Author Topic: Blue dye doesnt affect yields!  (Read 10663 times)

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hCiLdOdUeDn

  • Guest
Blue dye doesnt affect yields!
« on: November 12, 2002, 06:22:00 PM »
Hey

When makin methylamine.hcl you can do this

Clean the blue paraformaldehyde with 3-5gallons of H2O and a few alcohol soaks. This will leave the paraformaldhyde free of most of the dye (still light blue) but usable in the synth.

Also instead of buyin the good ole ammonium chloride you can make a conc. sol of NH4Cl from conc. ammonia solution and muriatic acid. This will leave a sol which some NH4Cl precipitates and the rest is a saturated sol (35g/100ml H2O) at room temp. This can be directly pluged into the brighstar synth!!

The methylamine.hcl will be slighty blue but in the Osmium al/hg it doesnt get in the final product and the yields are high~!



Sink or SWIM

noj

  • Guest
Blue?
« Reply #1 on: November 12, 2002, 08:31:00 PM »
Is the dye from an OTC source of paraformaldehyde? And couldn't all these posts about your success have been in the same thread?  :P

there's a big difference between criticizing your government and criticizing your country

hCiLdOdUeDn

  • Guest
Yes, there is an OTC source of paraformaldehyde ...
« Reply #2 on: November 12, 2002, 08:41:00 PM »
Yes, there is an OTC source of paraformaldehyde which contains a blue dye.

sorry about the multiple threads! :-[

Sink or SWIM

Chromic

  • Guest
hexamine
« Reply #3 on: November 14, 2002, 07:09:00 AM »
Once you try it compared to the HCHO/NH4Cl, you won't go back.  ;)

terbium

  • Guest
Hexamine
« Reply #4 on: November 14, 2002, 07:13:00 AM »
Why, what is the difference?

Baseline Does Not Exist.

hCiLdOdUeDn

  • Guest
swim needs a source first!
« Reply #5 on: November 14, 2002, 01:26:00 PM »
swim needs a source first! p-CH2O is fiiine so far  :)

Sink or SWIM

Chromic

  • Guest
Less stinky
« Reply #6 on: November 15, 2002, 08:46:00 AM »
I'd prefer handling 31% HCl over 40% HCHO. Also it's easier and cheaper to find hexamine and hydrochloric acid than to find formaldehyde and to *make* NH4Cl as in the post. Plus there's more "NH4Cl equiv" (ie as HCl/hexamine) used in the hexamine reaction, and according to K.C. Nicolau it's a good thing "to suppress the dimethylamine formation". Perhaps K.C. Nicolau (an old school bee, if you recall him) got that wrong?

terbium

  • Guest
OTC
« Reply #7 on: November 15, 2002, 10:32:00 AM »
I'd prefer handling 31% HCl over 40% HCHO. Also it's easier and cheaper to find hexamine and hydrochloric acid than to find formaldehyde and to *make* NH4Cl as in the post.
Yes, if you can only acquire OTC chems then perhaps you can't get formaldehyde so hexamine is the only way to go. If you can acquire simple but non OTC chems then paraformaldehyde and (store bought) ammonium chloride is the way to go. "Stinkiness" doesn't seem to factor anywhere into the decision.

Plus there's more "NH4Cl equiv" (ie as HCl/hexamine) used in the hexamine reaction,
IIRC, the ratio of ammonia to formaldehyde in hexamine is exactly the same as is called for in the Org. Syn. and Vogel preparations of methylamine.

and according to K.C. Nicolau it's a good thing "to suppress the dimethylamine formation".
I haven't a clue as to who K.C. Nicolau is but Vogel says the same thing so it must be true.


Perhaps K.C. Nicolau (an old school bee, if you recall him) got that wrong?
Whenever possible I prefer to get my information from  closer to the source - Vogel, Org. Syn. etc.

Baseline Does Not Exist.

Rhodium

  • Guest
I would really reccommend using ammonium ...
« Reply #8 on: November 15, 2002, 11:17:00 AM »
I would really reccommend using ammonium chloride/paraformaldehyde. The yield is 85%, and you don't need to handle ANY smelly/corrosive liquids...

Instructions:

https://www.thevespiary.org/rhodium/Rhodium/chemistry/methylamine.html


noj

  • Guest
Would Chromic's method of heating the second time ...
« Reply #9 on: November 15, 2002, 08:18:00 PM »
Would Chromic's method of heating the second time until ammonium chloride sublimes be a better workup than just heating until half remains? I seem to have difficulty knowing when all the ammonium chloride is removed, since it looks no different to me.

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terbium

  • Guest
Vogel or Organic Syntheses.
« Reply #10 on: November 15, 2002, 09:39:00 PM »
You should follow either the procedure in Vogel or the procedure in Organic Syntheses.

Baseline Does Not Exist.

BlingBling

  • Guest
Rub 1 off
« Reply #11 on: November 15, 2002, 09:57:00 PM »
>> I seem to have difficulty knowing when all the ammonium chloride is removed, since it looks no different to me.

When checking the final product, rub a little in between 2 fingers. If it disapears, it's MeAm, and most likely pretty pure. If it's grindy, almost descriptively fitting of the word "griemey" then it probably contains some ammonium chloride. I found this to be helpful when I thought making methylamine was fun.