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Hennig Brand
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[*] posted on 6-1-2014 at 18:46


DNT can be made much more easily than TNT, and with just nitrates and without the most highly concentrated sulfuric acid.

DNT in a Cheddite should actually increase sensitivity and propagation. It provides a continuous phase of high explosive material throughout the charge covering every particle of chlorate. The last table I posted was from a US military text published in 1984 and the text associated with that table described the mixtures as modern Cheddite formulations I believe. Nitroaromatics are generally considered to make Cheddites perform better, from what I understand.

Here are the 2 big reasons my charges had issues with propagation (I think).

1. The chlorate was not ball milled, but passed through a 100 mesh screen. Ball milling would have produced much finer material resulting in much better contact between the chlorate and the nitroaromatic(s) and fuel, resulting in better propagation, sensitivity, power, etc.

2. The chlorate was homemade and contained at least a small amount of chloride contaminant. The KCLO3 was made several years ago by electrolysis. I believe it was recrystallized once, but honestly I can't remember. The amount of chloride in any commercial sample, I would imagine would be far less than in mine. Sodium and potassium chloride are diluents, but they also cool the explosion, and also are hygroscopic which usually results in chlorate with higher amounts of moisture. Even small increases in moisture content greatly reduce sensitivity, etc, etc.

Honestly, I think the biggest difference between my test and Markx's test would be chlorate particle size. Small charges with weak confinement require other variables to be improved, and that means particle size, degree of mixing, density, strength of initiation, possibly added sensitizer, etc.

BTW, a couple or a few percent of aluminum powder is supposedly excellent for increasing sensitivity of Cheddites. I have never tried it with Cheddites, but I know it greatly increases the sensitivity of dynamites.

[Edited on 7-1-2014 by Hennig Brand]




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[*] posted on 6-1-2014 at 21:05


Quote: Originally posted by Turner  
TNT can be very nitric acid efficient depending on the operator and reaction circumstances.

RDX is by far the worst and most frustrating explosive if you value the costly nitric acid, 50ml gave me 6 grams of RDX and that isn't far off from theoretical yield.


Funny thing that HNO3 is more available to me than sulfuric acid, which why I prefer nitrations that do not need SA. :D According to my calculations, one will need a total of 533ml sulfuric acid, including oleum, and a total of 231ml HNO3 100% to get about 200 grams of TNT. The sulfuric acid is mostly recoverable through concentration, but it cannot be boiled up to oleum back anymore, so one will need to regenerate it somehow.
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[*] posted on 6-1-2014 at 21:09


Of course if I had stockpiles of pure Nitric Acid I would do a lot with RDX, but for me it's distilling it from already expensive sulfuric acid and nitrate. I once made around 20 grams and detonated that, cool material because it is very different sound than say an explosive like ETN, almost muffled and not as loud, but just as damaging.
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[*] posted on 7-1-2014 at 00:30


Quote: Originally posted by Hennig Brand  
DNT can be made much more easily than TNT, and with just nitrates and without the most highly concentrated sulfuric acid.

DNT in a Cheddite should actually increase sensitivity and propagation. It provides a continuous phase of high explosive material throughout the charge covering every particle of chlorate. The last table I posted was from a US military text published in 1984 and the text associated with that table described the mixtures as modern Cheddite formulations I believe. Nitroaromatics are generally considered to make Cheddites perform better, from what I understand.

Here are the 2 big reasons my charges had issues with propagation (I think).

1. The chlorate was not ball milled, but passed through a 100 mesh screen. Ball milling would have produced much finer material resulting in much better contact between the chlorate and the nitroaromatic(s) and fuel, resulting in better propagation, sensitivity, power, etc.

2. The chlorate was homemade and contained at least a small amount of chloride contaminant. The KCLO3 was made several years ago by electrolysis. I believe it was recrystallized once, but honestly I can't remember. The amount of chloride in any commercial sample, I would imagine would be far less than in mine. Sodium and potassium chloride are diluents, but they also cool the explosion, and also are hygroscopic which usually results in chlorate with higher amounts of moisture. Even small increases in moisture content greatly reduce sensitivity, etc, etc.

