Author Topic: "True Blue" NH3/Li reduction ie birch  (Read 11868 times)

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Osmium

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> Swim has always been taught and know...
« Reply #40 on: June 03, 2004, 03:36:00 PM »
> Swim has always been taught and know first hand that water becomes a
> solid or frozen at 32 degree's or 0 celcius

Seems like you skipped the following science class where the teacher talked about melting points being depressed by stuff being dissolved in water. What do you think is the purpose of antifreeze in your car? And what happens when a little water will be dissolved in a whole lot of NH3?


ordinaryguy

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A delayed respose to your questions
« Reply #41 on: June 03, 2004, 08:17:00 PM »
Scottydog,
Swim has never built a NH3 generator out of a bug sprayer. This means it would be irresponsible for swim to advise you in it's safety.(or not) If swim where to build one, swim would use a clean plastic gas can for the rxn chamber like Mr. Clean suggested. The rxn causes pressure to build and swim would not feel very confident that the pressure release on the bug sprayer could withstand it.

If you chose to use NaOH in the drying chamber and utilized glass wool at the entrance to the tubing it would prevent them from plugging.

A water filter is out of the question as NH3 is soluble in H2O. Any generated NH3 would disolve into the H2O instead of condensing. Are you sure the post wasn't refering to filtering the pressure remaining after the NH3 was condensed to filter out the odor?

My suggestion is that you search

https://www.rhodium.ws

for "the complete birch by mr. clean" and read the NH3 generation posts.


Jacked

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reply
« Reply #42 on: June 04, 2004, 11:26:00 AM »
I think SD was talking about a water filter with "no water in it".
 H2S04 is used to dry HCl gas would it dry NH3 as well?
 A no brainer? There is nothing in this forum that is a no brainer, or in this thread I might add.


wareami

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Suckback
« Reply #43 on: June 04, 2004, 02:52:00 PM »

Something should be done to prevent suck-back if this is utilized.



Ibee learned early on from a Chemistry Book that by simply attaching the tube to an inverted funnel then placing the funnel, basket side down in liquid will help to prevent suckback.


a $2.00 test sure beats the hell out of ending up bling or disfigured



Excuse me, but what's Michael Jackson got to do with this? :o


A no brainer? There is nothing in this forum that is a no brainer, or in this thread I might add.



The Resident Alchemist Deluxe musta forgot about ole Ware stickin his twocents in.....LOL!
Howdy CaveMan!




foxy2

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H2S04 is used to dry HCl gas would it dry NH3...
« Reply #44 on: June 06, 2004, 03:47:00 AM »
H2S04 is used to dry HCl gas would it dry NH3 as well?

I wouldn't try that one....


Jacked

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reply
« Reply #45 on: June 06, 2004, 05:30:00 AM »
Your right about that one, I don't know what I was thinking about at the time but it wasn't safety, that could be quite a violent adventure. Strike that!


up247365

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What works for swim might not work for you
« Reply #46 on: June 07, 2004, 07:19:00 AM »
Every time swim has made his own juice,the only problem he ran in to was the amount of juice needed and the amount produced. Swim can't do a big of rxn's as he would like to but that's it. You can bee as technical and scientific as you want to, no offence, but bottom line is that Swim's way works perfect every time and he has some of the best shit around, maybe not the most, but the best. And he is completely self-sufficient on gathering the ingredients to support his habit and passion.

TURNTABLIST

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Anhydrous Ammonia - Freezing Point: -77.7ºC +...
« Reply #47 on: June 09, 2004, 12:24:00 AM »

WizardX

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Reaction Tips
« Reply #48 on: June 09, 2004, 10:36:00 PM »
Organic Syntheses, CV 6, 731

2. It is necessary to use a dry ice condenser to shorten the time required to condense the ammonia (4 hours compared with 6 hours without the condenser). The ammonia tank was warmed with an air gun during the distillation. The condenser was removed after the ammonia was collected.
3. It is necessary to use a strong stirring motor since the reaction mixture becomes, temporarily, rather viscous.
4. One should not pour the liquified ammonia directly out of the cylinder since particles of iron compounds might be carried along, catalyzing the formation of sodium amide. For the exclusion of moisture it is also necessary to use a drying tower (potassium hydroxide) between the cylinder and the flask.
5. The sodium should be cut into small particles to increase the speed of dissolution and diminish the danger of stirrer blockage.
6. During this period the reaction mixture might turn white. In this case, another portion of sodium must be added until the solution becomes blue again.


