PETN

[stanfield]

"x g of 10 weight nondetergent motor oil"
I'm not a specialist in motor oil but what "10 weight" means exactly ? In france, the most common oil I found is "10w40" I thought "w" means weight but no, this is WINTER ! so, how can I know the "weight" of the oil ?

thanx !

[cutefix]

A 10 weight motor oil is a grade assigned by Society of Automotive Engineers(SAE) in classifiying these materials according to viscosity.
It corresponds to an oil with a viscocity number of 6-8 centistokes @ 100 deg Fahrenheit.
For more explanation about motor oil characteristics check this out:
<a href="http://www.vtr.org/maintain/oil-overview.html" target="_blank">http://www.vtr.org/maintain/oil-overview.html</a>

<small>[ May 29, 2002, 04:20 AM: Message edited by: cutefix ]</small>

[stanfield]

a big thanx, very interesting page both for explosives and automobile !

see ya !

[stanfield]

so, if I well understood, I need an oil like 20Wxx ? right ?

[Zambosan]

The xxWxx oils are multi-viscosity synthetics; I think you want to find a single-viscosity petroleum oil.

[john doe]

PENTAERYTHRITETETRANITRATE

Un agitateur magnétique est t'il indispensable pour rester vivant en faisant cet explosif oubiens sa importe peu ??

Merci

Keep it in English please. If you specifically need help in French, try emailing members like Stanfield directly. No, a magnetic stirer is not needed, hand stiring is fine. PETN isn't particularly liable to run away nitration followed by detonation.

<small>[ May 29, 2002, 03:16 PM: Message edited by: Anthony ]</small>

[stanfield]

A magnetic stirrer helps a lot !
When you add 100g of pentaerythritol the addition takes 1h30 minimum and you'll have to do some musculation if you want to stir the solution only with your arms ! :)

[Microtek]

Stanfield: I suggest you try the procedure where you first dissolve the pentaerythritol in H2SO4 and then add this solution to HNO3. This way, the nitration doesn't produce much heat, supposedly because the heat of dissolution has already been given off.
Dissolving the PE in H2SO4 takes a while, especially as it has a tendency to form lumps, but if you add enough glacial acetic acid to wet the PE before adding H2SO4, this lumping does not occur. The acetic acid is volatile, so it will evaporate as the soln heats up.
Yield of this method is excellent in my experience.

[stanfield]

I love the HNO3 method 'cause the final product is easy to purify...
Sulfonitric mix is cheaper to do but a bitch to remove all traces of acid !
HNO3 method is definitively my favourite !

I've also heard that the heat produced by the reaction is only due to the formation of water (esterification produce water...), is it right ?

thanx !

[shootersharp]

@stanfield
from which supplier have you bought your distillation apartus???

[stanfield]

My 5-liter apparatus ? a little reseller in france, 10 Liter and more are available... but the price rises !
Otherwise, she's nice ! I must take a photo and post it there !
I'm always looking for a cheap vacuum pump in garden store but it's not an easy task, there are lot of models !

see ya !

[Microtek]

Removing acid traces from the product is not a problem; you dissolve the PETN in boiling acetone ( solubility is high, so not much is needed ) and add dry bicarbonate. When the acetone solution gives neutral or slightly alkaline reaction with litmus paper, the PETN is crashed out with water.

[da man]

About PETN being made with only 95%+ nitric acid, how come it doesn't require sulphuric acid? It's a standard esterification reaction, right, so why doesn't it need the sulphuric acid to dehydrate the water produced?
Lately i've been making PETN using 70% nitric acid and adding sulphuric acid to dehydrate the initial water, and do the reaction as normal. Another question is why with the sulphuric acid/KNO3 method, you don't need to monitor the temperature, whereas with the 95%+ nitric method you do? So with this improvised method i use, could i add it more quickly and not bother keeping the temperature so low, because it takes a long time keeping the temperature low?

[shootersharp]

@Stanfield
Id like to have a to the @mail adress from this supplier, because i didnt find a good supplier for those things in germany! :(
THX
Shooter

[stanfield]

shootersharp, I well know the boss of this supplier, it's like a good friend and he doesn't sell to international countries...
The only solution is : I buy for you this apparatus then I resend it to you...

da man, the theoritical amount of nitric acid is 117 mL if I remember correctly, so why sould we use 400 mL of nitric ? that's easy : The PETN, in a solution of nitric acid wich the concentration is between 65% and 70%, the PETN is unstable (back to pentaerythritol by hydrolyse...). PETN is stable below 60% and above 80%. Furthermore, the reaction produce water so, when you add your pentaerythritol, the concentration of the nitric acid decreases by the formation of water... This is why we use large excess of nitric acid. At the end of the reaction, the concentration of the nitric acid is 82% and so, the PETN is stable. Then you MUST add lot of ice water to precipitate the PETN and espicially to pass rapidly below the concentration of 60%.

hope this helped you !

<small>[ June 01, 2002, 07:27 AM: Message edited by: stanfield ]</small>

[stanfield]

shootersharp, I always have my old distillation apparatus with 1 Liter boiling flask, maybe this could interrest you.. I will resell it for about 120€...

[da man]

Stanfeild, wouldn't it be more economical though to only use the required nitric acid (117ml for 100 grams i think you said) and add sulphuric acid to dehydrate the water (as in standard esterification reaction). This would mean the sulphuric acid would dehydrate the water, keeping the PETN stable, without having to waste precious, nitric acid. Do you know if this would work?

[stanfield]

Nitric acid isn't precious for me anymore since I received my 5 Liter distillation apparatus :) Now, I can produce nitric acid liter by liter ! so, wasting isn't a problem... But, for other people, who don't have my luck, the sulfuric acid method must be tried... Don't forget to well wash with acetone at the end...
But I don't know the ratio between nitric and sulfuric, keep informed first !

see ya !

<small>[ March 11, 2003, 12:36 PM: Message edited by: stanfield ]</small>

[da man]

Stanfeild, how do you distill your acid? I recently got a small distilling flask, and have attempted to distill nitric acid once, though it wasn't very succesful. I was using an oil bath to heat it, and i couldn't get it to boil, so i made it hotter, and then it bubbled up and went red (nitrogen dioxide), and there was still very little coming into the receiving flask. Alot of it was condensing on the top of the distilling flask, and just falling back in.
Do you have any suggestions, could it have not boiled because my apparatus was totally inclosed, which could have made increased pressure and made the nitric acid boiling temperature higher?

Thanks for your help.

[stanfield]

I really don't know why the vapour haven't passed through the condenser ! Is it a "homemade" distillation apparatus ? or a chemical grade apparatus ?

EDIT : If the vapour are falling back to the boiling flask, there isn't enought heat, try to heat it harder... I don't use oil bath, only pure flame !

<small>[ June 02, 2002, 03:23 AM: Message edited by: stanfield ]</small>

[Microtek]

Da Man: If the vapours condense too soon, try wrapping the flask in cotton wool and keep it in place with Al foil ( as used in the kitchen ). We used this in one of the labs that I worked in at university. When applying heat, I use a sand bath placed on an electric hot-plate bought from a camping store. Lots of NO2 is produced, but that can't be helped when distilling at atmospheric pressure ( the NO2 in your HNO3 is not a problem with PETN production using the H2SO4/HNO3 method ).

[stanfield]

Why Megalomania "recommend" a nitric acid free of nitrogen oxides ?

[Mr Cool]

NO2 makes the HNO3 more oxidising, resulting in decomposition of PE, higher temperatures, faster decomposition of PE, higher temperatures... ignition.
Unlikely in a small batch, but I bet that's the reason.

[10fingers]

That idea Microtek had about insulating flasks does help a lot.
I use a piece fiberglass insulation and hold it in place with a clothespin.
I think by doing this you can slightly lower the temp at the bottom of the flask and still have a high enough temp at the top so that the distillation products don't fall back down. This will speed up distillation time and reduce NOx byproducts.

[da man]

Thanks for your help, everyone, i'll try distillation again next weekend, i didn't get a chance this weekend, i was busy. Does anyone have a suggestion for heating it evenly, or is oil good? I'll try that idea for insulating it microtek, thanks.

<small>[ June 02, 2002, 09:05 PM: Message edited by: da man ]</small>

[ALENGOSVIG1]

I usually distill my nitric acid with an oil or sand bath. Both work good. There's always lots of acid rolling down my distillation flask but i get a steady stream of nitric flowing down my condenser.

i like the method microtek posted. The same thing can be achieved using a sand bath. You must burrying almost all of the flask in the sand.

Da man, you do have the distilling flask elevated above the recieving flask dont you? :D

[Microtek]

When using the H2SO4/HNO3 method temperature control is not a problem; when adding the H2SO4/PE solution to the nitric acid temp rises about 3-5 C if you add it all in about 10 seconds in a steady stream ( when nitrating 8 grams of PE ). Considering that nitration temp with this process is 40-60 C, I actually need to heat it.

[Mr Cool]

Just a general question about HNO3 distilation - how long does it take you lot to get, for example, 100mL? And what size glasswear do you use?

[stanfield]

I personnaly use Nitrate+sulfuric method and this is long...
Furthermore, now I bought my 5 Liter distillation apparatus, this is long long long ! (1000 mL of 100% nitric acid at the end :) ! )

I found, in a hardware shop near me, 58% nitric acid... What's the procedure to concentrate it ? I know you must add sulfuric acid, but how ?, which temp ?

thanx !

<small>[ June 03, 2002, 02:44 PM: Message edited by: stanfield ]</small>

[da man]

Stanfield, you just have to add conc. sulphuric acid to your nitric acid and distill as normal, add about 200ml sulphuric for 100ml of nitric i think (its probably more economical using your normal method of getting conc. nitric acid). I think there was a previous post on this, in the archives.

[stanfield]

I think this method is probably cheaper than nitrate+sulfuric because when you finished distilling you mixture, there is the diluted sulfuric acid who remains in the boiling flask, so, if you heat it, you could probably re-concentrate it and then, you could re-use it for distillation...
this have to be tested...

thanx !

[Microtek]

I use equal volumes of 62% HNO3 and 96% H2SO4. Distillation of 30 mL takes about 2 hours ( could be less; I don't attend it ).

[stanfield]

2 hours for 30 mL !!!!!!!!!!!!!?????????

[MACE]

hi

i think da_man`s idea to use a mixed acid is good because this will save some nitric acid. i distll my HNO3 form AN and H2SO4 it costs a lot of time to clean the AN and concentrate the sulfric. if anyone can give me some ratios for the acid mix i will try out.
an other question: has anyone an idea how to get nitric acid in germany?

***mass is just a physical interpretation of energy***

[stanfield]

did you tried at a drug store ?
other wise, I use sodium nitrate instead of AN so, the ratio must be a little different...

see ya !

[MACE]

hi

no, because the drugstore people ever asks me questions that i can`t awnser (know what i mean?). why shold i use KNO3 for HNO3 manufacture?it`s more expensive than AN.
last weekend i tied megalomanias method with concentratet HNO3 to make PETN.
i used 45ml HNO3 and 11g PE. i held the mixture at 1°C during the nitration (the procedure said below 5°C). after dumping the reaction into ice-water nothing hapans no crystals no nothing. i let it stand over night and still nothing. what`s wrong??

sorry for my bad english

[Mr Cool]

How concentrated was your HNO3? 70%, the usual stuff that people call "concentrated", isn't good enough without H2SO4. If you used 90%+, colourless HNO3 then I can't think of anything that could go wrong.

[Jumala]

Hallo mace,
I think it was a too low concentration of HNO3. Would you have had added H2SO4 it had removed the water and drives the PETN out of the solution.
You can also use the H2SO4 + KNO3 method like posted before. It hasn´t the perfect yield but the yield it is good and the method simple.

Oh, where have you bought the PE?

