. Circuit Court of Appeals subsequently ruled that Ghane's termination was proper.

Between 1994 and 1997, Ghane filed at least 19 civil rights lawsuits in federal court against various public officials and lawyers, records show. Courts ruled against him in all of the cases.

He tried to play by the systems rules, and the system naturally won, so what's new?

In subsequent years he occasionally contacted Kansas City journalists, hoping to interest them in a story alleging that he had been fired by the corps after he refused to spy for the Central Intelligence Agency.

Possible. Stranger things have been true, so why not this? Used to be anyone who said they'd be subjected to radiation testing by the government was considered a nutjob...till 50 years passed and they admitted they DID test.

He eventually took his story to theMissouri 51st Militia, an area constitutional rights group. The militia published his story in its newsletter, Necessary Force.

Naturally, anyone who associates with the Militia MUST BE A NUT! Everyone knows that, don't you?

A spokesman for the group, however, said Friday that members soon became skeptical of the tale and uneasy about being associated with Ghane after he asked for money. "We just moved on down the road." Mike McKinzey said. "I wouldn't swear that I believe anything he ever said."

Distancing themselves from someone targeted by major federal heat is a natural reaction, given the already bad name Militias have thanks to the OKC bombing.

Allen Rice, a neighbor at Timber Creek Apartments, said Friday that he had known Ghane about two years. Rice said he had tried to befriend Ghane but backed away about eight months ago because of what Rice called anti-government railings, particularly against the FBI.

And yet, oddly enough, the FBI were the first people the cops called when they went to his house...coincidence? NOT!

Rice said that Ghane blamed the government for the loss of his job, possessions, and house.

All of which was true, since he DID work for the government, who DID fire him.

"He shocked me by the things he'd told me," Rice said. "I was really scared."

And if a wolf farts in New Zealand, french sheep run...so what's his point?

In another paper, the AG said how the cyanide "could have killed hundreds, if configure properly".

:confused:

What the fuck does "configure properly" mean? Use as part of the Tabun molecule? Then where's the rest of the needed chemicals?

Or did he mean pack a room full of naked jews and turn on the gas? Oh...wait...Zyklon required POUNDS of pure HCN to kill...not that such events ever happened, the holocaust being a fabrication of Zionist revisionist history as part of an attempt to discredit Aryan history.

langg

May 23rd, 2003, 06:31 AM

first of all i m sorry for my bad english.
i have reacted NaCN with KOH to have KCN and NaOH in the presence of water as solvent .
when i evaporated the water form the solution solid mass with sour almonds odour left behind
now i added a consider able amount of ethanol in the residue to make tha NaOH disolve in it .but as researched further i found that a small amount of KCNalso dissolves in the ethanol so no problem after filtration i got a considerable amount of KCN.
FeCl3 also gave purssian blue colour in KCN solution.but still there is no surety about the purity of KCN.
I wanted to dissolve my KCNin the DMSO.but it dissolved in a very low amount giving less purssian blue colour in FeCl3 solution.then i performed following tests.
1) KCN + H2O ------->FULLY DISSOLVED + FeCl3 ----->P.BLUE COLOUR
2) H2O + DMSO -----> SOLUTION HOT=?:confused:
I dont know why the solution became hot.
3) KCN + H2O------->FULLY DISSOLVED + DMSO ----->TINY BUBBLES WITH NO SMELL AND HOT +FeCl3 ------>brown granuler precipetates :confused:
what are these granuler precipetates?
instead of using H2Oto disolve KCN for DMSO can any body on this forum tell me what shoul i use and any idea about above test which are confusing in there results.
thanx for any informations given.

sauvin

October 5th, 2003, 01:16 AM

I have potassium ferrocyanide and potassium carbonate. I do not have potassium hydroxide at this time.

Is it possible to synthesise potassium hydroxide from potassium carbonate given that activated charcoal, sulfuric and hydrochloric acids are not a problem?

Marvin

October 5th, 2003, 02:09 AM

sauvin, by boiling pot carbonate with milk of lime for a fairly long time, decanting and repeating the process you can convert a reasonable amount into pot hydroxide. I imagine fractional crystalisation will work for seperating the resulting mixture, or some sort of seperation based on ethanol might be easier. Not really the right thread for asking, but I imagine it will slip past.

langg, I'm not sure what you are trying to achieve but you are aware that the blue colour with FeCl3 is only due to Fe2+ impurities in it? To test properly you need both FeCl3 and FeCl2 or FeSO4. I'm not sure what pH the test should be done at either.

