TrickEMethod
(Hive Bee)
01-30-04 21:22
No 485647
      30min/$40 - NH3 generator!
(Rated as: excellent)
    

Best and final NH3 generator

Ok, the wait is over...  Here is a near perfect NH3 generator for under 40$ in less time than it took me to splice together this post. 

The key design chioce is to use the waste CO2 that sublimates from the dryice to sweep the Nh3 vapor way from the hungry H20.  H20 is both a required trigger for the reaction and a side component as well.  Since NH3 is highly soluble in H20 a significant portion(sometimes almost all) of the newly created vapor is sucked up before it can be collected.  This design solves the absorbtion/suckback problems.



  /-------------------------------------\
 |                                       |
  ----                               ----
 |--||                               ||--|
 |  | \-----------------------------/ |  |

|  |                +============+   |  |
|  |                |            |   |  |
|  |          \     |     /      |   |  |
|  |           \    |    /       |   |  |
|  |            --[= =]--        |   |  |
|  |           /  |***|  \ /     |   |  |
|  |          /   |***|   '  /   |   |  |
|  |         /    |***|     /    |   |  |
|  |        /     |***|     \    |   |  |
|  |   +====|     |***|     |====+   |  |
|  |   |    |     |***|     |        |  |
|  |...|....|     |***|     |........|  |
|  |...+=========================+...|  |
|  |........|     |***|     |....|...|  |
|  |........|     -###-     |....|...|  |
|  |...+====|               |====+...|  |
|  |...|....|               |........|  |
|  |...|....|               |........|  |
|  |...+=========================+...|  |
|  |........|$$$$$|....|...|  |
|  |........|$$$$$|....|...|--|
|  |...+====|$$$$$|====+....\ |
|  |...|....|$$$$$|..........||---\
|  |...|....|$$$$$|.......MMMMM    +-      
|  |...+===========================================
|  |........\$$$$$/.......WWWWW    +-
|  |.........\$$$/...........||---/
|  |..........-------------.........../ |
|  |.................................|  |
 |  -----------------------------------  |                                         |
  \-------------------------------------/

 
 
.....  Acetone / DryIce
|  |   Gatoraid cooler
+---+   1/4" Polypropalene tubing
MMMMM   Polypropalene fitting
$$$$$   Amonia Sulphate / Lie
   /|   Bug sprayer
*****   Lie



If you notice the system is not closed, there is a single path for gas to escape the generator... through the 1/4 tube which passes out through a liquid tight fitting where the spigot once stood.  To escaping out the tube, gases must first pass through the drying chamber inside of the bug sprayer.  The only way into the drying chamber is through its perforated bottom.  Filter paper keeps the lie, which fills the drying chamber, from falling through the holes.  CO2 will sublime from the dryice/acetone slush on the outside of the bug sprayer and enter the bug sprayer through the open hole left after removing the sprayer hose and mix with any NH3/H20 vapor reciently produced from the fert/lie reaction and together they pass through the drying chamber where the H20 is removed and then through the 1/4" tubing running through the dryice/acetone slush.

Since the reaction mix is already chilled to a very low temp and the vapor is immediately mixed with the cold CO2 gas, it doesn't take long in a -78deg C 1/4" tube to afford condensation.  The steady flow of CO2 then forces the liquid Nh3 through the remainder of the tube and into whatever vessel sits bravely at its end. 
 
Construction is pretty simple and with a couple of exceptions, quite open to substitution.  I can picture using a 2L soda bottle in place of the bug sprayer, trading physical evidence for cleanup effort etc...

If you use the sprayer as I did, you simply hacksaw the arm of the hand pump and then remove the pump innerds leaving the outer shell and threaded flang. 
Any flat thin plastic can be cut with a hole saw or other convientent hand tool to close off the top of the pump section, held in place by the threaded flang.  A hold is drilled into the new plastic cap to attach the 1/4" tubing with a threaded press-2-fit fitting.  Another press-2-fit fitting is used to allow the tube to pass out of the 3/4" hold at the bottom of the cooler once filled by the spout.  Since the tube must pass through and not terminate at the lower fitting you must use a small file or drill bit to remove the ridge/barrier on the inside of the fitting.

The 1/4 tubing, press-2-fit fittings, bug sprayer and  gatoraid cooler are available at hadware depots in most facist contries, for under $40.

To operate the device;

1) fill space outside of sprayer with acetone and dryice
2) fill the inside of drying chamber with lie
3) fill the inside of sprayer with well mixed fert/lie
4) inject small amount of H20 into side port of bug sprayer
5) enjoy the suthing experience of your lungs fring until you close cooler lid
6) be not in the way of the sub-cooled NH3 liquid the spurts out of exit tube

So that's that.  Anyone who can't make their own Anhydrous NH3 at home is way too stupid to deserve drugs.