[MACE]

hi

i got my HNO3 by destilation of AN and H2SO4 therfor i think the acid was &gt;90%. the color was not complete white there was just a very slight yellow color left (could this be the reason for my failture?).
i tried the process with H2SO4 + KNO3 a few days befor but i wasn`t able to hold the temperature below 40°C and the complete stuff boiled over and produced manny NOx (i did this outside).
i din`t add H2SO4 because i don`t know any ratios.do you think it`s posible to use 65% HNO3 with H2SO4? if yes can you give ratios?
i got my PE form omikron. it was 20,70DM for 250g. you can order online and they send your order by mail look at: <a href="http://www.omikron-online.de/cyberchem/" target="_blank">web page</a>

bye

[stanfield]

very interesting page ! I hope they sell all over the €urope !
Why the hell don't I find they pages myself !?

thanx !

[MACE]

hi

this weekend i figured out a procedure to make PETN with 65% HNO3 and &gt;95% H2SO4.
here is what i did:
-take 5g PE and grind up into fine powder
-mix 10ml 65%HNO3 and 20ml &gt;95%H2SO4
-cool acid mix to 20°C in an icebath
-add all the PE at once and stir
-cool the mixture until it reaches 15°C then take out of the icebath
-hold the temperature betwen 20 and 25°C for 20 minutes and stir from time to time
-now you should have a white pasty mass
-dump the mix into 150ml cold water and stir around
-filter and neutralize with sodiumcarbonate like usual
my yield was aprox 60% that`s not very good but i think it`s because i used only 5g of PE. also possible that the yield is a litle higher if you let it nitrate for 30 instad of 20 min.
if you try this out post your results.
bye

[stanfield]

Doing HE explosive in little quantity always decrease the final yield !

[MACE]

hi

ya i think you`r right but i thought a little batch wich goes out of control is better than a big one. in my hollydays next week i have time to try bigger batches and see if the yield rises. i don`have internet exsess in my hollydays so i can`t post the results until i come back.
bye

[stanfield]

why do you want to loose control ? the nitrations is stable in order to have free nitrogen oxides nitric acid ! don't worry ! :)

[MACE]

hi
i also thought so but as i begun to develop my procedure i did this:
-mixed the acids
-started the addition of PE at 30°C bit by bit
after approx the half of the PE was added the temp starts to rise up to 60°C (reaction still in the icebath!) and lots of NOx was produced at this time i stoped the reaction.
this is what i meen when i say out of control <img border="0" title="" alt="[Wink]" src="wink.gif" />

bye

[stanfield]

sorry, I don't saw you used both sulfuric and nitric acid method... I only use nitric :) . By that way, yes, runaway could occur, you must be cautious... 30°C is too HIGH ! lower the temp first then add your PE !

[bonnsgeo]

i have a real stupid question: when you add 97 % sulfurik acid into à 68 % nitric acid solution , the mix become very hot !? isn't it ? (with me it become really really hot ! ..i think its absolutely normal because of the water which react with sulfurik acid!)

so when you mix 100 ml of nitric and 200 ml of sulfurik is it really DANGEROUS or not ? :confused: .... how do you do that : do you mix it quickly or do you add slowly the sulfurik ?

thx for your answsers. :D ..because i really dislike this reaction. :(

and sorry for my english. <img border="0" title="" alt="[Wink]" src="wink.gif" />
bonnsgeo

[mongo blongo]

Heat is generated when the sulphuric is disassociated in the water in your HNO3. You have 68% HNO3 so there is quite a bit of water.
If I was you, I would add it slowly to prevent boiling and I would also spell sulphuric acid right. :)

[bonnsgeo]

i know mongo :) but all the persons who tried this mix always say that they mix nitric and sulfurik in one time !

the last time i did this mix ,it makes me 2 hours and an ice bath to do it for only 50 ml of nitric 58 % and 120 ml of sulfurik !) ...because i really slowly add the sulfurik!! (..and finally the nitration didn't work <img border="0" title="" alt="[Wink]" src="wink.gif" /> )

...

ci@o

[kingspaz]

bonnsgeo, you've been warned by mongo. don't mutilate the english language. you have 3 options:
1. spell it sulphuric (english way)
2. spell it sulfuric (american)
3. HED

HED may seem a harsh option but if people start spelling stuff like fucking k3\/\/\/lz then it will give the impression that its acceptable when it is not.

[bonnsgeo]

tss ... ok ok ...
i'd like you gave me an answser instead of a lesson of syntax. :mad:

ci@o ci@o

(B- Don't be cheeky to the moderators.)

<small>[ July 17, 2002, 10:25 AM: Message edited by: Bitter ]</small>

[MACE]

hi

if i make my 20/10ml mix the temp dosn`t rise so much. starting with a acid temp of ~20°C results in a mix temp betwen 30 and 35°C (in an icebath).
anyone else tryed my new procedure until now?
(i think we all know whats ment by sulfurik. don`t we?)
bye

[Anthony]

Personally, I'd cool both the HNO3 ane H2SO4 in the fridge, mix them and put the mixed acid back in the fridge to cool down. If you do this a couple of hours before you plan to start the synthesis then you're not standing around waiting for things to cool (I hate that).

[stanfield]

I don't like this idea, a fridge is wet, this will maybe decrease the concentration of your acid, no ?

[Anthony]

If your fridge is all wet inside, plug it back in <img border="0" title="" alt="[Wink]" src="wink.gif" />

You could put a lid/stopper on the container if you're worried about humidity. Then again, with 68% HNO3, you've already got a butt load of water anyway.

[MACE]

hi

precool the acids will be a good idea but i`m shure my mom will be very unhappy if i put stuff like sulfric or nitric in her fridge :D
other question
do you think it`s possible to use some silica gel balls(the stuff in the little bags which lies in new shoes for example) to concentrate nitric acid?

bye

[bonnsgeo]

hmmm mace i think this balls are just for humidity and that's all and if you put it in an acid it will react with it.

ci@o

[ALENGOSVIG1]

I dont now if the silica gel balls would work. Im assuming they wont but i could be wrong. your best bet for concentrating your nitric is to either dehydrate it with H2SO4 and distill it or dehydrade it and extract the nitric acid with methylene chloride. Two good sources of methylene chrolide (DCM) are acrylic solvent and furniture stripper.

[stanfield]

hehe, maybe a new explosive recipe ! 2,3,89,583 nitro-silica-gel ! muhahahahahahaha !!!

[da man]

MACE, i often make PETN from 70% nitric acid, and 98% sulphuric with about 90%+ yields (as good as with the standard 95%+ nitric method).
I use 150ml of 70% nitric (you could substitute a slight excess of 65%), 50ml of 98% sulphuric acid, and 26g of PE. From this method i usually get yields of over 60g!!! (and it uses little sulphuric acid).

<small>[ March 10, 2003, 01:30 AM: Message edited by: da man ]</small>

[MACE]

hi
da_man this sounds really good i will try this right now in my hollydays and post my results when i`m back.
i also try what happens with silica gel if put in nitric acid
(maybe stanfield is right :D )
bye

[bonnsgeo]

hello !
i tried to make plastrite , a french explosives like plastic (87 % of petn and 13 % of oil and pib)

<a href="http://noncar.levillage.org/evap.jpg" target="_blank">http://noncar.levillage.org/evap.jpg</a> (here the photo during the evaporation of gazoline)at this step there is gazoline + petn (9g) + polyisobutylene (1.5 g)

<a href="http://noncar.levillage.org/dry.jpg" target="_blank">http://noncar.levillage.org/dry.jpg</a> (here when there is no more gazoline)

<a href="http://noncar.levillage.org/oil.jpg" target="_blank">http://noncar.levillage.org/oil.jpg</a>

and ... the final step failed ... i added to much oil and so the mix is now a paste ... i hope some oil will evaporate to have something more "plastic" ....

SHIT ....

ci@o

<small>[ July 19, 2002, 09:31 AM: Message edited by: bonnsgeo ]</small>

[Mr Cool]

I've just noticed, that site claims to have achieved a yield of about 102%. Someone is either making things up, or not taking any care with purifying and drying the product. In fact, he says not to recrystalise from acetone! Unwise advice...
He has 300% of the amount of HNO3 needed, and comparatively little H2SO4. I have not tried the method so this is speculation, but I think it might be better to have a little less HNO3 and a little more H2SO4. Certainly most methods for producing nitrate esters have at least equal volumes of 98% H2SO4 and 70% HNO3 to ensure a full nitration.

[da man]

i don't know if it's an excess or not but i have tried that method and got very similar yields (around 60g from 26.2g).

[Mr Cool]

Hmmm... I will try it.

[bonnsgeo]

i have a question which is in my mind since a lot of time.

do you think it's possible that PE dont nitrate four times ? (we could obtain pemn (mononitrate)pedn (dinitrate) and trinitrate) i think particularly to the kno3/h2so4 method which is very slow and maybe the nitration is not perfect with it and we could obtain these products.

is it possible ??

thx
ci@o

[stanfield]

Could it be possible to use and press plastic PETN in a detonator ? I think this will be usefull because, when it will be pressed, it won't move anymore ! The powder will because of vibrations, transport, manipulating...

thanx !

[kingspaz]

that would be a good idea but you must remember that plasticised PETN will be much less sensitive to inititation than straight PETN. this would mean you would need more primary which probably would be less safe. if you make a detonator press then you could press the PETN in to a decent density meaning it shouldn't move around inside the detonator case.

[stanfield]

yeah, I know but with a "big" charge of lead azide or DDNP ?

[kingspaz]

well if you have the DDNP to spare then it could be a good idea but then the primary moves around too. i can't see any real advantages of doing this though.

[MACE]

hi

i`m back from my hollydays and i played around with the PETN procedures.
at 1st i tried the procedure with 102% yield and if you want to have a liquid that can change color,start to buble,give off some funky smelling red clouds this is a good procedure but if you want to make PETN this procedure is crap.
after this failture i played a little with the acid ratios of my own procedure.
if you use 20ml HNO3 , 20ml H2SO4 and 5g PE the PETN only prepicrates if you dump the reaction in cold water but if 15ml HNO3, 20ml H2SO4 and 5g PE is used the PETN prepicrates during the reaction with a much higher yield.
i used my procedure but this time with 15ml HNO3 (65%) and 30min reaction time and had a yield &gt;80% wich is fine for me.

bye

[stanfield]

nice, MACE !

otherwise, is there a way to "block" the powder in the (homemade) blasting cap ? What are your methods ?
thanx !

[Mr Cool]

MACE: I also tried that procedure, and I also got a slight runaway. I left it (in an ice bath) since it all looked pretty quiet, and came back to find it splattered about, and the flask was full of NO2. I still got a fair amount of PETN, but not 102% yield <img border="0" title="" alt="[Wink]" src="wink.gif" />

[MACE]

hi

i just press the PETN in my cap by handforce. i don`t know wich consitency your PETN is but this from my procedure is a very fine powder finer than flour and it holds itself in the cap. i also seal my caps with epoxy on both sides. (was this your qestion?)

i had my reaction in an icebath too (-15°C) but it still got out of control, this was about 10 min after the addition of the PE.
my yield was a litle more then nothing with this procedure.
i think if the mix starts to get yellow because the production of NOx the reaction will end up in a chainreaction.

bye

[bonnsgeo]

hi !

i tried yesterday the method hno3 (67.6%) + h2so4 (96 %) + pe.

for 6 g of pe (and 16 ml of nitric and 24 ml of h2so4) i think i ll obtain 12 or 13 g of petn (not well dry for the moment) its a good yield for me!

but my question is: when i add the last gram of pe, my mix was a thick paste a litlle yellow (like u Mace) i think its because of NO2 but why ? because it cant evaporate ..so it stay in the thick and sticky solution ...?
maybe the concentration of nitric was between 60 and 80 % because of the pe added before and i know that between theses concentrations its really dangerous to make petn ...

thx for your answsers
bonnsgeo

<small>[ August 05, 2002, 06:40 AM: Message edited by: bonnsgeo ]</small>

[MACE]

hi

it seems your yield is higher than mine can you post your temperatures and the reactiontime?
when i use the method with more H2SO4 than HNO3 i also get a pasty solution but mine dosn`t become yellow. maybe your temp was to high if the temp exeeds 30°C NO2 is produced. i think the HNO3 concentration isn`t a problem because the sulfric absorbs the water this is also the reason the procedure with 150ml HNO3 and 50ml H2SO4 won`t work (for me)

i got some N,N,Dimethylformamide any idea what to do with this stuff?

bye

[bonnsgeo]

hi.

i have a little more than 13 g of petn (my scale just show an integer weight) so the yield is 93 % (approximatively :) i m happy !)

mace: my temperature never exceed 20 degres celsius (i used an bath with water and some ice inside)
i added the pe really slowly, maybe thats why my yield is better (30 minutes for put 6 g .... :) i m patient :) ... it was a test so i did carefully !)

