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"True Blue" NH3/Li reduction ie birch

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Jacked:
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:
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:

WizardX:
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:
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.
--- End quote ---


And Anhydrous Ammonia Freezing point is at -107.9° F (-77.7c); a white crystalline mass forms.
--- End quote ---
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

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