Honestly, I think the biggest difference between my test and Markx's test would be chlorate particle size. Small charges with weak confinement require other variables to be improved, and that means particle size, degree of mixing, strength of initiation, possibly added sensitizer, etc.

BTW, a couple or a few percent of aluminum powder is supposedly excellent for increasing sensitivity of Cheddites. I have never tried it with Cheddites, but I know it greatly increases the sensitivity of dynamites.

[Edited on 7-1-2014 by Hennig Brand]



Probably the difference was in particle size, but I did not really measure the sieve curve of the oxydiser so I can not comment if it was much below 100mesh or not. Judging by eye is pure speculation. And I did not make an effort to get it as fine as possible, just a more or less uniform powder (around 30min in the ball mill for about 500g batch). The fuel was mixed in by just shortly shaking around in a plastic container. Actually I've been amazed how well this simple mix propagated in sub 50g qunatities...as a matter of fact I also expected a partial reaction, but I've not been able to find any unreacted material after any test. Just a fine coating of KCl on the surroundings.
Maybe the iron oxide contamination from the milling media also had a fertilizing influence? It's not impossible as many metal oxides act as catalyst for chlorate breakdown reactions....although at these reaction rates it may be less probable. Guess more testing is needed to clarify the situation :D




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[*] posted on 7-1-2014 at 03:39


Are chlorates compatible with more powerful nitric esters? Because instead of having problems with DNT (any aromatic nitro) one could easily synthesize liquid esters (EGDN?) and try it in chlorate/fuel/ester dynamite mixtures for example. As I understand the highest yield of all different nitrations is expected from O-nitrations (alcohols) - compare troubles and yields for TNT, RDX vs EGDN, ETN, etc. However what I said is purely speculative, check literature for compatibility, stability before ever considering to try. Btw, chlorate mixtures are inferior to AN ones, isn't it?
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[*] posted on 7-1-2014 at 09:21


Markx, in order to try and get much meaning out of your test a lot of assumptions are required. I have seen Youtube videos from several years back with people detonating liquid hydrocarbon and chlorate, and of course it works. Its power is less than the ones with nitroaromatics of course, and I bet it doesn't store well (but I could be wrong). If it was really better to use only liquid hydrocarbons and chlorate then why bother making more complicated mixtures for the last hundred years? I guess what is better may depend on your position (whether hobbyist or industry or military etc)

Quote: Originally posted by papaya  
Are chlorates compatible with more powerful nitric esters? Because instead of having problems with DNT (any aromatic nitro) one could easily synthesize liquid esters (EGDN?) and try it in chlorate/fuel/ester dynamite mixtures for example. As I understand the highest yield of all different nitrations is expected from O-nitrations (alcohols) - compare troubles and yields for TNT, RDX vs EGDN, ETN, etc. However what I said is purely speculative, check literature for compatibility, stability before ever considering to try. Btw, chlorate mixtures are inferior to AN ones, isn't it?


When you say highest yield, what are you basing that on? Is it based on nitric acid/nitrate or on the organic backbone used? I have noticed that it takes very concentrated acids, industry uses oleum actually, to get good use of acids (or glycerine) when making NG for instance. A DNT synthesis on the other hand allows me to get yields based on nitrate (and toluene) used in the high 90% range.

Ammonium nitrate is of course a better gas producer, since it produces all gaseous products and KClO3 has a lot of potassium and chloride taking up valuable space in the explosive. Ammonium nitrate is probably closer to an actual detonating explosive in its pure form than the chlorates are also. I think the Cheddites hold their own though, especially the nitroaromatic and nitric ester Cheddites. They also have another wonderful feature, chlorate makes up the largest proportion of these explosives (usually around 80%) and it is very easily made and in large quantities from salt and electricity.

