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Laboratory of Liptakov
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[*] posted on 7-4-2017 at 12:39


:cool:Thanks for link.....:cool:.....and oters....But is impossible, that on bottom will arise as firstly crystals NaClO3, because he has much highly solubility than NaCl. It is against logical. And if yes, on how temperature cooling ? On Zero Celsia? I read almost all about it, but still I do not know how to make apart both compounds. I need some tutorial: Take 100 grams NaCl/O3.
Dissolve in 100g (??) distill water. Heated on boiling point 100 C. Cooling on 63 C ??
Separation NaCl crystals on filter. Solution is pure NaClO3 (99%). Tutorial not exist.




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[*] posted on 7-4-2017 at 12:55



Na Chlorate is more soluble and this means that for to get it to come out of solution you simply must have a greater concentration of it in the solution. It will they ppt out..
Keep running the cell and adding raw material (NaCl) and the concentration of chlorate will go up and up and solid material will start to be deposited on the cell floor.

http://www.sciencemadness.org/talk/files.php?pid=375539&...

https://www.sciencemadness.org/whisper/viewthread.php?tid=20...



[Edited on 7-4-2017 by yobbo II]

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[*] posted on 7-4-2017 at 13:11


OK, I read all, it is system "salting out from the solution". Yet, that NaClO3 has highly solubility, is possible he get out from solution huge increase just simply NaCl. Absolut against reason.....:cool: It is as quantum physics. Nobody knows how is it possible, but work it. For sure I will rinsed in cell Schrödinger cat. Well, maximum simply method is increase NaCl + 10%, waiting on 70 C, again + 10% NaCl, again waiting on run temperature. ETC...
Until the cat climb out from solution....:cool:...LL




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[*] posted on 7-4-2017 at 14:08


I noticed recently that it bumps horribly if you boil it down too fast. Nothing boiling saturated NaClO3 flying all over the place....



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[*] posted on 7-4-2017 at 16:55


Quote: Originally posted by Laboratory of Liptakov  
How apart NaClO3 from NaCl solution ? I have 100g mix NaClO3 + NaCl as dry crystals. This mix content : 50% NaCl + 50% NaClO3
Or also 10% NaCl + 90% NaClO3. It nobody know. Graph for NaCl is solubility 35g in 100g Water at 0 C. And 39g at 100 C.
For NaClO3 is graph solubility : 80g at 0 Cels. and 200g at 100 Celsia. Exist some method recrystallization. I look on all S-M, but not find describe exactly how to make. Especially making so, for relatively best purity on NaClO3. NaClO3 estimate stay as solution. But at how concentration create before heating on 100 C ? Dissolving 200g mix-salts in 100g H2O at 99 C ? And after what? Decrease slowly temperature on 50 C? And by 50 Celsius separe NaCl ? Or separe by zero Celsius all crysralls ? Thanks..........:cool:
Exist 1000 tutorials how to make KClO3 but nothing for NaClO3.

[Edited on 7-4-2017 by Laboratory of Liptakov]

@LL,
you didn't do your homework wel :mad: ...everything is into this forum and especially into a tread in which you have replied...:D;):cool::P(*)

1°) Simply dry all the NaCl/NaClO3 (and NaClO4 if ever present)

2°) Then extract with dry aceton or ethanol....leave the unsoluble NaCl (NaCl is almost unsoluble into aceton while NaClO3 is soluble and NaClO4 even more)...solubility of NaCl into ethanol is low while NaClO3 and NaClO4 are much more soluble.

3°) evaporate the aceton/or ethanol (avoid too much heat and favor the use of a closed system to avoid risk of fuel-air explosion of aceton/ore ethanol vapour-flame point is quite low so risk is high) and condense it to recover the valuable solvent for reuse and some economical turnover.

4°) Collect the dry crystals from solvent evaporation...it is NaClO3 and NaClO4 if present.