N,N,Dimethylformamide &lt;= what is this thing ??

bye

[MACE]

hi

if i make PETN this weekend againe i will also add my PE slowly like you maybe there is some local overheating if i add the PE at once because of the sticky consistence of the solution
you say your temp was below 20°C i can`t imagine where the NO2 came from if i do the reaction there is no NO2 but it seems that the yield is not decerased by the NO2 so it maybe allright

N,N,Dimethylformamide is some kind of solvent we had at work the name sounds good so i take some

bye

[bonnsgeo]

hmm ... yes this yellow color is strange.

you added your pe at once ??? its not a good thing !!! :)

you ll lose the control of the reaction if you add all the pe at once.

be coooool with the nitration !

bye

[MACE]

hi

i didn`t have temp problemes if i add the PE at once the overall temp of the solution was still below 20°C only the yield was lower then your`s it seems it`s better to add the PE slowly (i`ll try out)
maybe there are some impuritis in your PE this could be a reason for the NO2
bye

[andreas]

It's not a nitration but an estrification as are the manufacture of glicerinetrinitrate, cellulosenitrate, mannitolhexanitrate just to name a few. So it may be a good idea to call it how it's named for the newbies, that way they'll learn more.

[bonnsgeo]

andreas: it is a NITRATION (and esterification just before !)! the exact name for the nitric esters is the "O nitration" because its a nitration of an alcool (acid + alcool = ester and ester + nitric = nitric ester like petn, nitrocellulose, nitroglycerine)

"O nitration" name is because of R-OH (R is the rest of molecule,OH is alcool group) which became R-O-NO2 the oxygene stay in place.

thats all !
bye :)

its hard for me to speak of chemistry in english so i hope it was clear !

[bonnsgeo]

mace ... i reelly dont think there are impurities in my PE ( i hope) ...my PE comes from ACROS organics (pentaerythritol 98%) so ...

maybe the 2 % are impurities :) ...

ci@o

<small>[ August 09, 2002, 07:09 AM: Message edited by: bonnsgeo ]</small>

[stanfield]

I've scanned my box of Pentaerythritol !
<a href="http://stanfield.150m.com/pentaerythritol.jpg" target="_blank">http://stanfield.150m.com/pentaerythritol.jpg</a>
copy and paste in a new window...

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

This adds value to the topic...how? :confused:

:rolleyes:

NBK
+++++++++++++++++++++++++++++++++++++++++++++++++
STANFIELD : Yeah I know ! I was bored so I scanned my box :) please apologize !

<small>[ August 17, 2002, 05:14 PM: Message edited by: stanfield ]</small>

[rikkitikkitavi]

the most common impurities in PE is di-pentaaerithritol C(CH2OH)3-O-C(CH2OH3) and higher polyalcohols, formed in the synthesis of PE.

They will of course all be nitrated and normally dont pose a problem.

Some explosives manufacturer prefer a small content(3-4 %) of di-PE.
Dont ask me why though.

More important is that the crystal size is uniform, so nitration time is constant through batches. PE for nitration is usually run through sieves.

/rickard

[Teck]

I have a question about butyl rubber caulk, what is its product name in stores. and also is it the same stuff used for windshields, like 3M windshield caulking? Also whats the best way to get the PIB out of the butyl rubber caulk, as some one mentioned acetone doesnt work too good.

Also, bad idea to store acid in your home fridge, as someone mentioned that theyre mom would be upset if she found out, I had an ancident where, I put a 500mL flask with concentrated sulfiric acid in the top frezzer and it accidently got cracked and leaked all over the top freezer and down through the whole fridge. When my mom opened the fridge she got freaked. In the end we had to through away the $1500 dollar fridge. It had black stains all over the insides and I think the acid eat away foam in the walls of the fridge.

well anyways about the PIB....

[MACE]

hi

your PE has the same quality as mine therefor i`ve no idea where the NO2 in your reaction came from (i don`t have any). i grind my PE to a fine powder befor i use it.
what is butyl rubber caulk?
i store my acids in PE bottles wich can`t brake :cool: (at least not so easy)
i don`t had time to make some experiments until now because we have some flood problemes here (possible you`ve seen in TV) maybe i`ve time in a week or so.

bye

[Jumala]

I don´t know why it produces NO2, too.
Perhaps the sulfonating of the PE first and then giving it drop by drop in the HNO3 could change this.

Hallo Stanfield, do you remember the price of your PE. I want to buy some but all prices I saw seemed to be to high.

[DarkAngel]

Jumala why don't you never reply on my emails?

<small>[ August 27, 2002, 08:45 AM: Message edited by: DarkAngel ]</small>

[bonnsgeo]

hi.

today i tried to detonate 4.5 g of petn
here is the draw of what i did
<a href="http://rdxmaster.free.fr/failed.jpg" target="_blank">http://rdxmaster.free.fr/failed.jpg</a>
(its written 2 cm for height of petn ..it was 1.5 cm maybe 1 cm i dont really know ..but my petn was well pressed)

The detonator detonated BUT NOT the petn !!! i found all the petn around the site i placed the explosive device, and the plaster at the bottom of the tube was still here with some petn on it (i burned it with a match to be sure : there was petn)

i suppose its because my detonator was nt inside the petn, it was just put on the petn (look at the draw) .. am i right ?

thx for your answsers.

[mongo blongo]

Yes that's defiantly the problem. First press the PETN and poke a hole in the PETN. Push the detonator into the cavity and press the PETN down again around the sides of detonator.

[bonnsgeo]

i have done again some petn today ...

50 ml of nitric at 67.6 % + 40 ml sulphuric at 96 % .

i calculated that i can use 9.5 g of PE with this volume of nitric and suphuric. i prepared 10 grams of pe.

i added the pe ..but when i was at 7 grams added, the solution became again yellow like the other day!! i added some pe again , it became very very yellow (like picric acid !!) and the temperature rised at 25 degres <img border="0" title="" alt="[Eek!]" src="eek.gif" /> i stoped and i added the water
and the mix became white. :p

it stay 2 gm so i only added 8 gm in the mix.

bizarre...
i think i must use more nitric and sulphuric.

bye.
Mace : good luck with your flood in germany ! :rolleyes:

[Microtek]

I think the usual molar ratio of PE to nitric acid is 1:12. This means that in your last batch, 8.5 g PE would have been appropriate.
I have experimented a bit with the procedure on the peaceschem web page and have come to some conclusions that I will share here:
Firstly, it is claimed that 62 grams of PETN is obtained from 26.2 grams of PE. However, the theoretical maximum from 26.2 grams PE is 60.9 grams of PETN, so obviously there is a mistake somewhere.
Secondly, I have found that the procedure is very sensitive to elevated temperatures, thus if 62 % HNO3 and a suitably increased amount of H2SO4 is used, a temperature of as little as 18 C will cause evolution of NO2 which will continue even after the temp has been lowered to below 5 C.
Thirdly, I found that using 34 mL 62 % HNO3, 15 mL 96 % H2SO4 and 5.00 g PE yield was 3.6 g PETN when nitrating 70 minutes at 4-5 C but 9.5 g when nitrating 90 minutes at 10-12 C.
In both cases, stirring was done for about 30 seconds every 5-10 minutes.
It may be that even better yields can be had by nitrating for longer periods or perhaps at slightly higher temps.
Finally, I have found that a faster and more robust method can be used with these concentrations of acid, namely the one involving dissolution of PE in sulfuric acid and then dripping this soln into HNO3 dehydrated with H2SO4. Temp is kept in the 40-60 C range and nitration time is around 30 min, though I haven't tried to optimize yield with this method.

[bonnsgeo]

hi !

1)microtek ..in my book its written that ratio Pe/nitric = 1:5 !!

thats why i used 50 ml of nitric at 67.6 %
calcul
density = 1.41
50 * 1.41 = 70.5
70.5 / 100 * 67.6 = 47.58 gm of hno3
47.58 / 5 (ratio)= 9.51 ... so i wanted to use 10 g of pe <img border="0" title="" alt="[Wink]" src="wink.gif" />

are u sure about 1 : 12 ???? i think its too much nitric !

2)yes i think that sulfonitric mix are more sensitive to temperature , but my mix is always at 11 or 12 degres celsius ..

3)with this mix sulphuric + nitric i always obtain a yield &gt; 95 % with no long time of nitration , i just slowly add the pe and i wait five minutes after the last addition and thats all.

bye
thx .

[rikkitikkitavi]

usually you have a MASS ratio of 1:5-1:6 , like you used bonnsgeo.

47,6 grms HNO3 = 0,75 moles (47,6/63)
10 grms PE = 0,075 moles (10/136)

thus the molar ratio is 1:10 so that means with a mass ratio of 1:6 , molar ratio will be 1:12 (do the calculus)...

it is always very important to define if it is mass or molar ratio of course.

/rickard

[bonnsgeo]

yep. ok.

hmm i thought something ... it very very strange this yellow color , because the last time i did petn i used 24 ml of nitric and 16 ml of sulphuric and i succesfully nitrated 6 g of pe !! (i obtained 13g of petn) so this time i used 50 ml of nitric (double !!!) and i only nitrated 8 g of pe :( Maybe its the time, the solution is programmed to become yellow after 30 min <img border="0" title="" alt="[Wink]" src="wink.gif" /> lol

i am not lucky !
bye

[Anthony]

The mention of nitrating at temperatures below 18*C has me interested. For the XNO3/H2SO4 method, I follow the procedure on MrCool's site which advises a 90min nitration at an initial temperature of 35*C for the PE/H2SO4 addition and then held between 30*C to 40*C.

I recently got a shitty yield and attributed it to my suspect fertilizer grade NaNO3, but I'm wondering if the high temperature could be to blame?

[Anthony]

I recrystalised my shitty yeild of crude PETN from acetone earlier. Left behind was a large amount (more than a few grams) of shitty sludge that was insoluble in acetone. I suspect that it is unreacted PE due to it's appearance, so the NaNO3 could well be to blame.

One thing is that the "purified" PETN is still a dull yellow from the brown/black dye in the H2SO4 used, it's very persistant. I guess it doesn't really matter, but it would be nice to have a pure white product.

[nitriees]

I make PETN yesterday, the H2SO4 i used obtained from boiled down new battery water until giving dense fume, KNO3 arround 96% pure and PE is &gt;97% pure lab grade.
Add KNO3 into H2SO4 until all dissolve, the temperature fall and i feel the solution cold. Is it normal? I tought it suppose to be temperature rise.
Add PE/H2SO4 to KNO3/H2SO4, nothing happen, no temperature change and no crystal formed. With ocationally still, after 90 minutes, no changes. Leave it there. Room temperature is 28~31 degree celcius.
Some "light" crystal and some bubble formed on top of the solution after i come back 6 hours later. I call it "light" crystal because they are floating at the middle of the solution.
After filter and wash with water and sodium bicarbonate, leave it outside to dry. Will test later whether it is PETN or not.
The same KNO3/H2SO4 i prepared earlier, try to make nitrocellulose, but failed. I take out sample during nitration time of 30 minutes, 60 minutes , 2 hours and 24 hours respectively. Tested all burn like normal cotton.

[Microtek]

There must be something wrong with your H2SO4 if it doesn't produce heat when mixed with KNO3. There are no other obviuos mistakes, so I think that's where you should look for improvement.

[Mr Cool]

I also got a bad yield with the KNO3/H2SO4 method on my site, but I didn't bother trying to improve it because I just use ~95% HNO3 instead now. Maybe I will though, since it is easier. My product did all dissolve in acetone though, so what I got was relatively pure.