Nitric esters can be used in Cheddite type explosives, there is quite a bit written about it in "Nitroglycerine and Nitroglycerine Explosives" and several other sources I have seen.

[Edited on 7-1-2014 by Hennig Brand]




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[*] posted on 7-1-2014 at 11:47


I meant overall simplicity of production, and back in the time when once I prepared some quantity of EGDN(actually it was a test of synth) using concentrated H2SO4 (not oleum, not even more than 92% based on density) + AN mixture as nitration agent and pure EG. If I remember correctly I got nearly quantitative yield based on EG, and maybe the nitration mixture was taken with only a little excess. It was a smooth synth, no troubles, and low temps (from 0 to 10 C) cause less oxidation thus I say higher yields compared with nitroaromatics (high temp).
Unfortunately a good anode for chlorate remains a dream for me, do you use TiO2-RuO2 as usually people use? (I managed to produce 50g of chlorate with DIY Ti-Co2O3 anode, and when it finally passivated I gave up).
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[*] posted on 7-1-2014 at 13:52


I think the nitroaromatics, like DNT or MNN, make the best use of acids though. Getting to DNT is pretty simple. It does take a bit of time though and temperature control and monitoring, this is true. I have a really unpleasant allergic reaction (or some sort of physiological response) to MNT and even toluene itself a little bit, so I don't like working with it unless I have very good ventilation.

I just use graphite rods for making chlorate. If you start with sodium chloride and make sodium chlorate before conversion to potassium chlorate, it is easy to vacuum filter the solution through a layer of diatomaceous earth. Filtering through diatomaceous earth can remove practically all graphite particles, leaving you with nice snow white chlorate. I do have a pretty good size MMO anode that I used to make sodium chlorate in the past, and a platinum anode and titanium cathode I have used in the past to prepare sodium perchlorate. The sodium perchlorate was immediately converted to potassium perchlorate once all the chlorate contaminant was destroyed. Wish I had made some ammonium perchlorate. Ammonium perchlorate was used a lot in explosive formulations as well.




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[*] posted on 7-1-2014 at 16:09


MNT is toxic so no wonders on its bad effects. When I tried to use welding rods as anode for chlorate process they were degrading way too fast even at low currents, I guess these rods are not made of true graphite, rather from pressed carbon.
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[*] posted on 7-1-2014 at 16:18


The following relates to storage stability issues with these type of explosives.

Here is a couple of old posts from an archived copy of the old Rogue Science forum, which seemed interesting. The thread was called "Degradation of Chlorate-Vaseline Mixtures Over Time".

"Faeriedragon

July 8th, 2005, 09:59 PM

What is the chemical reaction that renders the chlorate & vaseline explosive mixture useless over time? I've seen this degradation happen before. When the mixture is freshly made, a speck of it works properly even with the drop of a hammer. A week later, the same mixture will not generate any reaction, even when smacked quite viciously. I've read that similar cheddite formulas were once used in wars half a century ago and now we've moved to better things but...how was the explosive stablized to prevent it from degrading?

Diabolique

July 15th, 2005, 06:19 PM

Many explosives that are plasticized (incl. Cheddites, Comp. A, Comp. C-series, etc), suffer from recrystalization. The result is that the plastic mixture solidifies and becomes insensitive to initiation. Something similar happens in blasting gelatin.

In Chlorate-Vaseline, the vaseline slowly disolves a tiny proportion of the chlorate (doesn't need to dissolve much), and the solution-deposition differential between the small and large particles (due to the mass:surface area differential) causes the large particles to grow and eventually merge. The result is like concrete, and about as explosive.

This is used to allow Comp A to be press-loadable into munitions, then solidify into a stable charge in the munition.

To reduce this, and prolong the plastic life of the explosive, ~0.5% of lecthin (food additive) is used. I believe I learned this from T. Urbanski's 'Chemistry and Technology of Explosives' - which cost ~$50 per volume when I was a teenager. Today $1500 for the set. My background - I taught this stuff in the Army. :eek:"

And the same member posts again in another thread the following year. This thread was called "Guhr Dynamite + KClO3 nitrobenzene cheddite".