(*)
Here are some interesting solubility tables into ethanol I have gathered
tables provided by PH Z into NH4ClO3 tread

And here is a little later reply where I wrote:
***********QUOTED from myself*********
Side note:
It is to be noted that into the tables one may see that for the case of NaCl/NaClO3...the use of aceton is preconized to effect separation because NaCl is quasi totally unsoluble into aceton while NaClO3 is very soluble in it and NaClO4 even more...
Here it seems it is also the case with absolute ethanol that is quite a good solvent for that specific chlorate and perchlorate but not a good one for NaCl...
This is very interesting for all the old weed killer (60% NaClO3/40% NaCl) bags I own or for the purification from electrolysis chlorate cell from chloride...
*********END OF QUOTE***********
Quoted from here
A reply further into the same NH4ClO3 tread

[Edited on 8-4-2017 by PHILOU Zrealone]
I invite you to search into this http://chemister.ru/Database/properties-en.php?dbid=1&id... and the upper left "Search in database (English) " then you can type NaCl for example and get solubilities at various températures and sometimes into different solvents than water...

[Edited on 8-4-2017 by PHILOU Zrealone]




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[*] posted on 7-4-2017 at 23:01
solubility


Thanks Philou.. However I am before put questions about separation making dissolving process and tested solubility my mix just in acetone. Into 50 ml acetone was insert 25,9g of mix salts. Heated on 50 C and cooling on 25 C. However after filtration and evaporate acetone, was on inert surface only 0,03g some. Practicaly nothing. I find and look on table on wiki. I are same digits as in your recommend tables about solubility. My opinion was, that on wiki are bullshit. Why it say: Because this mix, after mixing in sugar ( ratio 35 sugar / 65 ) burning very quickly, same as should by this mix, from pure NaClO3 + sugar. And according a lot videos with pure NaClO3 + sugar it seem, that I have almost pure NaClO3. However in acetone total not soluble. Ethanol (14,7g/100ml) was not tested yet. Go on it....:cool:...LL



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[*] posted on 8-4-2017 at 05:26



US 3151935

has some discussion regarding subject.

If the acetone contains some water do you know what are the solubilities? or do they change much with a few % of water?
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[*] posted on 8-4-2017 at 12:20


Good patent.. Very details about problematic solubility and next important things...Thanks...I´ve what for study on long times...:cool:...LL



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[*] posted on 8-4-2017 at 16:28


Quote: Originally posted by yobbo II  

US 3151935

has some discussion regarding subject.

If the acetone contains some water do you know what are the solubilities? or do they change much with a few % of water?

As a first approximation you may put the solubility of the salt into pure water and into aceton into a solubility as a function of the % of water and the % of aceton graph by putting the solubility at 100% water and 0% aceton on one side and the solubility at 100% aceton and 0% water on the other side...then draw a line between the two and you have a good idea of what might result from a few % water...this is observable into the link to graphs and tables into my previous post...but with the case of ethanol and different water content.




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[*] posted on 9-4-2017 at 13:42



Would there be an issue with ignition with the mixture when drying. A small amount of acetone mixed with sodium chlorate sounds like stuff that might ignite with a spark?
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[*] posted on 10-4-2017 at 10:45
separation NaClO3


The problem with splitting, separating NaCl from NaClO3 resolved. Both substances were dissolved in the smallest possible amount of water, at temperature 20 C. The water is brought to a boil. Observing, watching level boiled solution. If on surface arises a gray coating - fine crystals, the solution is immediately (maximum hot) filtered.
Upstairs in the filter, during process filtering, arises crystalls NaCl. In solution bottom filter in flask, arises next crystalls NaCl, (after cooling to 20 Celsius. ) The solution is filtered or decantated at 20 C. We have Pure solution NaClO3 + water, in purity 99%. Done. For best purity is possibe process repeated again.
Self / answer sytem....Liptakov.....:cool:...LL




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[*] posted on 10-4-2017 at 14:08


Quote: Originally posted by Laboratory of Liptakov  
The problem with splitting, separating NaCl from NaClO3 resolved. Both substances were dissolved in the smallest possible amount of water, at temperature 20 C. The water is brought to a boil. Observing, watching level boiled solution. If on surface arises a gray coating - fine crystals, the solution is immediately (maximum hot) filtered.
Upstairs in the filter, during process filtering, arises crystalls NaCl. In solution bottom filter in flask, arises next crystalls NaCl, (after cooling to 20 Celsius. ) The solution is filtered or decantated at 20 C. We have Pure solution NaClO3 + water, in purity 99%. Done. For best purity is possibe process repeated again.
Self / answer sytem....Liptakov.....:cool:...LL


Did you mearure the amounts of NaCl and NaChlorate to get the 99% figure?
Will this process not depend on the amounts of Chloride and Chlorate (the ratio) that you have been starting off with.
If you have a mixed solid of 3% chloride and 97% chlorate will you have chloride being ppt out first?