[rikkitikkitavi]

if you concentrate sulfuric acid by boiling it starts to fume at about 75-80 %. You have to continue until the boiling point reaches above 300 C so concentration goes above 95 %. Otherwise, increase sulfuric acid amount. Sulfuric acid looses much of it dehydrating power below 80 %.

/rickard

[kingspaz]

nitriees, the two nitration attempts you carried out have one thing in common - the H2SO4. also as has allready been pointed out heat should be given out when KNO3 is added to the H2SO4 as nitric acid formation is slightly exothermic due to NO3- being a stronger base meaning H+ will bond more strongly to it than HSO4- releasing energy (i think... :confused: ). i believe you boilded the acid and got confused with steam and maybe thought that was the white fumes. when i have concentrated battery acid this way i haven't had much noticable fumes...
when i have done it i let the water boil away and the solution reaches about 1/5 of its original volume. when this happens the size of bubble produced from boiling decreases rapidly due to lower ratio of water:acid. after heating like this for a a fair bit longer you should notice youself choking on very acid fumes which appear thicker and tend to drift more than steam.
hope thats helped!

<small>[ August 29, 2002, 03:55 PM: Message edited by: kingspaz ]</small>

[nitriees]

Thank you for all of your advice. I will check on the sulphuric acid concentration.
Microtek, do you already try the method you mention earlier,

"Finally, I have found that a faster and more robust method can be used with these concentrations of acid, namely the one involving dissolution of PE in sulfuric acid and then dripping this soln into HNO3 dehydrated with H2SO4. Temp is kept in the 40-60 C range and nitration time is around 30 min, though I haven't tried to optimize yield with this method."

Heat dissipation during dissolve PE in H2SO4 at early stage will reduce the chance for " runaway " nitration ?

[Microtek]

Yes, it may very well reduce the risk of runaway nitration/oxidation. Much of the heat of dissolution is already dissipated by the time the PE is introduced into the nitric acid and you actually need to heat the mixture to keep temp at 40-60 C.

[nitriees]

I try to make PETN again last night, it fail again.
I try two procedures. For the first one, i add KNO3 into H2SO4 slowly,
the solution become very thick and fuming but the temperature just slightly rise. Leave it for reaction for one hour with occasional stirring. Add PE slowly until all of them dissolved, leave it for nitration with occasional stirring on room temperature ~ 28 degree celcius. The solution become warm and start to boil suddenly after 15 minutes and give a lot of NO2, only brown solution left after the run away. I dump this solution into ice/water nothing produced.
The second try, i add KNO3 into H2SO4 and leave it for one hour to reaction in ice bath, add PE into H2SO4 in another biker and warm it up until all the PE dissolved, leave it for cool down.
Add PE/H2SO4 into KNO3/H2SO4 slowly by four portion with ice bath and stir occasionally. Let nitration for 90 minutes. After that dump the solution into ice/water arroud 3 times the solution volume, no PETN crystal produce. Don't know what's wrong, anybody know?

[nitriees]

For the first procedure, Which contribute most of the heat and caused run away reaction?
1) PE dissolve in H2SO4 OR
2) Nitration of PE
For the second procedure, seems like no nitration happen, will it because of low temperature, 0 ~ 5 degree celcius. I used ice/water bath for the whole process because afraid run away reaction happen again. If keep the nitration with temperature 30 degree to 40 degree
celcius, will it trigger run away reaction?

[Anthony]

In the second method, a lot of the heat is generated when you add the PE to the H2SO4, which obviously you control before adding it to the "HNO3". So you don't get as much heat evolved in the HNO3 as you would if you just add the PE alone.

So a runaway reaction is very unlikely and is quite safe to do the reaction at 35*C.

[kingspaz]

a good way IMO to prevent a runaway is to stir like crazy. regardless of what the temperature is if you don't stir well enough then this allows 'hot spots' to develop and the runaway may begin in these areas. if you continue stiring vigourously then no hotspots will develop and thus runaway is less likely.

<small>[ September 10, 2002, 04:11 PM: Message edited by: kingspaz ]</small>

[nitriees]

I try the second method again last night, i mix the PE/H2SO4 with KNO3/H2SO4 in ice/water bath, let the mix solution in there for 30 minutes to absorb any heat develop then put the mix to water bath for nitration ( arround 25 degree celcius )with occasionally stirring. The solution is quite for initial 30 minutes but suddenly boil and give brown NO2 within few seconds. Another failure...
What is the optimum temperature for PE nitration? Less than 5 degree
nothing happen; 25 to 28 degree run away reaction.....
My KNO3/H2SO4 is fuming (white fume) all the way, before or after the additional of PE/H2SO4 either in ice/water bath or room temperature, is it normal?
Vigorously stir by hand continuosly during 90 minutes of nitration is difficult job, i don't have magnetic stirrer.
Any other way to obtain the nitration and minimize the run away reaction?

[Anthony]

I have no idea why your reaction is suddenly boiling. Every time I have made PETN, I have done the reaction at 30-40*C and the heat is easy to control, in fact, I need to use a hot water bath to keep it at around 35*C for the whole 90mins after the addition.

It is quite normal for your H2SO4/XNO3 to fume, it is simply HNO3 vapour.

[Microtek]

When using the first method, temp must be held low, I would recommend below 15 C.
When using the second method, the temp must be raised to between 40 and 60 C once all the PE+H2SO4 has been added to the HNO3 it must be held in this interval for about 30 min with stirring. It may very well be neccessary to heat the mix to keep it above 40 C.
I still think your acid is too dilute, it would also explain the runaway as HNO3 at lower conc is strongly oxidizing.

[nitriees]

The sulphuric acid i used is boiled down from 250ml to 60ml with constant fire for 80 minutes, initiallly the acid boiled with a lot of bubble, after 70 minutes the bubble became less and lesser and just occassionally give some smaller bubble. I left it boiled until no more bubble and dense fume for another 10 more minutes. Will it be sufficient? Do i need to further concentrate it, any method?
When adding KNO3 to the dilute acid i used previously, temperature drop and no fume giving off; the acid concentrate with above method giving fume continuosly and the mix warm up a bit, this is the difference.
How long do i need to wait for the KNO3/H2SO4 to react to produce enough HNO3, one hour is enough? I will go for another try with one day left for reaction.

[nitriees]

This time run away reaction appear just 30 seconds after finish PE/H2SO4 adding.
The KNO3/H2SO4 left for 24 hours reaction seems less thick compare with 1 hour, but still fuming. I let the 24 hours reaction with lid on to avoid moisture absorb.
I divide the PE/H2SO4 to four portion and adding done at room temperature ( 28 degree celcius ). First portion added with stir, wait for 5 minutes, no temperature change. Add the second portion, same thing. Put all the remaining PE/H2SO4 in with continuosly stir,
within 30 seconds, the mix solution became dark brown and start give
off a lot of NO2 and whole thing boil up.
Next try will be do this absolutely in ice salt bath &lt;5 degree celcius.

[nitriees]

Keep the acid and PE mix in 0-5 degree celcius with continuosly stir, runaway still happen. After finish the PE/H2SO4 adding, the mix solution maintain below 5 degree celcius, everything working fine.
The solution start change to brown and give off NO2 and boil after 30 minutes left for nitration although stir is continously.
After NO2 stop let the solution stand for another 60 minutes with stir. Adding 5 times ice water to it, clear yellow solution, nothing precipitate.
The solution boil and give off NO2, is it shown that the nitration of PE start but go to uncontrolable state?
Urea is used to make red nitric acid to white nitric acid, will it be help if add small quantity of urea to my KNO3/H2SO4? Any other suggestion?

[kingspaz]

nitritees what order do you do the additions?
try H2SO4 + KNO3 then cool this to 5*C then slowly add the PE in VERY small portions...small = less than 1cm^3.

[nitriees]

Yes, i let the KNO3/H2SO4 cool to 3 degree celcius first before PE addition.
I add the PE/H2SO4 into it very slowly almost 3 drops per addition and stir for 5 minutes for temperature stable then so on, take arround 45 minutes to finish. The temperature maintain less than 5 degree celcius during addition and 30 minutes after addition before it boil up.

[Microtek]

All of your posts point at too low H2SO4 concentration; if the HNO3 is too dilute oxidation reactions will dominate rather than nitration. When NO2 is given off or when the solution turns brown, it is usually a sign of oxidation. If I were you, I would test the strength of H2SO4 by titration, making sure that it is done very accurately.

[kingspaz]

beat me to it there microtek <img border="0" title="" alt="[Wink]" src="wink.gif" />
or instead of using a titration you could take the conc H2SO4 you have and boil it for 10 minites or so. this should remove the remaining water. and also next time you concentrate the acid from the dilute you should time how long it is heated for before its concentrated enough. titration may also be useful for working out your initial concentration aswell as the resulting concentration. good idea microtek. if i make no sense its because i'm ill and tired...

[nitriees]

I give it another try last night. Heat PE/H2SO4 mix to 50 degree celcius until fully dissolved, let it cool.
Add KNO3 slowly into H2SO4 with multiple small portion until no more KNO3 can dissolve, separate the salt and acid liquid.
Add PE/H2SO4 into acid slowly by few portion with stir, temperature slightly rise. Wait for 1 hour, nothing happen.
Put it into warm water bath maintain between 30 - 40 degree celcius, the solution change to yellow and start give very small bubble, after 30 minutes, some crystal precipitate, the amount of the crystal arround duble of PE added. I thought it is PETN but when i add 3 times of ice water to it, all crystal dissloved left only clear solution. PETN do not dissolve in ice water right? Will it be potassium sulphate? Is nitration happen or not?

[stanfield]

Does anyone have a solubitility table of PETN in nitric acid at different concentration ?

thanx !

[stanfield]

Today I detonated 50g of PETN on a tree, here are the results ! :

<a href="http://perso.wanadoo.fr/stanfield/50g_avant.jpg" target="_blank">1</a>

<a href="http://perso.wanadoo.fr/stanfield/50g_minuterie.jpg" target="_blank">2</a>
Again, thanx to JUMALA for his Timer !
<a href="http://perso.wanadoo.fr/stanfield/50g_apres.jpg" target="_blank">3</a>

<a href="http://perso.wanadoo.fr/stanfield/50g_apres_grosplan.jpg" target="_blank">4</a>

<small>[ March 02, 2003, 09:15 AM: Message edited by: Mr Cool ]</small>

[Keyser Soze]

Nice test Stanfield, but is it really necessary to have you( i'm presuming its you) standing in the picture? Even with the bubble wrap over your face, the picture shows some of your features. And are the large pictures screwing up anyone elses page size?

[Mr Cool]

Nice test. I think it's a good idea to be in the picture to give a sense of scale.
But I must ask you to put the pictures somewhere else and link to them, as people on dial-up modems will have to wait a long time for this page to load!

[Flake2m]

[fag voice]Stanfield you look like a hunk! :p [/fag voice]
This test is impressive, especially the damage on the tree (I think it is an oak tree).

If you had been bothered to drill a hole into the tree (20mm would bet enough) and stuff the PETN into it before the det, you could have taken a chunk out of the tree!

[Mr Cool]

That's better. I've changed them to links, and the page loads much faster.

[stanfield]

thanx Mr Cool !

No ! it's not me on picture (I'm not crazy !) ! it's a friend (my lab assistant :) )

The sound was amazing, I made a timer with 3min 41sec, during the countdown, we ran about 400-500m ! even so, BAAAAAAAAAAM !

But next time I'll put the PETN in a pipe to increase damages... or drill a hole in the tree. (it was a "hard wood", so the damages aren't very important...)
One day, I'll try with a Linear Shape Charge to see the difference !

Next test, 100g of PETN ! <img border="0" title="" alt="[Eek!]" src="eek.gif" />

[DBSP]

OT. Stanfield would you mind sending me some info on the timer to my mail?.

Nice pics, why don't you do as you said and drill a hole in a smaller tree next time, that way it should fet cut off, adding to the display. Try a tree about 20cm in diameter.