Is your cyanide contaminated with much hydroxide? It certainly wont be neutral but from the sounds of the preperation, this would worry me.

If you are trying to dissolve the cyanide in DMSO, why are you dissolving it in water first, would it be more usual to be using it anhydrous?

sauvin

October 5th, 2003, 07:10 PM

It's very relevent to me because the lack of hydroxide at the moment is the only thing keeping me from trying the ferricyanide+hydroxide->cyanide salt method. I understand your claiming it might not be strictly relevent to the thread in general, though.

Also relevent: I found out the hard way last night that using damp charcoals is not a bright idea. I mixed together 120 grams of cyanuric acid, 200 grams of sodium bicarbonate and 30 grams of charcoal, all ground very finely and scrupulously mixed, into a large stainless steel salt shaker. I selected this vessel because the lid screws on, and I was hoping by filling it up to the very top with this mixture, attrition to oxidation would be minimal. I was unable, however, to turn the vessel a bright orange, it mostly stayed a dullish to medium bright red for about an hour. I don't know yet what kind of yield it's going to return.

I've been having relatively good luck with filtering out the black stuff with coffee filters. The result has generall been very clear, and dumping some ethanol into the water precipitates the cyanides. It's then just a question of leaving the filter out to dry, which happens in just a couple of hours in the wintertime when I tend to keep the indoors very warm :)

I'll let everybody know how this turns out when I've chunked up and dissolved my last fuse-melt.

mongo blongo

October 5th, 2003, 07:38 PM

KOH can be made by electrolysis of KCl in soloution.It can also be found as "pH up" for hydroponics. Maybe someone who has more detailed/other information on KOH synthesis can make a new thread on the subject since KOH has a wide range of applications in our field other than this.

Anthony

October 6th, 2003, 02:51 PM

KOH is also the active ingredient of some drain unblockers. Don't know about the purity/contaminents though.

sauvin

October 7th, 2003, 05:45 AM

I've just dumped perhaps a teaspoonful of potassium ferrocyanide into a flask and covered it with perhaps a quarter cup of battery acid (dilute sulfuric acid). The immediate result was a bluish white foamy substance. I then put the flask on an electric kitchen stove burner on medium heat and boiled it until it turned into a dark turquoise mousse-like substance.

What do you suppose this substance is?

Second question: if there is no way to separate cyanate from cyanide, if both are dumped together in some strong acid, will the resultant gas(ses) be 100% HCN?

Third question: IIRC, HCN can also be produced as a reaction between ammonium gas and methane gas. Do these gasses simply interact spontaneously to produce HCN, or are there other conditions required (heat, spark, etc)?

I am still considering the approach suggested earlier in this (or another) thread involving simply dumping potassium ferricyanide into a slightly acidified container of potassium hydroxide solution. If that approach fails, it's little loss, because the (ferro|ferri)cyanides I'll be purchasing towards the end of this week can always be used to generate HCN to be chilled and dumped into a container of potassium hydroxide (iirc - I'll be reading up more (again) before trying it).

Fourth question: when potassium (ferro|ferri)cyanide is subject to a strong acid, it releases a number of gasses, such as the desired HCN and various nitrogen oxides. Will these oxides react with potassium hydroxide solution to introduce impurities into the precipitate?

nbk2000

October 7th, 2003, 01:04 PM

slightly acidified container of potassium hydroxide solution

An impossiblity!

Acids neutralize bases. Thus, if you had an acidified solution of KOH, you'd have an acidified solution of a potassium salt (chloride if HCl, sulphate if H2SO4, etc), not an acidic solution of an alkali.

The fact that you didn't catch such a simple mistake yourself makes me believe that you're doing things you've no business mucking about with. And trying to make HCN when you've no clue is a quick way to suicide. I know, having almost done it to myself.

sauvin

October 7th, 2003, 08:19 PM

I'll cheerfully enough admit I'm not a chemist. This is why I ask so many stupid questions, but I DO have a need for cyanide and am unable to purchase it. I'm actually a mechanical designer (undegreed engineer) looking into the feasibility of a Joe Sixpack Gold Extraction appliance.

I've found at a party store/janitorial supply a $3.99 litre-size bottle of some solution containing potassium hydroxide of unknown strength.