The acetone would be much better for this kind of one off seperation.

Yob
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[*] posted on 14-4-2017 at 04:24
AnWax


Hi everyone,

I'm kinda new to the forum. This is my first post but i have already read through a lot of posts, my main source of other people's experiences.
I happen to have some pure paraffin lying around, and i was wondering what would be the best method to mix it with AN to obtain a AnWax mixture?
Correct me if i'm wrong, but i think some etn should be more than enough to detonate it?

Thanks for advices!

Ps. I apologize for any grammatical errors.
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[*] posted on 14-4-2017 at 13:14


Of course, that ETN should be enough detonate any AN -WAX. Usually 3 grams is enough for AN-WAX , if is wax added as solution in gasoline and follow evaporate gasoline. Better is always add 2% Al. Much deminers has opinion, that main charge 1 Kg and more requires a big booster, for example 10g Hi - brisant EM. It is not pretty right. If is main charge medium sensitive, enough No.8. Or small booster 2 - 3g at it. For full strenght..........:cool:



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[*] posted on 25-4-2017 at 06:54


Is sulfur a better sensitizer for AN than aluminium ?
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[*] posted on 26-4-2017 at 01:31


Quote: Originally posted by Si Da Sci Guy  
Is sulfur a better sensitizer for AN than aluminium ?

No but the mix of the two mixes would be synergetical over the two appart.

There might be storage issues between Al/NH4NO3/S due to air moisture and hygroscopicity of NH4NO3, mild acidity of S (air oxydation leads to SO2 and SO3 traces or it is trapped inside the S crystal matrix) and mild acidity of NH4NO3...thus chewing protective oxyd layer of the aluminium

--> generation of H2 gas (flamable),
--> generation of much heat that may accelerate decomposition if in larger enough quantity to allow for good heat dissipation.

The powder will invariably loose power upon storage since untreated Al powder will be oxydised and the amount of active metal will be less.

Into hermetical container, pressure may rise upon storage.




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[*] posted on 26-4-2017 at 06:27


Thank you for your response PHILOU Zrealone.

So throw them all in, maybe 2.5%S 2.5%Al 95% NH4NO3.

What do you make of adding an AN decomposition catalyst in like ammonium chloride, will that help during the detonation?
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[*] posted on 26-4-2017 at 11:31


I know I'm jumping in here and asking lots of questions but here is another quick one:

is 8675.9 kJ/mol ( 8.675 MegaJoules ) high for a standard enthalpy of combustion. The molecule is Myristic Acid and has a molar mass of 228.38 g·mol−1.


I mean is that a lot of energy ?
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[*] posted on 26-4-2017 at 11:48


It looks high for a small molecule, but compare it to an equal weight of methane, with ∆H ≈ 890 kJ/mol. Methane's molar mass is 16 g/mol, so approximately 18.3 moles of methane has equal weight to one of myristic acid. 18 moles of methane combustion is worth about 16 megajoules.

I wonder if AN/paraformaldehyde might have a better oxygen balance than ANFO. Possibly AN/polyoxymethylene?

[Edited on 26-4-2017 by clearly_not_atara]
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[*] posted on 26-4-2017 at 20:14


Quote: Originally posted by Si Da Sci Guy  
I know I'm jumping in here and asking lots of questions but here is another quick one:

is 8675.9 kJ/mol ( 8.675 MegaJoules ) high for a standard enthalpy of combustion. The molecule is Myristic Acid and has a molar mass of 228.38 g·mol−1.


I mean is that a lot of energy ?


You can judge from the structure.

Acetyl group + a carbon backbone chain.

Just a combustible compound, like any other organic compound, nothing "energetic" in the sense of EM

[Edited on 27-4-2017 by DubaiAmateurRocketry]
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[*] posted on 27-4-2017 at 17:34


Quote: Originally posted by yobbo II  

Would there be an issue with ignition with the mixture when drying. A small amount of acetone mixed with sodium chlorate sounds like stuff that might ignite with a spark?

No risks since aceton is too volatile and will cool down by evaporation the NaClO3 below its decomposition temperature.