"Diabolique

August 3rd, 2006, 04:07 PM

The finer the ingrediants, the faster the detonation. Some become easier to detonate, but others became very difficult to initiate into detonation.

Using (90%) KClO3 with (10%) vaseoline, the velocity increases with density, which is related to particle size and loading pressure, until it reaches a critical density, where it becomes insenitive even to PETN or RDX boosters. I understand that this, and uniformity of the mixture, are the problems with most Cheddites and related explosives. In WW1, the Germans added sulfur to Carbonit (bombs & grenades) to make it more cap sensitive. You may try this to sensitize some mixtures.

You may want to add 0.5% lecithin (find in health food stores) to slow down the recrystralization of the chlorate. Semtex today eliminates lecithin from its formulation to reduce diversion to terrorists - it hardens like concrete after a year or two. KClO3 & vaseoline will harden in about two weeks without lecithin."




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[*] posted on 7-1-2014 at 16:34


Regarding carbon anode erosion. Current density is a big factor, but it may also be that your carbon rod is lower density than some resulting in accelerated erosion. The rods can be soaked (days) in linseed oil or safflower oil I have read, and then lightly sanded before using them. Apparently this treatment does slow down erosion. I bought a box of 50, either 1/2" or 5/8" diameter and about 1 foot in length carbon rods a couple years back, and IIRC I only paid 40-50 cents for each individual rod. I think I was getting 1/2 lb or more of chlorate before the anode was useless, so I figured it wasn't worth bothering with the treatment (always meant to try it anyway though).

It seems to me that the anode always eroded far worse at or just below the surface of the electrolyte. If this portion of the carbon anode was well covered or sealed, the anode would last quite a bit longer most likely.

[Edited on 8-1-2014 by Hennig Brand]




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[*] posted on 8-1-2014 at 05:26


In the early days of my electrosynthesis experiments I also used graphite as anode material for chlorate production(sawn off section of a huge industrial graphite anode). Aside from current density another big factor for anode wear was cell temperature. With graphite and a cell temp over 40C the anode wear became really pronounced. The anode worked for a long time, but getting the graphite particles out of final product was really frustrating. I used KCl based electrolyte and hot filtering was the only option for purification. The bottleneck was filter material...it had to be permeable to allow for a fast filtration without the solution cooling too much and product precipitating in the material, yet it had to catch the graphite dust. The best I found was actually coarse glass wool (laminar thermal insulation board type), it caught the graphite particles exceptionally well even in a rather loosely packed form.



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[*] posted on 8-1-2014 at 06:06


I have done the hot filtering with KClO3 too, but it is so much easier and more effective to start with sodium chloride. Best to produce sodium chlorate with your cell, filter out the graphite particles, then perform the metathesis reaction with potassium chloride and obtain nice clean potassium chlorate. Yeah, higher temperatures probably do increase erosion, but higher temperatures, to a point, are beneficial for the process in general. I usually ran my cell in a very cool basement, at a moderate amount of current for the size of the cell, and the cell got warm but not really hot. Also, the cell was sealed and a vent line was attached which lead outdoors. Doing this outside or in an outbuilding of some sort would be preferable, but I was doing this when there was a lot of snow and it was 20C below much of the time.

I found that bit about carbon electrode treatment from Yarchive. The author was Bill Nelson I think (was a lot of names in some of those posts), back in 1994.

"Carbon electrodes don't corrode, but they _erode_, because
of the action of singlet oxygen produced in the electrolyte. They can be
stabilized by impregnation with high molecular weight binders, but this
just slows down erosion, it doesn't prevent it. However,
since carbon electrodes are readily available (from #6 dry cells, for
example), they are often the choice of DIY chemists. They can be used
successfully if they are properly prepared. First, all of the zinc salts
must be entirely removed. This requires boiling in hot water for a few
hours, which also removes most of the manganese dioxide. They must then
be dried thoroughly in an oven and allowed to cool. The carbon should
then be impregnated with a binder. The two easily obtained binders are
safflower oil or better, linseed oil. The carbon should be soaked in the
oil for two or three days, removed and wiped off, and allowed to dry
(harden) for at least a week. Then, and this is quite important, the
surface must be lightly sanded with find sandpaper to make the carbon
adequately conductive."