And on the eight day, God created Meth...
... and hasn't done much of anything usefull since!
 
 
 
 
    foxy2
(Distinctive Doe)
01-31-04 20:13
No 485769
      So what kind of results do you get?     

So what kind of results do you get?
How much material goes into each part of the generator and how much NH3 gets produced?
Has the NH3 proven anhydrous enough for a good reduction?
 
 
 
 
    TURNTABLIST
(Newbee)
02-01-04 06:21
No 485835
      Did You Use This? How?     

SwiTT's not one to say something will not work without trying it himself, but from his experiences, your post seems to defy logic. Maybe SwiTT is reading it wrong.

 You said the bug sprayer (generator) is submerged in Dry Ice/Acetone inside of a Gatorade cooler.

 That means the reaction of (NH4)2SO4 + NaOH has to take place @ -78C. From everything SwiTT has seen this reaction creates NH3 + Na2SO4 + H2O + HEAT, ie:(NH4)2SO4 + NaOH ------>  NH3 + Na2SO4 + H2O + HEAT.
 
 Since the reaction is exothermic, considering the reaction would even take place at that low of a temp, the pressure from the violent boiling of acetone would blow your cooler apart no doubt. But maybe you are only using a cup of NaOH and two cups Fert, obviously that wouldnt cause massive heat to be produced. SwiTT has seen then Generator get up to 180F so he is basing his assumption on that.

 Would the reaction even work at that temp? Maybe? Who Knows? But say it did produce NH3 + Na2SO4 + H2O, at that temp the NH3 would condense very quickly and its doubtful it will have the pressure to make it thru the dryer before it gets sucked into the extremely cold water in the bottom of the sprayer.

 The water generated is almost immediately turned into Ammonium Hydroxide. The FREEZING POINT of Ammonium Hydroxide is -77C so its not going to turn to ICE, and water that cold + NH3 will create a vacuum in the sprayer instantly. Just don't see the "sub-cooled NH3 liquid spurting out of exit tube."

 SwiTT has come to these conclusions from his experiences generating NH3 and the knowledge gained from working in Industrial Process.

 If he is wrong, he apologizes and never said it doesn't/won't work, but to him it doesn't seem possible.
 
 
 
 
    TURNTABLIST
(Newbee)
02-01-04 06:36
No 485837
      On the Flipside.     

Its seems to be a good plan except for the sprayer being in the DryIce/Acetone bath. But hell it may work like a champ.

 SwiTT was running 1/4" stainless tubing down-hill thru DryIce/Acetone similar to your set up but at one point a coil dipped and created a small up-hill angle in the submerged tubing. Liquid NH3 pooled and then froze solid in the tube. This caused ammonia to blow back the other way. Just a heads up that It can happen.


TT
 
 
 
 
    TrickEMethod
(Hive Bee)
02-01-04 12:27
No 485863
      I had put off posting the device because of...     

I had put off posting the device because of complete lack of time, so I had to settle for a complete lack of detail and background.  I just finally decided to get started somewhere.  I didn't realize how many key items I missed.  The device is targeted at producing a limited qty of NH3, for personal sized reactions... a few hundred ml. or so...

IN SHORT: If you are making 200ml of NH3 the reaction is not going to take all that long nor produce all that much H20 to clog the drying agent.  Nor will the sprayer settle to extreem temps, given the limited contact with the dryice slush. 

I've been quite busy for a bit and have only run the device twice, and my current situation makes 'testing' the NH3 ill advised right at the moment. I did not experience any of the problems that were described and am reasonably sure the NH3 produced is quite anhydrous. 

1) The fert/lie in the sprayer will hardly hit -78 before the reaction completes, especially since I only filled the cooler with about 2-3in of acetone.  The majority of the tubing rests in the acetone, but the majority of the bug sprayer is not(avoids floating the sprayer as well)

2) The seal that is achieved in my gatoraid cooler allows excess CO2 to escape and keep the pressure to a few psi, an adjustable vent would be one of the first improvements.  So far the tube has remained unclogged, which I would assume indicates the NH3 is indeed dry. 

3) I have such an excess of NaOH in my dryer relative to the minimal H20 vapor that results at these low temps

There are still more details that I will include and will forward pictures tonight to be included in the post as well.  If time permits, I may make a trip to the hardware depot and add an adjustable pressure vent to the device as well.  Leaving the venting to chance is quite cavalier when NH3 is involved, luck success and a lust for extreem simplicity lulled me into complacent laziness I suppose.

Ratio's, output and timing will hopefully follow tomorrow or the next day.

Bye for now

And on the eight day, God created Meth...
... and hasn't done much of anything usefull since!
 
 
 
 
    TrickEMethod
(Hive Bee)
02-01-04 21:39
No 485987
      One bit of background...     

One bit of background...