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[*] posted on 27-4-2017 at 17:46


Quote: Originally posted by Laboratory of Liptakov  
The problem with splitting, separating NaCl from NaClO3 resolved. Both substances were dissolved in the smallest possible amount of water, at temperature 20 C. The water is brought to a boil. Observing, watching level boiled solution. If on surface arises a gray coating - fine crystals, the solution is immediately (maximum hot) filtered.
Upstairs in the filter, during process filtering, arises crystalls NaCl. In solution bottom filter in flask, arises next crystalls NaCl, (after cooling to 20 Celsius. ) The solution is filtered or decantated at 20 C. We have Pure solution NaClO3 + water, in purity 99%. Done. For best purity is possibe process repeated again.
Self / answer sytem....Liptakov.....:cool:...LL

True!

The solubility of NaClO3 was contradictory into several documents I have found...so I did test it...was 1,6g / liter aceton (coherent with US patent 3151935A what mentions 1,7 g/L). This is 8 times better than NaCl...so in principle with a Sohxlet extractor, one could extract more selectively NaClO3 from a NaCl/NaClO3 mix...

Based onto that patent solubility of NaClO4 is 216 times better than NaClO3 and 1840 times better than NaCl.

Into the "traité de chimie minérale" about sodium and lithium...they expose the solubility of NaClO3/NaCl mix saturated into water as function of the T°. The NaCl is usually dropped out of the solution by the mutual ionic effect since while NaCl almost doesn't increase its solubility when warming; NaClO3 does it exponentially...so more Na(+) and NaCl kicked out of the solution faster (at a lower concentration than when alone)...Solution if filtrated warm, then slowly cooled down and almost pure NaClO3 are collected...
--> That is the process LL has used/reinvented ;-)




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[*] posted on 27-4-2017 at 17:54


Quote: Originally posted by Si Da Sci Guy  
Thank you for your response PHILOU Zrealone.

So throw them all in, maybe 2.5%S 2.5%Al 95% NH4NO3.

What do you make of adding an AN decomposition catalyst in like ammonium chloride, will that help during the detonation?


That composition may work for a detonation process but (is it stoechiometrical? --> if not then) not for a good burning composition (like rocket or deflagrating banger).

Nearly anything catalyses the decomposition of AN into a detonation process -->nearly anything is a sensitizer of AN.
AC will of course be.

The mix AN/AC (NH4NO3/NH4Cl) may be troublesome for corrosive reasons towards container especially if metallic... moisture will probably set some traces of nitrosyl chloride free and be kind of a solid form of an unefficient aqua-regia.




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[*] posted on 27-4-2017 at 18:02


Quote: Originally posted by Si Da Sci Guy  
I know I'm jumping in here and asking lots of questions but here is another quick one:

is 8675.9 kJ/mol ( 8.675 MegaJoules ) high for a standard enthalpy of combustion. The molecule is Myristic Acid and has a molar mass of 228.38 g·mol−1.


I mean is that a lot of energy ?

Nearly about the same as any organic oïl...
and a little less than same lenght mineral oils (paraffins) because part of the myristic molecule (an organic carboxylic acid) is already oxydised (-CO2H terminated)...

-->compare the heats of combustion of ethane, ethanol, ethanal and ethanoic acid to understand this.
(or the ones from methane, methanol, methanal, formic acid and carbonic acid)...

Carbonic acid has no more energy to be combustible on its own (to the contrary...it will extinguish fire).




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[*] posted on 27-4-2017 at 18:09


Quote: Originally posted by clearly_not_atara  


I wonder if AN/paraformaldehyde might have a better oxygen balance than ANFO. Possibly AN/polyoxymethylene?

[Edited on 26-4-2017 by clearly_not_atara]

The OB depends onto the % of fuel vs oxydizer so the question has no sense per se. ;)

But if the % of paraformaldehyde/polyoxymethylene and mineral oïl are the same in both compositions; then yes ;) the (-CH2-O-)n variant will be higher in OB than the (-CH2-CH2-)n one...

But the detonic parameters have to be analyzed to determine which of the two will be more potent...fuel oïl contains more energy but is lighter...POM is denser but contains less energy...stil a decent amount....
Into a detonation process POM may depolymerise into CH2=O and react instantaneously with NH4NO3 to make "virtually" hexamine dinitrate equivalent (7000 m/s VOD) or Methylamine nitrate equivalent (6500 m/s VOD) thus better than ANFO (3500 m/s at best)...

[Edited on 28-4-2017 by PHILOU Zrealone]




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