BTW, in my first post of this thread, back on page two, I included a copy/paste from a text regarding Cheddites and didn't include a reference. The text it was taken from was, "Industrial Nitrogen Compounds and Explosives" by Geoffrey Martin and William Barbour, published in 1915.

Regarding storage stability, having all the chlorate particles coated in solid nitroaromatic(s) should prevent or at least slow down the recrystallization and hardening process, which eventually leaves the explosive completely insensitive to initiation (I think).

[Edited on 8-1-2014 by Hennig Brand]




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[*] posted on 8-1-2014 at 12:16


Quote:

Sodium and potassium chloride are diluents, but they also cool the explosion, and also are hygroscopic which usually results in chlorate with higher amounts of moisture. Even small increases in moisture content greatly reduce sensitivity, etc, etc.

I dont't have the values ready right now, but are the chlorides really more hygroscopic than the chlorates?
At least for sodium i'm pretty sure that that's not true.


Have you guys ever thought about using catalysts like iron oxide?
They speed up deflagration a lot, but I've never seen them in detonating mixtures with KClO3 or NH4NO3



Quote:

a couple or a few percent of aluminum powder is supposedly excellent for increasing sensitivity of Cheddites


The effect on AN mixtures is very distinct, even 1% of dark al make a big difference. But I wonder how unsafe this gets. One could add the oil first an than the Al...
But it's still some kind of chlorate flashpowder.



Quote:

In Chlorate-Vaseline, the vaseline slowly disolves a tiny proportion of the chlorate (doesn't need to dissolve much), and the solution-deposition differential between the small and large particles (due to the mass:surface area differential) causes the large particles to grow and eventually merge. The result is like concrete, and about as explosive.


Any Idea if this will this happen with liquid paraffine oil too?
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[*] posted on 8-1-2014 at 12:42


I've read that in some old cheddites MnO2 additive was usually present, anybody knows what for?
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[*] posted on 8-1-2014 at 13:24


I guess I was a little unclear there. Never used sodium chlorate due to its water loving tendency. Potassium chlorate when pure is very non-hygroscopic, and potassium chloride and sodium chloride are both much more hygroscopic. Sodium chlorate is in some of the old Cheddite formulations, but I doubt most people would be interested in using it, if they had a choice, probably for most of the same reasons people into fireworks would usually prefer to use the potassium salt.

Explosives in general are dangerous, and chlorate explosives are probably more dangerous than most. I don't know how to quantify it exactly, but I know there is a big difference between a pile of loose chlorate-aluminum powder and a Cheddite where the chlorate particles are well coated in nitroaromatic and/or wax and/or oil. If the aluminum particles are well coated, as well as the chlorate particles, I would imagine this type of mixture would be much safer than chlorate-aluminum flash powder. Not really 100% sure on this one.

Yes, I would imagine that chlorate recrystallization and charge hardening would be a problem with liquid hydrocarbons. I am assuming they mean petroleum wax when they specify paraffin in Cheddites, but I guess in other parts of the world paraffin can mean a liquid hydrocarbon like diesel fuel or kerosene. Just assumed if its role was as a moderant that it would probably be solid at room temperature and coat the chlorate particles like the solid nitroaromatics do, but I could be wrong. The only Cheddite I can think of right at the moment without a solid coating material is the Vaseline Cheddite, and most of the time I have seen that Cheddite referenced paraffin (petroleum wax?) was included in its composition.