[mongo blongo]

I have seen many references to "Jumala's Timer" but I can't seem to find any info on it either. Is it in one of the archives?

[Mr Cool]

Maybe there's a schematic on the FTP? It's worth having a look.

[stanfield]

20 cm in diameter is too small !
I want to kill a big tree :D !

huh... Jumala sent the schematics of his NEW Timer to me but I think he never published these on the web. On his webpage (when it worked), there only was the schema of its OLD Timer... by consequences, the schematics of his new timer never met public and maybe I'm not authorized to publish them... until he gives me permission, I'll never publish them, it's HIS work...

anyway, here are his old timer wich is based on the same CMOS4541 and is very similar...:
<img src="http://perso.wanadoo.fr/stanfield/Timer_Jumala.JPG" alt=" - " />
(68Kb, is it allright this time ? :) )
what's better ?
- drill a hole and fill it with 50g PETN
- or a linear shaped charge ?

thanx !

<small>[ March 02, 2003, 04:46 PM: Message edited by: stanfield ]</small>

[DBSP]

Just remembered this pic that illustrates how powerfull PETN is, in the pic below you see what kind of damage a 140g APAN charge does on a tree, not the same kind of tree but still. The charge was held in a piece of a wine bottle, the 700ml kind.

<a href="http://dbsp.sensorystatic.com/pictures/140g_APAN_charge.JPG" target="_blank">http://dbsp.sensorystatic.com/pictures/140g_APAN_charge.JPG</a>
<a href="http://dbsp.sensorystatic.com/pictures/result_of_140g_APAN.JPG" target="_blank">http://dbsp.sensorystatic.com/pictures/result_of_140g_APAN.JPG</a>

This was 140g of APAN, you only had about 50g of PETN, notice the differens in power ?

(pics might not still be up, just wait they will be up soon)

Drill a hole, the tree sustaines more damage if "hit" from the inside than from an LSC from the outside(I think so at least).

Realised I allready have the schematics of that timer. Thanks anyway.

<small>[ March 03, 2003, 12:38 PM: Message edited by: DBSP ]</small>

[Mr Cool]

Try a LSC Stanfield, it'd be much more interesting and just as much fun, also more useful to others if it worked well. Placing a charge inside the tree will create more damage, but I still think a LSC would be better.

[ShockWave]

Nice stuff that PETN, but I had expected much more damage.

But very nice pics.

What a waste of the electric timer and battery's, if you were using about 2 meters wire connected to the timer and the primary and than placing the timer behind the tree, you would still have a great timer.

But I must say, doing it your way looks more impressive, more dangerous :D :D

[stanfield]

Yeah, the stress was intense ! I always have fear that the Timer bugs in my hands ! but Jumala is the master in electronic and his timer is VERY reliable.

by looking at these pic :
<a href="http://dbsp.sensorystatic.com/pictures/140g_APAN_charge.JPG" target="_blank">http://dbsp.sensorystatic.com/pictures/140g_APAN_charge.JPG</a>
<a href="http://dbsp.sensorystatic.com/pictures/result_of_140g_APAN.JPG" target="_blank">http://dbsp.sensorystatic.com/pictures/result_of_140g_APAN.JPG</a>
I realized that PETN is extremely powerful... At the explosion site, I was disapointed because I though the damages would be more important but when I'm seeing theses APAN pictures, I'm amazed by my PETN explosion :)

The timer (with battery) cost me 3-4€ (3-4$), I always buy big quantities of electronics components so the prices decreases... I've bought 100 9V battery for 20€ ! :)

other question :
For Christmas I've bought a digital camera (you saw !), there is a video function (10 pictures/sec), so, what will happend if I left my camera on the explosion site, at 10m (for example) ? Will it be broken by the shockwave or will it be insensitive ?

thanx for all and apologize my bad english...

[ShockWave]

that's why you can use 2 or 3 meters wire to make sure if the timer is making a error or something that you are not dead, you also can use 10 or 15 meters wire, maybe the timer is not expensive but i'll guess that it takes a few hours to build the whole thing.

I don't see a difference between the damage of 140gr apan and 50gr petn, except that the damage of the apan is much bigger, strange.

I also have that 10pics/sec function, but how do you want to press the button at 10meters ?!

at 10 meters the camera will not break, but the change is very small that you get a pic of the explosion, only if you are lucky.

[stanfield]

nonono, it's a real "video" function but instead of a video at 60fps, my camera got 10fps ! :p Yeah maybe "FPS" is better than "picture"...

see ya !

<small>[ March 03, 2003, 04:23 PM: Message edited by: stanfield ]</small>

[Jumala]

Hallo Stanfield,
very interesting pictures. I saw you put the timer and the batteries on the charge. Off coarse this works but you loose always the equipment. Perhaps you can put the timer/batteries behind the tree/target then you can pick it up for future use after the job.

I have uploaded the timer plans and a 12V -&gt; 250V transformer plan to the FTP Upload folder.

PETN is very good for making caps. Do you ever tested a cap made from PETN and fine perchlorate/Al flash. Since wantsonfet has detonated ANNM with 4g flash it should be no problem to do the same with PETN. This would give detonators without dangerous primarys like leadazide or DDNP.
I will mail you some pics about my idea of though caps.

[kingspaz]

i think the problem with flash for base charge initiation is its reliability.

[stanfield]

my detonators are made by 1g of PETN and 0.1/0.2g of lead azide.
Lead azide is very stable when pressed ! I never had any problem with it !

By the way, I can't download your files !

COMMAND:&gt; RETR transformer 12v - 250v.jpg
550 Permission denied.
ERROR:&gt; Requested action not taken (e.g., file or directory not found, no access).

see ya !

<small>[ March 03, 2003, 05:49 PM: Message edited by: stanfield ]</small>

[shooter3]

Stanfield. Formula for external charge; DxD/40. Formula for internal and stemmed charge; DxD/250.

D is in inches.

Charge is in pounds.

20 inch tree external charge; 20x20=400/40=10 pounds of explosive.

20 inch tree internal charge; 20x20=400/250=1.6 pounds.

[stanfield]

This tree was about 60cm in diameter so about 23 inch... I found I need 13 pound of explosive, so about 6 kilo of explosive ! right ? it's huge...

and for internal charge, 2.23 pound of explosive ?
1kilo ? it's huge too, no ?

thanx anyway :)

[Microtek]

Note that if those formulas are from army field manuals, the charge weight is in pounds of TNT so you need to divide by the relative effectiveness for PETN ( about 1.6 I think ) and also note that army formulas tend to use a little more explosive than neccessary ( so they are certain the tree/bridge/bunker will be destroyed ).
If you primed the charge at the surface touching the timer, the effect would have been greater; the part of the explosive that is between the detonator and the timer might as well not have been there, and the shockwave did not impinge directly on the target.

[stanfield]

argh... it's hard to understand :)
May you make a draw please ?

thanx.

<small>[ March 04, 2003, 11:58 AM: Message edited by: stanfield ]</small>

[DBSP]

Shockwave, the hole point is that the damage is about equal between the PETN and the APAN, only that it was 50g of PETN and 140g of APAN!!!

Could someone please send me the timer scematics(new one), I can't get my FTP account to work so I haven't been able to download anything since the system with personal accounts where introduced.

Thanks in advance.

[Chainsaw]

Hi! haven't had time to talk here for a while... like 2 years :)

What do you people tell chem supplier when you buy PE? They do ask what you are going to do with it, don't they? I mean there is no reason for ordinary people to obtain it.

"The chemical is used as intermediate for Alkyd resin, Rosin ester, Explosive and Lubricants. No consumer use is reported."

Well... which reason should i pick? Lubricants? :p

<small>[ March 12, 2003, 07:54 PM: Message edited by: Chainsaw ]</small>

[kingspaz]

do a little research into why its used in resins. see, you're doing some independant research into resins <img border="0" title="" alt="[Wink]" src="wink.gif" />

[stanfield]

A few days ago, I made a batch of PETN with 400g of Pentaerythritol and 1700 mL of 98% nitric acid. I obtained the amazing yield of 913,8g of PETN ! (I took some photos, if someone is interested...)

An today, I detonated 75g of it on a big rock !
http://stanfield.150m.com/75g_petn.htm Here are the results

give me yout opinion

I tried to blast the tree again but the hole I've dug is too little... I'll have to enlarge it later !

bye !

------------
fixed link - kingspaz

[bonnsgeo]

Very impressive stan :) !!

do you have an idea of the density of Petn in your putty ?

bye

[stanfield]

It's very well pressed...
When your are wrapping the PETN into the plastic foil you're able to very well press the PETN, Give it a try and you'll see.

[ZaphodB]

Does anyone know whether you can use polyisobutylene as a plasticizer for PETN? A friend of mine has got 120g of polyisobutylene over eBay and he wants to use it with his PETN (~1kg).
(We're going to use only ~500g first, set off by HMTD-and we'll try to get it on tape.)
Has anyone here ever used polyisobutylene as a plasticizer?

[bonnsgeo]

i never used really polyisobutylene but i used yellow-tack to extract an equivalent of pib + adipate mixture.
it worked not very well for me.

i used too a "self amalgamating tape" made with pib and it worked not too bad.

i used both with petn. (rdx is too expensive to make for me)

In all case pib is a great binder. You must add di ethyl hexyl adipate or sebacate to plasticize your polyisobutylene.

good luck.
...polyisobutylene on Ebay ...lol ...good joke :D

[ZaphodB]

Not a joke ...

The stuff my friend has got was pure, though ...

http://cgi.ebay.de/ws/eBayISAPI.dll?ViewItem&item=2318751888&category=30522

Even if you don't understand what is said in the text, you'll see where it says Polyisobutylen - this is available in the Home Improvement section. :D

[bonnsgeo]

oh ok ! it's self amalgamating tape !!!

its not really pure pib. (pure pib is white)

tape is very hard to dissolve.
but it works a little.

the results is soft black piece of rubber but it break it easily. and it doesnt stick to anything. :rolleyes:

bye

[bonnsgeo]

Hello.

I have some problems for making explosive plastic because of the size of my PETN crystals.

I read on different patents that the ideal size is less than 100 microns.
I read too that Rdx and hmx are the most used for pbx because the size of crystals are very little contrary to petn.

Do you have an idea how to reduce the size of my petn crystal ? i know recristallisation in acetone with adding lot of water is good , but do you have an other way to make fine crystals ?


bye

[Microtek]

How about putting a suspension of PETN in water in a blender and blending it for a while. I think I saw an article along those lines.

[Argy]

Hum, i read a post (i don't remember who posted it) about the recrystalisation, the process was used for RDX, you must add 500g of RDX and some gelatin in 5L of water and then put it on a magnetic stirrer while the water evaporation, when the bigger part of the water have been evaporate then you can use a hair dryer (not sure about this word) i think that's should work with PETN too, as Microtek say ;)

PS : Sorry for my bad english :(

EDIT : I forgot to say ... this process is used for plasticize the RDX with PIB (C-4)

[Bitter]

Rapid cooling produces the finest crystals, so if you are going to attempt recrystalisation, make sure the liquid you are dunking it in is as cold as you can get it.

[stanfield]

When I heated my 900g of PETN in 3L of acetone, I then dumped the liquid in 10L of cold water, the final powder I've obtained is really fine ! The crystals seems to be very small, smaller than the first times I've tried to make PETN. The first time I made PETN, I waited the aceton to cool to 25°C and then dumped = this is not good !

[kingspaz]

the quicker you precipitate the crystals the smaller they form. this holds true for most situations.

therefore, if you made a saturated boiling solution of PETN in acetone and dumped it onto a large excess of ice at the lowest temperature easily obtainable (-20*C - deep freeze setting?) then it should precipitate extremely fast and be very fine. plus PETN is a nitric ester so dumping it into cold water with some detergent in should have the same effect.