Organic Syntheses, CV 5, 467

3. Only five or six pieces of sodium should be added at one time in order to avoid an almost uncontrollable exothermic reaction. The solution turns blue and then white as the sodium is consumed. When the solution turns white, another portion of sodium may be added. The last 50 g. of sodium may be added without waiting between portions because the reaction is much slower at this point.
4. Because dissolution of the salts is a highly exothermic process, the water should be added slowly. A stream of nitrogen may be passed through the reaction during the addition of the water to ensure that no fire is started by bits of sodium that may be adhering to the upper walls of the flask.


Organic Syntheses, CV 4, 887

5. During the addition of the lithium the solution turns deep blue. After this has occurred (after about one-third of the lithium has been added), the rate of addition can be increased considerably.

TURNTABLIST

  • Guest
Sorry, 28-30% NH3 in Water
« Reply #49 on: June 10, 2004, 11:17:00 PM »
Sorry, 28-30% NH3 in Water freezes @ -77o according to

http://www.usask.ca/chemistry/courses/laboratory/114/msds/ammonium_hydroxide.pdf



And Mr Clean's complete birch says

OOPS: turns out, the freezing point of NH4OH (aqua-ammonia) is 1 degree higher than the freezing point of anhydrous ammonia.




And Anhydrous Ammonia


Freezing point is at -107.9° F (-77.7c); a white crystalline mass forms.


http://www.rmtech.net/Anhydrous%20Ammonia.htm



PRODUCT NAME: Ammonium Hydroxide
CAS NO: 1336-21-6
TRADE NAMES/SYNONYMS: Ammonia Aqueous
FORMULA: NH4OH
FORMULA WEIGHT: 35.05
DOT HAZARD
CLASSIFICATION: Corrosive Material
PIN(UN#,NA#): NA 2672
WHMIS CLASS: Class E
INGREDIENTS: %: 28-30% NH3
TVL: 25 ppm
HAZARD: Corrosive


Ammonium Hydroxide
_________________________________________________________________
PHYSICAL DATA

PHYSICAL STATE: Liquid
VAPOR DENSITY: 0.6 (air=1)
ODOR THRESHOLD: 50 ppm
SPECIFIC GRAVITY: 0.9
FREEZING POINT: -77o


Offline aamer

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Re: \where is problem
« Reply #50 on: September 16, 2015, 12:11:47 PM »
Swim have five kgs of Ephedra Distachya or Ma-Huang. He extracted alkaloids with two different methods.
 first by Hydro-Diffusion Extraction (also known as percolation) is the newer extraction methods for essential oils..He  fed steam in from the top on to the botanical material in cylinder while in the case of steam distillation, steam is fed from the bottom. When he got the distillate He evaporated it to low bulk after acidifying it by HCL then extracted by toluene then rendered alkaline with lye. After drying he got 100 grams of free base by this method.
Second  with solvent method he added plant material powder in water for two days with good stirring. The mixed extract is filtered and rendered strongly alkaline with sodium carbonate and the mixture again filtered. evaporated to low bulk and The filtrate is saturated with sodium chloride, then alkaloids extracted with toluene he got 100 grams of free base by this method.
.After this he decided for Birch reduction. He carefully collected fb obtained by both methods which is brownish black oily type. Slowly he dried it with low moderate heat under a griller.
 In three necked 5ltr round bottom flask in ice bath with calcium chloride  (super cooling) whilst fitting it into the bucket system. He added NH3 , stirrer ,then added 15 gms of Li metal in and wait 20 minutes for it to dissolve, When Solution turns dark blue he added pre addition 500 ml petroleum ether then he pour freebase gently into the dark solution.
Other 100 gms he put in flask fb first with petroleum ether then poured NH3. Then he poured sodium 45 grams till solution become royal blue.
 After adding water and evaporating NH3 he found brownish black colored residue in the bottom of flask. which is not in the pet ether. In both cases. While a little amount of oil found in solvent. He extracted it and bubbled he got 3 gms of cubic and needle type  small sized crystals. Which is soluble in water but not in alcohol…. He is in hot water. Any one must help him where is the problem. He is sure that plant matter is Ephedra distachya or Ma-Huang

Offline Necrogram

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Re: \
« Reply #51 on: November 16, 2015, 04:16:32 AM »
Is there a simpler route to generating usable NH3 Mister cleans genorator and condenser?
SWIM has not been able to aquire a tank since the late 90's. Since the dawn of the 'SnB and variations of the BIRCH and Benkesser, just starting to dream again has had it's barriers with new gaks.
I am hoping to glean a few more simpler methods.

Thanks Bees!

Also wanting to check out more threads on p2p from Benz aldehyde then to racemic Methamphetamine using sodium borohydrate.