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megalomania
June 18th, 2003, 03:46 PM
Tony Montana
Frequent Poster
Posts: 143
From: Australia
Registered: JUN 2001
posted 06-27-2001 04:19 AM
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I was wondering if anyone can help, I have made HMTD a few times before. But, this time I used a cheap citric acid that cost about 1 dollar for half a kilo, anyway. I dissolved the required amount of Hexamine, without a hitch like always, within minutes the hexamine was gone leaving a crystal clear solution. Then adding the citric acid made the solution alot more cloudy than normal. I mean cloudy appearance with dust looking floating particles. Its obviously some impurities in the citric acid, will this affect my reaction? Is there a known way of purifying citric acid??After P.S. I have just mixed it so, if anyone is interested I will tell you how precipitation goes, from this cloudy mix!


Tony Montana
Frequent Poster
Posts: 143
From: Australia
Registered: JUN 2001
posted 06-27-2001 10:27 AM
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Well into the reaction now, the HMTD solution now has a quarter of an inch of froth like the head of a beer and also looks like its carbonated(bubbles up the side of the jar). And precipitation is alot slower than usual?
I used 6% peroxide and cheap citric acid, both of which I have never used before and the reaction is not following its normal route. Has any similar things happened to any of you???????
Am I just paranoid??????
P.S.The sooner you reply the better, check the time of my first post, thats 5 minutes after reaction started. Hence, wont need help 12 hours from the time of origanal post.
As I will have finished sythesis, and will be busy testing(now im bored as fuck waiting for it)!!!!!!!!!
[This message has been edited by Tony Montana (edited June 27, 2001).]



kingspaz
Frequent Poster
Posts: 347
From: UK
Registered: SEP 2000
posted 06-27-2001 05:23 PM
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i could be too late here but when using 6% peroxide it takes a couple of days for all the crystals to precipitate. also i wouldn't store the HMTD for very long because of the impurities but if you leave the HMTD under running water for a couple of hours you might be able to remove almost all contaminants.


Tony Montana
Frequent Poster
Posts: 143
From: Australia
Registered: JUN 2001
posted 06-27-2001 06:30 PM
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No, perfect timing, you actually ended up saving the day!(Fuck,I didnt think using slightly different ingredients would effect the reaction this badly)Q:Kingspaz: do you think it is wise filtering(approx:12 hours into reaction) as there would be at least a gram so far, then returning the filtrate to reaction vessel, to complete precipitation?
Is this 1/4 inch foamy head a usual occurance with 6% peroxide?
Do you refridgerate, precipitating HMTD solution?
Do you roughly know how much precipitate forms, during the 2nd day of precipitation, I mean, I am sure that it does, but my synthesis states 6% peroxide, and complete precipitation takes place within 8-24 hours.
What I am trying to say is, is from your experience with 6% peroxide, is it worth waiting, are decent amounts of crystal formed on day 2?????



ALENGOSVIG1
Moderator
Posts: 766
From: Vancouver, Canada
Registered: NOV 2000
posted 06-27-2001 08:20 PM
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When i make HMTD i add the hexamine and if i listen closely i can hear it bubbeling like soda. Seems it gets carbonated when the hexamine is added. When all hcl addidion is done (i use hcl), there is a immediate formation of a very thick foam all throughout the mixture. When filtered, the HMTD foam seems to condense in crystals. I use 35% H202 and 28% HCL. the hexamine i got when i bought 2 portable cooker stoves for 12 dollars. I just wanted then to be able to make meals when im camping etc, but when i opened up the packages, there was about 300 grams of hexamine between both of them.
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Tony Montana
Frequent Poster
Posts: 143
From: Australia
Registered: JUN 2001
posted 06-27-2001 08:24 PM
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The KING: was right! About 16 hours, now. And can visibly see the precipitation occuring, which would indicate to me that it is far from finished...
And looking at it now, I dont think it would be wise to filter until complete precipitation has occured. I asked if you refridgerated your HMTD, because I did not and thought that maybe you did, which would account for, what I saw as a the precipitation taking a day to long!!!!
But I was wrong, and looking now, its looking like if left for 2 days as you said. It will nearly double the amount of crystal I will yeild! Thank you again!
You saved half my precious HMTD, and for that im gratefull.
Q: By the way what sythesis are you using, I dont want the whole fucking thing. Just the book its out of?
I used the improvised munitions black book, which turned out to be fairly accurate, but lacking vital information, as you can probably see!!!!!!!!!!!!!


Tony Montana
Frequent Poster
Posts: 143
From: Australia
Registered: JUN 2001
posted 06-27-2001 09:34 PM
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ALENGOSVIG1: You mention using HCl (hydrochloric acid) in place of C6H8O7 (citric acid). Are there any advantages from using this method(faster precipitation, larger yields, etc)????
Also I would think HCl would generate more heat than C6H8O7, do you have to refrigerate precipitating solution, or am I just wrong about that one?
Your input would be appreciated alot!
Before I was safety first, explosives second. I used to do some stupid stuff, the first time I made HMTD, the bubbling/small crackling sound the reaction creates, that you just brought up, was an experience for me. Anyway, I was in my bedroom with a couple of friends, stirring a jar of reacting HMTD on my lap, and that fucking noise started. I thought OHHHH FUCK its about to explode. Anyway that pissy little noise, thats pretty novel nowadays, brought me the closest I have ever come to actually shitting in my pants!
It may sound weak, but you cant judge until you seriously think you are about to get an instant castration!!!!
I made an oath to god second after the scare I promised, that I would never be so reckless again and, that I would serve him for the rest of my life, for letting me keep my testicles.


ALENGOSVIG1
Moderator
Posts: 766
From: Vancouver, Canada
Registered: NOV 2000
posted 06-27-2001 10:23 PM
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I dont know if there is any advantages to using HCL in place of C6H8O7 except that HCL is much cheaper. There is more heat in the reaction so the reaction vessel must be placed in an ice bath and the hcl added in 5 ml portions. i dont think that it would heat up the solution too much if you were using 6% H202 but im using 35% which causes more heat to be generated. I suppose the HMTD must be washed more thoroughly when using HCL but i always wash any non water soluble precipitate with alot of H20 and H20 NaHCO3 solution
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Tony Montana
Frequent Poster
Posts: 143
From: Australia
Registered: JUN 2001
posted 06-27-2001 11:02 PM
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Yes, with 6%H2O2, virtually no heat was produced, need for an ice bath literally came down to personal choice(and habit). I chose to apply ice bath during reaction and let it precipitate at room temp. I easily cooled the solution to 5 to 6 degrees celsius, and it did not try to climb back up. In my position at the moment, C6H8O7 is actually easier to acquire and cheaper. As theres a health food shop nearby (which hippies own) stocks heaps and practically throw it away, if HCl preformed better, I would not hesitate.


Mr Cool
Frequent Poster
Posts: 991
From: None of your bloody business!
Registered: DEC 2000
posted 06-28-2001 06:49 AM
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I use HCl, and extract the NH4Cl byproduct to use in smoke bombs.
Apart from that I don't think it's any better.


kingspaz
Frequent Poster
Posts: 347
From: UK
Registered: SEP 2000
posted 06-28-2001 08:35 AM
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Tony, the method i use is as follows:
30ml of powdered hexamine is added to 200ml 6%peroxide solution. i stir this for 5 minutes then leave it to sit for a further 15. then i add 50ml H2SO4 from a car battery. then i stir some more and leave the solution in the fridge for a couple of days. i'm not sure the proportions are optimal but thats what i use. i think the reason precipitation takes longer with 6% peroxide is because there is 94%water in it.