[BLASTER]

Verified efficient method of preparing PETN from diluted HNO3

use
32,7 ml of 70% HNO3 (75% excess)
18,9 ml of 96% H2SO4
10,0 g of Pentaerythrite
------------------------

or
34,0 ml of 65% HNO3 (66% excess)
24,8 ml of 96% H2SO4
10,0 g of Pentaerythrite
------------------------

or
34,8 ml of 58% HNO3 (48% excess)
36,3 ml of 96% H2SO4
10,0 g of Pentaerythrite
------------------------


Nitration:
1. Cool nitration mixture during mixing of acids, thus minimalize even minimal decomposition of HNO3. Nitration mixture must be cooled before nitration process to temperature of 10°C.
2. While stiring, add pentaerythritee in small portions (1-2g) to nitration mixture, always after previous batch is dissolved. Nitration mixture gradually thicken as PETN forming in solution.
3. Constantly monitor reaction temperature and maintain it in 10-15°C range. Interval of adding pentaerytritol conform to reaction temperature, must not rise over 15°C, leave beaker in cold water.
4. Stir with mixture for next 5 minutes after all pentaerythrite is added and dissolved. Mixture is now thick, but stirring is going well. During nitration process must not be developed any brown fumes of NOx!
5. Now put beaker with mixture into water bath and maintain temperature at 50°C, continuously stir with mixture. During 20 minutes at this temperature, all of possible sulfoesters come into PETN for maximal yield of nitration.
6. While maintaining mixture at higher temperature, mixture must be monitored for developing of NOx fumes. Only light brown colour can be in shrouded beaker. Raised development of NOx pointing to higher temperatures used (even during previous nitration) or insufficient chmemicals purity and further heating may end up in uncontrolled reaction and oxidation of formed PETN. In this case it is better to do not heat at all and end just after nitration (if brown fumes apperas during nitration), the yield will be lower. In case of accidentally runaway reaction during heating, immedialtely pour mixture into cold water, don't try stop reaction by cooling beaker, it will not help.
7. When heating after 20 minutes pass off, pour reaction mixture into cold water and follow standart procedure of filtration, neutralization and purifying of PETN.

Yield was 22,1g of PETN from 10g of pentaerythrite, ~95% of theoretical yield (with 65% HNO3 used).

This procedure is result of my research of most effective method preparing PETN from diluted HNO3. Acid ratios are precisely calculated on data from PETN nitration graph published by T. Urbanski in his book vol. IV. Generaly said, PETN is forming to maximum 30% of water portion in nitration mixture. But, when also H2SO4 is contained in nitration mixture, minimum ammount of water must be keep, or oxidation with small yields occur. With this acid ratios 20% of H2O is minimum. So, this nitration mixture has 20% of water on nitration start and 30% at the end, area for most effective nitration, but again only with this ratios. For other acid ratios must be all recalculated. Excess of HNO3 is used to controll ammount of reaction water. Only ammount of nitration mixture can be extended for lower mixture thickness, but it lower utilization of acids and overall efficiency. But it isn't necessary.

I hope there is no major mistakes in my translation to english ;-)

[stanfield]

yes, but PETN made from sulfuric acid is harder to purify... Use at your own risk !

see ya !

[BLASTER]

Not definitely true, initially contains more acid, but after careful neutralization and recrystalization from acetone, you will stop at same finite ammount of residual acid. Look at couple of patents about preparing/purifying PETN. Almost no acid remains only after special methods (mixing with other liquid or melted nitroesters). Limiting factor of final purity is not initial ammount of acid, but finite residual ammount which always reamins almost same after recrystalization from acetone, regardles of preparation method used.

[stanfield]

so, I trust you !
but I only have 58% nitric acid here... In all case, I must distill my acid. So, the waste of time is the same !

[BLASTER]

Only 58%? What a shame ;-) 65% is standart here for HNO3 (btw some people says that 70% is commonly available, but depends on area). But no problem, I've just make calculations of ratios needed for your available HNO3.

[stanfield]

Don't bug you. :)
I have a big 5L distillation apparatus. Obtaining 98% nitric acid is a piece of cake for me !

thanx anyway.

Oh! by the way, how do you make your calculations to know exactly what amount of sulfuric you need with you dilute nitric acid ?

[BLASTER]

I've edited previous post with preparation, added recalculated amounts for HNO3 of concentrations.
Calculating is done by trial and error, you must find optimal ratio between HNO3/H2SO4/H2O in nitration mixture, while looking in Urbanski graph, if resulting ratios of nitration mixture fall in optimal nitration area. Of course you must observe also ratios of mixture at end of nitration, when reaction watter is added to water contained previously only in acids. Also resulting acid ratios must be prepareable with acids of concentrations you want to use. Sounds really complicated, but I've done excell spreadsheet for this purpose, so I only tuning initial values and immediately see results and compare in graph. Then I use other spreadsheet specially for nitration mixture ratios calculation and look if it is possible to prepare with assumed acids, if not, slightly adjust initial ratios and again verify results.

[stanfield]

hehehe, doing a trial for me is longer than making 1L of nitric acid at 98% ! :)
thanx anyway, I think this is usefull for lot of people.:o

[Mr Cool]

It'll be useful for me if it works like you said! Though I think I might not heat it all the way to 50*C, and let it react a little longer instead...

[BLASTER]

Preparation method is wrote exactly as I prepared PETN in real, I recommending to follow it in all details, then you can compare if want to make something different way. Heating is safe, if you just follow all instructions. Danger of oxidation exist in case you dont strictly follow instructions and ratios (specially temperatures and times).

[Mr Cool]

I'm posting this for BLASTER, since he is unable to do so.

http://www.boomspeed.com/mrcool/PETNGraph.jpg

"Area I - Formation of PETN with yield of 94-98% without formation
of sulfoesters. Area II - Formation of PETN via sulfoesters.
Area III - Area of low yields (10-50%) due to the high NOx
production and oxidation processes Area IV - PETN not forming"

[simply RED]

What are the numbers on the bottom of the graphic?

[BLASTER]

Bottom line is percentage ratio of HNO3 in nitration mixture.

[simply RED]

Can you explain how the graphic is read. I am staring for half na hour and still can't understand...

[bonnsgeo]

i think to heat the mixture of H2so4+ hno3 at 50 °C is really dangerous and useless.

I ALWAYS do my petn by this way (cause i cant get (or make) nitric at 99%) and i NEVER heat the mixture.

i keep it at 10 / 15 °C (never more) and i wait for 10 minutes after all the PE was added (in little quantities) and i often obtain 95 % of yield.

Don't heat !

[stanfield]

you'd better wait 20-30 min in order to get a full esterification... that's not dangerous !

see ya !

[Mr Cool]

bonnsgeo, what ratios do you use?

[bonnsgeo]

Last day i did petn for making some plastic explosive and i used:
42 ml of HNO3 at 67.6 % (density = 1.41 ; equivalent to 40grams of pure hno3)
then i added 30 ml of H2so4 at 98 %. (density 1.83).
the temperature never go up than 15 degre celsius , never !

i know that with 40g of hno3 i could make more petn but the solution become very thick , my magnetic stirrer cant turn (at the end) because of that .

then i nitrated 10 grams of PE and i obtained 19g of petn (bad yield this time but i lost some petn during my recristalisation because my bottle falled but i always obtain around 94 / 95 % of yield after recristalisation in acetone)
bye

[Argy]

Thanks BLASTER your posts will be usefull for me because i can get 95%+ HNO3 but it take me a lot of time and it's realy boring ;) your method look better :D

Just an information for the guys who can't find pentaerythritol, there is a laxative medicine called Auxitrans 5g witch is sell in france without medical prescription and it contain 5g of PURE Pentaerythritol, so i think it'll be nice for PETN ;)

Maybe there is something like it in others country

[Mr Cool]

Very interesting, Argy! So, PE is OTC after all :).
And thanks for the ratios, bonnsgeo and BLASTER.

[Arthis]

Hum, noob question, but OTC stands for what ?

[zaibatsu]

OTC = Over The Counter?

[Argy]

At the moment, i didn't try to make PETN with this medicine but i'll try it soon, then i'll give you the results (anyways i'm sure it will work since my "Vidal" book with composition of medicines told me that is pure pentaerythritol) :D and there is an advantage with buying pentaerythritol in this form : if you have a medical prescription you get 35% money back from social security (I love my country hehe :p )

[BLASTER]

Explanation of graph picture reading posted above. From left H2SO4 axis point right-down diagonaly, from bottom HNO3 axis point right-up diagonaly. In crosspoint you got amount of H2O readed horizontaly from right axis. Crosspoint stays in area of actual nitration mixture reaction properties. Of course, you can start from and follow any axis you want. Hint: if you not found specific ammount of acid on axis, for example 40% of H2SO4, point left-up diagonaly from oposite HNO3 mixture ratio without water (60%) and this line points from 40% of H2SO4.

[Arthis]

I'm a bit puzzled...
The graphic means that if you don't have access to highly concentrated nitric acid, let's say you have 58%, if't better to dilute your sulfuric acid, then it will work ?
I don't understand why mixing low conc. NA with high conc. sulfuric acid will result in a low yield. After having mixed the acids, the number of moles of NA, SA and water are the same in the solution, if you make the equivalence with the concentrations you have. The only difference I actually see is the problem of the decomposition of NA in NOx gas. But then you would just need to gently mix them to avoid the decomposition. The graphic does not precise that.
Where's the problem so ? Can someone explain me ? (if you understand what I said, it's not really clear... sorry for that).

[BLASTER]

The key is ratio of HNO3/H2SO4 and H2O in nitration mixture. First we need mixture with H2O ratio at maximaly 30%, it means if we want to use HNO3 alone, it must be at least 70% theoreticaly, or, we can use almost 100% H2SO4 to lower water ratio in mixture. Next thing, if we use H2SO4 in mixture to lower water ratio, we must also observe minimal amount of water, because mixture with H2SO4 and water content below 30% (for specific H2SO4/HNO3 ratios) is highly oxidating to pentaerytritol. So, you must count for water ratio to volume of final mixture, not for acids alone. Keep in mind that this ratios will change during nitration, because of dilution by water formed from nitration of PE. Most efficient is, when nitration mixture water content change during nitration from minimum (20%) at oxidation level to maximum (30%) where PETN will forming at end of nitration.

[Argy]

Today i tryed your method Blaster (58% nitric) all was right i added the pentaerythritol i stired well and i get a pasty mixture... then i heated my becher but when i get over 30° C, i get a big production of NOx, all my mixture became black and i had to throw it fast into water, i lost all my PETN :( i'm sad and NOx is realy toxic, impossible to breathe at 2m of the becher (and i only had 70ml of acids in my mixture!) bahhh i'll try again without heating! but tomorrow :p

[bonnsgeo]

arghhh crazy man !

read correctly : DONT HEAT !!!!

[Arthis]

In the post of Blaster, it's said you need to heat the beaker, after having added the PE, to 50°C.
So where's the confusion ?

[Argy]

I was going to heat the beaker at 50° but i didn't get over 30° C :(

[Argy]

I re-tryed to make PETN with 58% nitric acid + pur sulfuric acid but without heating, i stired a very long time instead and now it's in my bunchner funnel, it's seams to be PETN, but i'll have to test it to say if it work well =)

[bonnsgeo]

Dont heat. its dangerous and useless !!

just wait 20 min after the last add of PE.


to know if its petn or not there 3 easy ways: 1)petn dissolve in acetone (not pe)
2)you must have more petn (in mass) than pe. example for 10 g of pe you should have around 20/22g (23.2 in theory). 3)Pe dissolve (slowly) in water ..not petn.

and detonation :)

[BLASTER]

Argy: did you cooled mixture while nitrating below 15°C? Also low purity of PE and free NOx in HNO3 can cause oxidation.
What I can said is, that heating should maximize yield, but of course you got some PENT without heating too. Next, I've tested actualy preparation with 65% HNO3, maybe I'll try acid diluted to 58%. One time I also ended with brown fumes everywhere, but it was due to higher temperatures while nitrating (20-25°C), everything fine, but heating after 15 minutes ended in oxidation. also next important thing is continuous stirring of mixture all time.