MnO2 is a catalyst commonly used to lower the activation energy of chlorate mixtures (increase sensitivity). I don't know if I have seen a Cheddite formulation with it, but it is used (or used to be maybe) in small impact sensitive type fireworks and in some oxygen generator applications. Do you have any references? Would like to read about that.

[Edited on 9-1-2014 by Hennig Brand]




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[*] posted on 8-1-2014 at 14:23


Not much I have to say, I looked in my refs to find where I read that, but only little information is found (russian book "chlorate and perchlorate explosives", Blinov ) : mixtures containing MnO2 were used by french and called "Prometheus", oxidizer is composed of 90-95% KClO3 and 5-10% MnO2, fuel: nitrobenzene (50%) + turpentine (20%) + oil(30%, crude?), oxidizer/fuel ratio is 87:13.
Surprisingly the web search gave nothing related, maybe I search wrong? But I remember I've seen it more detailed somewhere..

[Edited on 8-1-2014 by papaya]
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[*] posted on 8-1-2014 at 18:38


That’s interesting, there are so many ways to sensitize these mixtures. We have actually bumped on a half a dozen or more in the last while in this thread.

Industrial prices for potassium chlorate are about 2 to 3 times, per ton, what they are for ammonium nitrate right now. Industrially this would make chlorate explosives unattractive. However, for the hobbyist, if there was no access to nitrates it would be much easier to produce chlorates than nitrates on a reasonable/usable scale. Cheddites, and chlorate explosives in general, don't have the performance of the powerful molecular explosives, but they are very well suited to the hobbyist in some ways.




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[*] posted on 9-1-2014 at 00:55


For those who are familiar with the russian language:


Attachment: Blinov_I_F_Hloratnye_i_perhloratnye_vzryvchaty.djvu (1.4MB)
This file has been downloaded 563 times

This is a rather nice compendium of information on the kind of mixtures that are being discussed here.




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[*] posted on 9-1-2014 at 04:45


Wow, wish I could read that. Is there much new information, or is it a lot of repetition of what we have discussed already in this thread? If there are some things that stand out as being new and interesting, please, feel free to share in English. If you didn't mind you could write a brief summary of some of the things that seem new.



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[*] posted on 9-1-2014 at 06:29


Well, the main functional topics rely on same principles as already discussed on this thread....understandably the laws of nature have a broad jurisdiction :D
There are some interesting facts about history of chlorate based energetics and their use though. For example potassium perchlorate based "cheddites" predate chlorate based ones as their development was independent from the development of (electro)synthesis. Potassium perchlorate occurred naturally in chilean salpetre deposits (4%) and was extracted from there. And there is a huge plethora of different compositions discussed (or mentioned at least)....to give some as example: manlianites, cratites, coronites, chloratites, cremonites, carlssonites, albites, almetrites, permonites....the list goes on :D I'm not sure I translated all of them correctly into english as the russians have a habit of translating (sort of) names and doing the reverse engineering on that is like solving a differential equation- you end up with a multitude of solutions.
There is also a lot of practical technical information on the precursor materials properties (chemical, thermal stability vs. different contaminants, hygroscopicity vs contaminants, brisance aptitude to detonation vs additives fuels etc).
I really do not know which picks to take for translation..........best would be of course to fully translate the book, but I honestly can't find the time or strenght in me to do that. Even the thought of it drives me to drink :D




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[*] posted on 9-1-2014 at 09:55


It sounds really good, is there any way of feeding that into a translator?
Just drink some Vodka, the Russian will be just flowing out of you then. :D




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[*] posted on 9-1-2014 at 10:22


Russians don't like vodka jokes btw., it's something like democracy jokes for americans :D
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[*] posted on 9-1-2014 at 10:59


I'm Canadian and there was no disrespect intended really. Just trying to increase his activity/energy level through agitation. :D

Well, ok, I might of been having a little bit of fun at his expense. :)

I am trying to do the translation using various free software, but so far no luck.




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papaya
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[*] posted on 9-1-2014 at 11:09


First you must do OCR, then automatic translation, I guess you already knew..
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