Starting over a year algo, I built several more complicated setups to produce NH3.  Each of these suceeded in producing useable NH3, with varying degrees of complexity and output.  The final device came along at the same time as an intense wave of official interest and intrusion into my habits and welfare. 

The device barely even tested was dismanteled and dumped along with a dozen other trunkloads of toys, tools and treats.  I had been a tinkerer and enthusiast as opposed to a producer, but my enthusiasm earned me a level of interest that makes any type of NH3 product research as comfortable as masterbating in church.

My final swing at a NH3 generator was by far my favorite son with such a bright future ahead of it.  Its untimely death in obscurity cried out for redress.  So reciently I picked up another gatoraid cooler, bug sprayer and some tubing and picked up where I left off.  In the next day or so, I will run a few more cycles and up the volume of NH3 targeted.  But the situation being what is is, I will leave it to those with friendlier neighbors to really test the limits of this style of device.

The basic device described will produce smallish - but certainly usefull - quantities of workable NH3.  Whatever performance variations or limitations exist beyond the trial runs (50-100ml) completed before my life got interesting are yet to be determined.

More details will follow...

And on the eight day, God created Meth...
... and hasn't done much of anything usefull since!
 
 
 
 
    TrickEMethod
(Hive Bee)
02-01-04 21:41
No 485988
      Pooling of NH3 in the tubing is one thing that     

Pooling of NH3 in the tubing is one thing that you will not need to worry over.  The volume of CO2 gas being generated from the dryice/acetone slush that takes the same path through the drying chamber and out through the tube will insure that all condensed NH3 is moved forward.

Depending on reaction conditions and quantities being targeted and length of 1/4 tube, an over-abondance of CO2 gas could result in a buildup of pressure which favors absorbtion of NH3 by the H20 and runs the risk of "blowing" the lid off the cooler.  Nothing like this seemed to happen during my two small runs.

An adjustable CO2 vent is being added that bypasses the bug sprayer, drying chanber and condenser tube.  The location of the vent minimizes the likelyhood that NH3 might be vented as well.  This is benifitial to both safety and control the flow rate of gases through and out of the condensation tubing, with minimal aditional cost or complexity.

Just took some pictures of the rebuilt device, will forward...

And on the eight day, God created Meth...
... and hasn't done much of anything usefull since!
 
 
 
 
    TURNTABLIST
(Newbee)
02-03-04 00:09
No 486151
      AH     

It makes more sense to SwiTT now.
 
 
 
 
    TrickEMethod
(Hive Bee)
02-04-04 08:44
No 486338
      Promised pictures...     

I promised some pictures, sorry I'ts taken so long.  I've lost the USB cable for my camera.  Going to try to borrow one today.

Has anyone given the device a try?  It takes less than an hour to put together.

And on the eight day, God created Meth...
... and hasn't done much of anything usefull since!
 
 
 
 
    dwarfer
(esoteric)
02-05-04 11:33
No 486619
      I'm impressed     

This appears to be the best design I've seen.

It may be a real clandestine breakthru.

hope those pictures come out...

dwarfer
 
 
 
 
    localbuilder
02-18-04 11:14
      Amonia Sulphate
(Rated as: UTFSE!)
    
 
 
 
    Old_Grignard
(Stranger)
04-10-04 08:20
No 500068
      Very Bad design for many reasons     

This is a bad design for many reasons, but the two most obvious ones are these:
1.  Your drawing shows your reaction mixture submerged in the dry ice/acetone mixture.  This will result in the generation of very little gas.  One of the ways to increase gas generation is to heat the reaction mixture after initial gas generation has subsided.
2.  Without a precooling of ice water, which is very cheap, all cooling is done with dry ice, which is expensive and waseful.
However, the problem with objection 2 will never occur because you will never get any gas because of objection 1.
Go back to the drawing board and try to get some appreciation of the reaction and reaction conditions before you try to design apparatus.
 
 
 
 
    xxxxx
(Hive Bee)
06-19-04 11:51
No 514297
      fractional crystalization of h20 from 28% nh4oh     

the percentage of water in an nh3/h20 mixture varies according to temperature from 0% nh3 100% h20 at 212f to 100% nh3 0% h20 at -33f. theoretically you could remove ice crystals from nh4oh as they formed (and not let the whole batch freeze solid) all the way down to -33f where you would have pure anhydrous ammonia. you can check the progress by measuring the specific gravity of the remaining liquid. with a standard freezer at 0f you could get up to 40% nh3 60% h20. if you put this in a vessel with a valve and allowed it to reach room temperature ammonia gas would be released when the valve was opened.
 
 
 
 
    18294
(Hive Bee)
07-28-04 11:45
No 522264
      pictures?     

did you ever take the pictures? Are they posted in some other thread or something? SWIM Used the search engine with no luck.

Anyone else tried this setup? SWIM is thinking about giving it a try this weekend.