[Argy]

My PE was 100% pur and the temp while nitration was under 10° :(

[Argy]

Yehhh i have dry PETN now! :-D and i get it with your method BLASTER (without heating) and 58% acid, i'm sure it's PETN because i dilluted it in acetone greatly, it's a lot of work to get pure, dry and with small cristals PETN, but it's realy great now it's like dust and i'm realy happy. thanks again Blaster! :D

[PyroTech]

Argy, I can get the same percentage HNO3, could you post how much H2SO4, HNO3 and PE you used? And how many grams of PETN came off?

Thanks!

[Argy]

I used 102ml of 58% nitric acid with 108ml of sulfuric acid (95-99%) i added 30g of PE and i will tell you how much PETN i get tomorow because at the moment it's in my funrace for perfect drying ;p but i get really more PETN than PE.

[Argy]

I made PETN again, with 20g of PE and the total weight of my PETN is higher than 100g (the first time i used 30g of PE and the second time 20g) so the yeild after recrystalisation drying etc is higher than 200% (compared to the mass of PE)

[rooster]

argy, you never count yield that way. Yields are always between 0% and 100%, and are measured out from how many moles PE you used, and how many moles PETN you got. I think the weight in a 100% yield reaction for PETN is something like 1gram PE to 2,2grams PETN. So, I'd say you got around 90% yield.

[kingspaz]

rooster, you have no right to tell people off for calculating yields when you do it wrong yourself. calculating 'yields' your way is next to useless as it provides no information on how efficient the reaction was.

yields are actually calculated by taking the number of moles of product obtained and dividing it by the number of moles of product the equation predicts. you therefore get a measure of the amount you obtained as a percentage of the maximum possible amount you could have obtained.

[Arthis]

100+ g of PETN for 50 g PE means a ratio over 87%, that is great. Still using the method you told a few days ago ?

[Argy]

Yes i used this method with 58% nitric acid but i lost PETN during the 3 filtrations, dissolution in acetone, drying, etc :-p

Next time i'll try with 68% nitric acid but 1L is about 7$ for me (58 is about 3-4$) :( by the way 1L is enough for a lot of PETN :cool:

[rooster]

sorry for the wrong info, arthis... U can see what alcohol deos to you...

Thanks for the correction kingspaz

[Argy]

I'm sorry, my calculations was based on the weight, but next time i'll do it as you said.

[kingspaz]

you can use moles or weight since the resultant fraction is the same. you just have to make sure you divide the amount of product you got (moles or grams) by the amount of product you should get (in the same measurement as the experimental product) then multiply by 100. using mass is easier because you don't have to work it out, just simply measure it.

[BLASTER]

For those who don't believe in heating of PETN mixture after nitration, I've done nitration batch of 20g PE with my method, from 65% HNO3, but, not heated, only stay for 30 minutes at 10-15°C.

Initial ammount of PE used: 20g
Theorethical ammount of PETN: 46,4g
Ammount of prepared PETN without heating: 38.9g
Final yield without heating: ~84%

Previous yields with mixture heated: 95%

So, aditional more than 10% of PETN can be obtained by heating mixture after nitration.

Key to success is at first place right ammount of reagents, then reaction temperatures and times and of course STIRRING of mixture, while heating, it must be continuously stirred!

[bonnsgeo]

So you were unlucky.

I obtained lot of times around 94/95 % of yield and i never heated something !

Just be careful.

bye.

[BLASTER]

bonnsgeo: may be, but you wrote nothing about concentration of HNO3 you used, did you make it with 65% HNO3?

[bonnsgeo]

i said (on previous page) than i use 67.5 % HNO3 and 98 % sulfuric acid.
the ratios i use are on the previous page.

bye

[Argy]

I get more than 84% with 58% nitric acid only, i didn't heated but i waited for about 30mn with stirring, the temperature was over 20°C, i think i should heat but not over 35°C until my mixture get yellow (in my experience, when the mixture become dark, you MUST stop nitration, if you don't then you'll get a run away reaction in the following minutes :p )

[DBSP]

I made a batch of PETN for the first time two days ago.

I used 35ml of 62% HNO3, 25ml of 96% H2SO4 and 10g of PE.

I prepared an icebath and chilled the mixed acids down then slowly added the PE, But since the temp didn't even rise above 0* while adding I added the lot and continiued to stirr constantly. After a hile the temp had gotten to 10*. I then removed the beaker from the icebath and continiued stirring, After an hour with continius stirring the temp had gotten to 25* I then poured it off into 500ml of cold water and filtered it.

Dissolved it inhot acetone and neutralized it with NaHCo3, filtered the solution and dumped it into 300ml of cold water, filtered and spread it out to dry. Last night I weighted it, it still seemed a bit damp. A couple of hours ago I weighted it again and it still weighed the same (20g) and still felt the same.

Does PETN seemeto be be a bit damp even when dry? I don't know because I have never made it before.

Anyway to be the first time i make it I'm satisfied with a 81-91% yield. My scale is only +/- 1g accurate, thats why I'm not shure of the yield. Might try heating it a bit next time I make it.

I would be grateful if I could get an answer before saturday because I'm going on a holiday to a place wher it is perfect for some serious blasting, thus I'd like to know if my PETN is OK.

Btw the temp is about 25* C round the clock at the place the PETN is dried.

[Argeleb Elb]

My PETN isn't damp at all, i make it dry with my furnace (50-70°C). :)

[BLASTER]

PETN is like damp after only washing/cold neutralising, it contains acid and even if you wash it to neutral, when dried after short time it will go acidic, just put pH paper into your PETN. It will turn purple.
When I make PETN, after few washing to neutral I put it into beaker with water to make suspension and then heating it in water bath to 80°C. Shortly after start heating, suspension will turn acidic, then I neutralize it with diluted amonnia (NH4OH) to neutral and do it periodicaly for some 20-30 minutes. After that time suspension stays neutral. Let it cool, wash few times, filter and dry it.
It's easy step and significantly improve quality of PETN. Anyway, for log term storage or blasting cap use I recommendig aditional recrystalization from acetone. But for immediate use is described neutralization enough.

btw you should use more H2SO4 (not HNO3) when less concetrated HNO3 is used to bond additional ammount of water and then incease nitration mixture to PE ratio. Anyway your yield looks good.

[Mr Cool]

In what way did it seem a bit damp - clumping together, felt cool to the touch..?

[DBSP]

It felt a bit damp, it was a bit clumpy and when I took a small pinch of it between my fingers it didn't fall appart like AP but was rather smeared out. Anyway a bit water in the PETN is said to increase the VOD so it probably doesn't matter.

[Anthony]

I remember my PETN being like that, I just attributed it to being a very fine powder, flour is very similar IME.

[DBSP]

I just got back from my vacation. I've got 11 new vids and a whole bunch of pics.

I've used the PETN pressed into .22WM shells by hand with a .22LR shell with AP pressed into the end of the WM shell making a perfect det. The first time I detonated one of these caps I was amazed by the power of PETN. The caps have all worked great and no duds.

I've just made this my standard det. [proud of myself, allthough a bit tired now scince I've just driven 1000km with only 2h of sleep]

[xabxulu]

Today I have done two tests of homemade detonators with PETN, detonated with silver double salts. For the first one, I went in country (I have some neightbors who have another "funny-sense" than me ;) ) and the PETN didn't went off (not enough double salts I think). So, I decided (stupidly... Very stupidly !!) to do the second test at home...... with more double salts......... --> BOOM !!!!! I had never eard an explosion like this with less than 1 gram of explosive (without double salts). That's really amazing, and I decided to take some "hollidays" to calm down my street :)

[Omogen]

DBSP i saw you asked something about the nitration of PE.
I found a nitration guide in the swedish compilation pyrokemi2k.

Since my english is very bad it would take days to translate the guide to english but if there are some other user here that really would like to know how to make PE i can make a sacrifice.

Although im not so sure if the acetaldehyde is easy to obtain. I ran some searches on it and it seems like its the substance that gives you a hangover. By that i guess it means that its toxic and therefore quite hard to find.

Gimme some replies if you would like to know the nitration.


oh right...DBSP since im from sweden i wondered where you obtain Nitric/sulphuric acids.

The method by going through the battery for obtaining sulphuric acid and after that nitric acid is quite hard since i havent a vaccum destiller.

[Efraim_barkbit]

Omogen, you can get sulphuric (96%) and nitric(62%) acid if you go to denmark and have a look around in MATAS shops. It is a chain of beauty shops that also sell some chemicals.
not all of them has the same assortment, and I had to go to seven or eight shops to find the sulphuric when I was there last month.
I am thinking about making some nitrocellulose soon, to get the hang of nitrations, and then I want to try something more "serious". I would try PETN if I could get PE, (how did you get it DBSP??) but I think I´ll give RDX a try, but it seems to be a little more difficult.

EDIT: wasn´t sure if a word really existed in english, so I deleted it

EDIT2: explanation of edit no1

[Omogen]

yeah well...its a long way to danemark from stockholm and to travel all that way just to get ahold of acid is pretty weak IMO. But maybe thats the only way to get ahold of it.

The simplies way is to borrow some acid from school i guess.

[FrankRizzo]

Is PE still available in the US in less than MT quantities? I know Pyrotek used to carry it, but it seems its been discontinued. Any help would be greatly appreciated.

[DBSP]

There are several threads that deals with PE and where to find it. Have a look -->here<--- (http://www.roguesci.org/theforum/search.php?s=&action=showresults&searchid=16823&sortby=lastpost&sortorder=descending) for instance.

This thread is about PETN and not PE so try to keep it that way, especially when thare are threads about PE alone.

[IPN]

SWIM had his first experience in PETN this week.

SWIM made some PETN with BLASTER's method using 34ml 68% nitric acid, 25ml 98% H2SO4 and 10g PE (from acros).
Yield was 22g after recrystallization from acetone.

12g were pressed to a paper tube and 1g HTMD was placed on it and the tube was then sealed well. The charge was buried under 10cm dirt and a ~8kg rock was placed on the dirt.
After detonation the rock had moved approx. 5m

PETN rocks!!!:D

Pictures of the test can be found here:
http://koti.mbnet.fi/otto2000/Kuvia/

(Sorry for the big file size)

[Hubert]

Hey
35ml HNO3
25ml H2SO4
10g PE

Tmperature of HNO3+H2SO4 was 5*C, and I put 10g of PE time 15min, and I stirring with ma hand 30s for 1-2 min. Temperature was 10-17*C
After I added my PE, I continue stirring (120/1 obr/min) for 35min.

I have 12g of PETN :mad: Where is the problem??

[DBSP]

What was the conc. of your acids?

Read my reply a bit up on this page, I let my PE nitrate for about an hour with constant stirring with the temp rising from about 5* to about 25* after an hour. I got 20g of of PETN at least.

Would be interesting to now the conc. of your acids, it might be the problem. Reacting it a bit longer wouldn't hurt either.

[Hubert]

hey
I m very unhappy :(

My acids was:
HNO3 65% (Technical 94%)
H2SO4 95% (Technical 94%)

Technical acids is very cheap ~7,5 dolars 20l

When I make my PETN with KNO3 and H2SO4 my yeild was 4g PETN (2,5g PE)
Maby i make with more PE my yeild was more larger


--------
Today I make some PETN and I very angry because I get only 5g PETN from 5g PE :(.

I milled PE.
I make 17,5ml HNO3 65%, 12,5ml H2SO4, and 5g PE.

1.I coled acids to 5*C, and I added 5g PE. temperature was 7-16*C, Whole time I mixed (it was 15min)
2.The mixture was white, max temperatur was 16*C for short time 1-2min, no longer.
3.I stirring mixtur over 1h (one hour) temp. was 8-15*C.
4.Next I added mixture acids and PE to 500ml coold water (H2O- 10*C with ice), and filter.

Maby I most heating to 25*C or 35-50*C as in metod BLASTER.
Maby H2SO4 ist to little and much water ???
I fulfiled all requirements, maybe about something I forgot ???
This acids ist problem ??? (technical)

When I make 20g PETN (10gPE) i celebrate this :D.

I'm sorry behind my English, I learn still :)

I make ma PETN with heating maby this metod is beter for my.