Sarevok

October 8th, 2003, 12:20 AM

Originally posted by sauvin
I'll cheerfully enough admit I'm not a chemist.
Not being a chemist is not an excuse. There are various books available at any library and bookstore. Read and learn.

If you don't know the difference between an acid and a base, then you NEED to learn the basics of chemistry on your own. Also, you need to do various kinds of common procedures on an improvised home-made laboratory.

If you simply want to make a toxic compound without having knowledge, skill and experience, you will kill yourself. Ah... I'm sure you are not giving a shit about this post... More carrion for the vultures.

According to The War Gases, HCN can be prepared by reacting acetylene and nytrogen using electric sparks. Having the HCN, cyanide can be easily obtained. I'm sure its not hard, just hazardous.

sauvin

October 8th, 2003, 12:33 AM

I wil agree that I have a lot of reading to do. Nobody in this forum is my teacher. Fear - I tend to learn rather quickly.

I have confidence in my ability to work with deadly gasses for the same reason I have confidence in my ability to work with thin-walled vessels containing great pressure: I'm paranoid about the last little detail of a system or process design.

Fear more: chemistry is becoming my new hobby. Whether or not anyting commercially useful arises isn't actually relevent - it's relaxing and fun.

I think I'd discourage most people from trying the acetylene/(any gas here) in the home, especially where "electric spark" is involved, when the only place they realistically have to tinker is the kitchen. The low-pressure HCN methods seem more attractive.

BTW: thanks for the tip about the impossibility of "slightly acidified hydroxide solution". I'd read that somewhere and didn't realise that the PH of such a solution couldn't be adjusted with a sufficiently large dollop of HCl.

nbk2000

October 8th, 2003, 04:02 AM

Nobody in this forum is my teacher.

Oh oh...

If no one here can teach you anything, then that must mean you don't need us to answer your questions 'cause you already know the answers, correct? :p

I do believe we've had a few people here over the years who've copped that kind of attitude...and they're no longer here. :)

As I've said of myself:

"Sometimes the teacher, always the student"

You'd do well to remember that.

And it doesn't matter how quickly you learn if what you're learning is WRONG. You don't have a grasp of even the most fundamental aspects of chemistry (acid/base for instance) and you wish to mess with a one-breath lethal chemical like HCN. Yes, one breath of HCN can kill you, and there's nothing anyone could do to save you because you'll be dead before the ambulance shows up.

This isn't the sort of thing you fuck with with on a casual basis. I did when I was young and foolish (19) and almost died because of it by simply dropping a pea sized chunk in a test tube of acid and getting a whiff of it blown in my face.

Later, I killed my aunts bird and sickened my grandma to the point of puking while distilling HCN in the kitchen (I was wearing a gas mask at the time, so I didn't notice! :D), and that was with fractional ounce amounts.

I wouldn't try that sort of shit now that I know better without a fume hood, but you have yet to go where I've been, but I can't teach you nothing since you already know sooooo much. :rolleyes:

But I'll give you a hint anyways. Dip copier paper in an iodine solution so that it turns blue. If, while still wet, it turns clear...hold you breath 'cause the airs full of HCN! Oh, and if you smell a superstrong "chlorox" kind of smell, you're in big trouble. ;)

sauvin

October 8th, 2003, 05:12 AM

I aplogise in not being precise.

By saying "nobody is my teacher" I actually meant that nobody in this forum is being asked to hold my hand and gently guide me down some lily-lined garden path. I have yet to meet the man or woman who knows nothing I did not already know, or who could not conceive an idea that had not yet occurred to me - in this sense, the entire world is my teacher, like it or not.

In fact, it'd be damned absurd to say "I am not a chemist" in this forum, where people obviously very well versed in chemistry abound, and then claim "nobody has anything to teach me". This would not only be potentially fatal ignorance, it would be arrogance, and grounds for banishment.

Even my gerbils have something to teach (although perhaps not in chemical matters).

Most of my *CN is on the patio, where the wind can reduce relative concentrations admirably. If I go into HCN generation, I'll be on the far side of paranoia to be certain gas leaks cannot occur before chilling and subsequent absorption into some other substance. This shouldn't be as challenging as gang valves operating under tons of pressure per square inch.

Hang-Man

October 9th, 2003, 07:08 PM

What is everyone doing with all this HCN/Xcyanide(s) they are manufacturing? I mean, there are safer poisons. Also, what are the laws regarding cyanides?

sauvin

October 9th, 2003, 07:57 PM

As I understand it, potassium and sodium cyanides, hydrogen cyanide and various cyanogens are either watched or controlled. The only way for me to obtain KCN is to manufacture it myself.