[BLASTER]

no heating AFTER PE+acids reaction -> poor PETN yield (no more than 50-60%)

let the mixture to react at least few minutes before heating, very good mixing required!

[Hubert]

Please look in this link
www.snop.piwko.pl/petn.rar this is PDF file , synthes of PETN with some pictures.
I finde my problem, my HNO3 was only 55%.
Thanks for helping :D

Check your post after you post it and make shure you don't double post. I deleted your second duplicate post.

DBSP..

[BLASTER]

Nice pdf, but there is mistake, ammounts of acids are substituted.
There should be 34ml of HNO3 and 25ml of H2SO4 (24.8ml exactly) and not contrary.

Final heating allow react unreacted PE, which unwillingly dissolve at low temperature in nitration mixture with suspension of forming PETN. This is key for high yields. For higher safety, nitration is made in two steps.
One must only watch for abnormal temperature rise of mixture while heating and maintain temperature at 50°C.

[Mendeleev]

I've never heard of an HE being manufactured with either very concentrated nitric acid or a mixture of semi-concentrated nitric and pure sulfuric acid, but the discussion got me wondering can other HE's be manufactured using either method, such as RDX, HMX, or NG? Also, concerning the discussion on binders way earlier in the thread, I would try some of that fix-a-flat stuff, it is liquid tire + aerosol in a can, used for fixing flat tires.

[MACE]

hi

I've made an excel-sheet to calculate acid ratios for blasters procedure. you can enter acid volumes, acid concentrations and quantity of PE. the result will be displyed as a red line in the urbanski graph. i'll hope this will help a bit

here is the link: http://people.freenet.de/MACE/petn2.rar

bye MACE

[BLASTER]

MACE: Great tool :-)
All: latest improvement in PETN preparation from mixed acids - dissolve all PE in nitric aid first, then add in small portions to sulfuric acid. Don't worry, just keep temperature below 30°C. No additional heating is requred, after all PE is added, wait few minutes while stirring and then dissolve mixture in water.

[MACE]

hi

@blaster
do you have any yields for your new procedure until now? i'am a little bit worried about the acid ratios and concentration at the begining of the sulfuric addition. i think there will be more than the critical 30% h2o in the reaction mix at this time and the produced petn will be oxydized.

bye

[BLASTER]

The big asset of this improvement is, that PE is completely disolved in time of reaction. This is useful, because PE dissolving very slowly in mixed acids. And next, PE never fetch up in oxidation acids mixture, because all PE is nitrated to PETN before this can happen.

PE+HNO3 must be added in small portions to H2SO4 !!! PETN then forming immediately. If you do it in reverse, nothing happen until about half of H2SO4 is added to PE+HNO3, then violend oxidation start and everything squirt out !!! (tested and proven)

I tried this method many times, while searching with friend (who invented this improvement) best reaction conditions. My yields was around 85%, but problem was in PE with low melting point (~180 deg).

[MACE]

hi

yes, the problem when adding the PE to an acid mix was that you always had a slury of PETN and unreacted PE in the solution never knowing if all the PE had reacted. do you cool yor mix while adding the PE HNO3 solution or do you control the temp just by the speed of addition? is there anything else to that i should know about this procedure? maybe i'll try it out next weekend (if my H2SO4 arrives this week) and post my results. my PE sould be better grade. an other reason for the lower yield could be the much H2SO4 at the beginning of the addition. if you do a calculation with my tool and input a high quantity of H2SO4 and a low quantity of HNO3 and PE you can see that the red line is in section II which means that some sulfo-esters are produced. only if you add more HNO3 PE mix the line would move into sction I.

bye MACE

[mp5]

Do somebody need Pentaerythritol?
Delivery to Germany and parts of Europe.
eMail to: mp5@gmx.de
http://members.tripod.com/teveten11/pe.html

[jim2]

I tried Blaster's new method last week and it worked very very well.The PE mixed with no problem what so ever never going over 10 * C .When adding to the h2so4 slowly the temp never went over 15* C. All the PE mixed-no over heating-no fumes- a white product- easy to work with and completed quickly.Yield was about 80%.

Blaster , again thanks for your testing and method.

[Zerox]

This is what I did:
cool 35ml of nitric acid to about 10c ,then add the pe(10g), stir untill theres no pe left. then slowly add the h2so4 keep the temp around 10-17c.. petn should form after all the h2so4 has mixed,and it should be pretty thick. then add 150ml of cool water .. fillter wash with bicarb then........done
the yield was about 17g, ok for me..


stupid thing why cant i detonate it..

[PhoeniX_KEA]

I ran accross the following statement on a Hexamine product description. I would like to follow up on the statement made here. Is the following possible? If so, how?
GENERAL DESCRIPTION

HEXAMETHYLENETETRAMINE (HEXAMINE) is a white crystalline powder with slight amine odor. Specific gravity is 1.27 at 25C .
HEXAMINE is soluble in water, alcohol, and chloroform, but insoluble in ether. Formaldehyde and ammonia yield methenamine, or hexamethylenetetramine, which is used as a urinary antiseptic.

Nitration of methenamine gives the explosive cyclonite, or RDX. Formaldehyde and acetaldehyde react with Hexamine in the presence of calcium hydroxide to give pentaerythritol, the tetranitrate of which is the explosive PETN.

[Mendeleev]

First of all this is the wrong thread, second of all we already knew that, there are about 10 threads about RDX. NBK should arrive soon...

[Not_Osama]

http://www.alibaba.com/catalog/10373906/PETN_pentaerythritol_tetranitrate.html
Theres no way it could possibly be this easy. Im sure there has to be some kind of catch.
BTW this same company is also selling CHEAP ammoniated dynamite...
Either ive died and gone to heaven or im missing somthing BIG!

[chemlab456]

Hello,

i am the guy who started the mannitol hexanitrat thread. Now I find out that MHN is a bad Primary. Now i use pre filled Caps with .7g PETN and i add on the top of those boostern a combination of 0,05g lead azide mixed and compared with .1g PETN in a special less friction container ( i worked on it over 3 days). My question how long can i store these boosters. They are really airtight (perhabs 0,01ml of air inside) and closed with pressed paper and isolating tape (I remove it befor using and add the electric ignitor, description see above).

And other thing, most of you say that they want to prevent larger crystalls, purify to get a safe Secondary like PETN but on the other hand some of you use a self made BP fuse in a very "senational" Blastingcap and some run around with a 450g batch full of AP (perhabs not neutralize) in a metallic coke-can with a short fuse? Why are these differences?

thanks for answers
sorry for my mistakes but i`ll learn it ....

[Bert]

And other thing, most of you say that they want to prevent larger crystalls, purify to get a safe Secondary like PETN but on the other hand some of you use a self made BP fuse in a very "senational" Blastingcap and some run around with a 450g batch full of AP (perhabs not neutralize) in a metallic coke-can with a short fuse? Why are these differences?


Heh heh... 'cause they heard that big crystals are dangerous, but it's so much fun to run around with a coke can full of AP. Especialy when you drop your cigarette into it while lighting your home made fused "sensational" blasting cap!

Purifying PETN is for long term storage stability...

This is OT, but-

The guy I learned to make AP from DELIBERATELY RECRYSTALIZES IT to fairly large crystals (1 - 5mm) because he uses it for miniature SFX shots in video and film work. He likes to load a single large crystal onto his glow plug igniter for the type of shots that you've probably seen in many movies and TV series. It's easier for him to just grab a single crystal the right size for his effects than weigh such tiny charges... He's over 60 and still has all his fingers. These single crystals deflagrate nicely, not blowing up his miniatures any more than he wants them to- I know Lead azide has the reputation for going off from crystal stresses, but somehow I don't think every primary (or secondary) has quite the same properties.

[chemlab456]

I always neutralize or recrystallize if possible, because i wont loose a finger or worser. But on the other hand some people recryst. their secondary but dont do the same at the primary. The primary is the weakiest member in the chain. Because that are Boosters and Electric igrnors a very important task for me. How long can i sore the pure PETN in these airtight container without any dangeraus??

[Bert]

How long can i sore the pure PETN in these airtight container without any dangeraus??

I have no idea how pure your product is, of course. Industrialy, PETN and products made with it properly are good for decade+. The primary would be the weakest link, as you noted.

[Myrol]

Today i made (probably) some PETN! I had dissolved 37g Ammonium nitrate in 55ml 96% Sulfuric Acid and mixed it slowly with 10g Pentaerythrite! The Problem: The Temperature does not rise very much! I was able to add the PE gram-wise without to much trouble! I started at 16°C after the addition of all PE it was at 25°C with no permanent chilling :confused: :eek: :o I let it stand for 5 minutes unchilled and the Temperature rise to 27°C, chilling was now necessary! I let it react out and dipped everything into warm water....neutralization...filter everything out and now drying :) The Test with Acetone shows the result (when its dry!).Oh man I hope I did no Bullshit with wasting good chemicals :rolleyes:

[Myrol]

Harhar....today I made around 110g PETN with 111ml 98% Nitric Acid and 10ml 96% Sulfuric Acid! I weighted the 111ml with my scale and she says exactly 167,1g! Thats a quality of 98% looked up from a PETN.xls document! I did some calculations with the Program and found out this great ratio for Acids to Nitrate 55g Pentaerythritol! So I chilled the mixed Acids and spent the PE slowly to the mixture! The Problem: After adding 48g I was something to hastily and my (now) weak chillingbath was not more possible to hold the Temperature under 22°C! It roses slowly to 24-25-26-27-28°C and my inner sense says: Shit, stop it! The now with orange NO2 filled Vessel was ready for a Runawayreaction and I had to dump everything into cold water to prevent a big waste of Chemicals! After thinning everything was fine! The PETN was quite fine after Neutrailzation and dries now near my desk :) Hmm I must say I love PETN fucking more then NG! Its stronger, safer, A SOLID, the Crystals are very Heavy :p its odorless and much more stable compared to NG :cool: The Yield is amazing and making high-concentrated Acid is not more that difficult since i'm using 65% HNO3 with 96% H2SO4 1:1! (The 111ml was distilled over in 20min!!)

[Myrol]

Yee haw! Today I blewed successfully 4 Charges up: 1x 30g APPN 50/50, 1x 4,6g PETN with 0,5g APPN, 1x 5g PETN also with 0,5g APPN and one time 8g APPN in two shotshells fired together :) The APPN was VERY Nice....a kick for my Ass and tada...a hole with 50cm diameter wich was 25cm deep! The first PETN-charge was louder as the 8g APPN (the second also :D ) and mades a Crater around 40cm wide the second nearly the same result....BUT the 8g APPN......absolutely harmless......The Sound was...well....not very impressive and the Crater....mmm...He was 30cm wide, ahh yes 30cm :) Harhar, my friend was pretty scared trough the first explosion....I looked also after the now three-week old 0,8kg APAN+1,7kg ANNM Crater.......HOLY SHIT!!!!!!!! He was defenately 1,80m wide and 50cm deep!!!! I cant believed it as I sawed him the first time: "Noooo, that could not be our crater :confused: !", but it was true.....Yeeee :p

[jim2]

HI all,

Last night I had this wierd dream.I tried making petn 8 0r 9 times and had no trouble but the last 3 times the same thing happened.Using Blasters method I cooled the acids down to 8 * C in an ice bath(using 62ml hno3( 70 %)- 38ml h2so4-20 gr PE).Added the PE to the hno3 over 16.5 minutes,when it was all mixed I mixed another 5 minutes to be sure.so far so good.Temp about 10* C.Started adding hno3/PE to the sulfuric acid very slowly,temp not over 20*C and all okay until the hno3/PE mixture started to turn brown.I dumped it quickly in water and the reaction stopped.THis browning of the hno3/PE mixture started after I got a new bottle of hno3(twice it happened ) so I bought another bottle and thought the problem solved. Today,using the new bottle of hno3 the same thing happened( 2 different companies).I Did the same thing as the 8 times before.Could the PE or the h2so4 go bad just like that?Any ideas would be most appreciated.Thanks