It's used in various ways - I _had_ been interested in a Joe Sixpack Gold Recovery type appliance; many major gold mining firms use cyanides in a leaching process.

Hang-Man

October 9th, 2003, 08:04 PM

Yes I know that. let me be more precise. my question is two fold
a) Can I be arrested for possessing cyanides? Which ones?
b) [cyanide] is used in various ways
I know cyanide has 'various' uses; I want to know if you guys are just killing birds off or if you turn it into something strange and wonderful which I've never heard of. I doubt anyone here is using it to extract gold.

+++++++++++++

Why not try reading the whole post first before asking question A, to which the answer has already been provided in the form of a newspaper article. :rolleyes:

NBK

sauvin

October 10th, 2003, 02:50 AM

As I undersatnd it, yes, you could conceivably be arrested for possession of potassium or sodium cyanide. The charge, if I'm not mistaken, would be "possession of a CBW", if not "possession of a controlled substance". The sentence for such an offence isn't clear to me, except that life without possibility of parole appears to be possible.

Wild Catmage

October 12th, 2003, 05:21 PM

If you want a container to stash your cyanide in, have a look at http://www.pzg.biz/zyklon_b.htm :D

Hang-Man

October 12th, 2003, 05:33 PM

ya right, if I ever end up in court the last thing I want brought to light is an order form "My Third Reich HQ" if there’s one thing The Man hates more than terrorists, it’s Nazi terrorists with cyanide. It would be cool to have though..

sauvin

October 12th, 2003, 06:09 PM

English only God damn it! :mad:

You've already been told once. One more time and the Sturmhuhn will put a bullet through your HED.

sauvin

October 18th, 2003, 02:46 AM

I don't remember being told once to use English only but I know damn well I get a bit carried away from time to time.

I've tried potassium hydroxide + potassium ferricyanide thing. Nothing visible happens. When I mix denatured alcohol with it in an attempt to make (possible) kcn precipitate. It results in three layers, the bottom being a clearish colour (I forget which colour, think it's reddish), a dark layer that looks like a clould of darkly coloured particles of some kind and a milky frothy top layer. I don't know what to make of this.

Either somebody earlier in this thread didn't think something through when he talked about mixing hydroxide with ferricyanide or there's something I don't understand. I may have to try gas generation next but am avoiding that because while I don't actually care what happens to myself, I DO have innocent neighbours so it's going to be a pain in the ass looking for someplace remote to do this.

sauvin

October 18th, 2003, 03:23 AM

Actually, the gas generation is going to have to come from the ferrricyanide. I WAS going to do it by reacting the ferricyanide with acid. It can also be done with heat.

Idiot that I am, I've not tried everything I could think of without posting. If I decompose the ferricyanide in a hydroxide solution, gas generation happens precisely where it's needed without tubing and chamberings and suchlike.

sauvin

November 30th, 2003, 09:05 PM

(from an earlier post)

Why not we make the things easier!
1. buy K3[Fe(CN)6] as much as you want from the chem suplier!
2. dissolve the ferocyanide in water and add KOH
K3[Fe(CN)6] + 3KOH = 6KCN + Fe(OH)3(p)
immediately Fe(OH)3 precipitate falls, decant the liquit and evaporate the water. pure KCN will be left!
This method is described in the book: "inorganic chemical reactions" by Elena Kirkova. I never tried it so far.
By the way:
3Ca(CN)2 + 2H3PO4 =} Ca3(PO4)2(p) + 6HCN
this makes a good wepon, just put the cyanide and the acid in separated ampules and put the ampules (test tubes) near 200g urea nitrate. for example 200g UN and 3kg ampules.

(end earlier post)

I'm discovering that this method works well. If you have the means for measuring precisely how much of each to use, theoretically consuming all the ferricyanide and all the KOH, nothing more need be mentioned except that if too much water is used, it may be easier to precipitate the cyanide salts with ethanol.

Unfortunately, I do not have the means for measuring precisely enough and so have been using an excess of KOH. After filtering to remove the iron, I add ethanol that results in an emulsion that is rich in cyanides. I've found that adding this emulsion to a huge volume of water and filtering THAT after adding a bit of alcohol again yields acceptably pure cyanide salts with trace amounts of lye.

This approach is desirable during the winter months because cooking in the grill in the northern stages in December isn't pleasant.