Can ~30% HCl be concentrated ?

nubee · Master Archiver

Can ~30% HCl be concentrated ?

can some water be removed somehow ??

as want to make a salt, and figure the less water the better results ill get...

ApprenticeCook · DILLIGAF

Please dont tell me you want the actual solid form of HCl? thats just crazy talk...
If you want to make the HCl salt of an amine use HCl gas prepared from the drying of your 30% aqueous HCl. You do need to dry the gas as much as possible, so use CaCl2 drying tube inline with your gas generator and gassing medium (amine freebase in np solvent).

-AC

nubee · Master Archiver

no not solid.. Laughing

i do need to make ibogaine hcl, from crude raw extract, so method calls for dissolving in acetone and adding a few drops of hcl.

but i have had trouble before with nothing happening, so am thinking may have more luck if it is more anhydrous or by gassing instead?

can i dry acetone with mgso4 ? is it worth it ?

can i remove soe of the water in 30% hcl to increase "potency" ??

or would you strongly recomend gassing ?? though i have no setup and would like to know the easiest otc ?

IndoleAmine · Dreamreader Deluxe

Gassing needs nothing special - a distillation setup, piece of rubber tubing and a glass tube to extend the dip tube of your receiver adapter to the bottom of your receiving flask... (nothing uncommon)

You can concentrate HCl 30% by bubbling HCl gas through it until 37% are reached (=saturation), for this you can use a HCl30%/CaCl2 mixture to generate wet HCl gas, which will suffice for this procedure. Just two acid-resistant plastic jugs, rubber stoppers and acid-resistant hose (surgical silicone tubing? Simple red lab rubber hose?) to bubble the evolving gas into the 30% acid....

(maybe you can also add CaCl2 to HCl 30% and distill directly to get 37% fuming HCl, but I doubt it, since heat means less gas can be dissolved generally..)

If you start gassing HCl, you could of course do the little step of using a drying tube in line, and avoid the use of aequous HCl at all... Wink

But why not use more acetone, or better: azeotropic drying with a nonpolar solvent like toluene? Add toluene, then amine, then HCl 30% in calculated amnt. to RBF fitted with dean-stark and condenser, reflux until all water has been collected in the trap, let cool. If the HCl salt oils out, simply decant the toluene and add lots of frsh anhydrous acetone to the oily remainder and place in freezer for some hours.

Works everytime, with every amine HCl tried so far...

IndoleAmine · Dreamreader Deluxe

About solidifying HCl - its no crazy talk, you just need something colder than -85.05°C and a suitable cold finger condenser or similar, really nothing special - you could even sublime it under vacuum........ Laughing

From Merck 13th:

Monograph Number: 4815
Title: Hydrogen Chloride
CAS Registry Number: 7647-01-0
CAS Name: Anhydrous hydrochloric acid
Molecular Formula: ClH
Molecular Weight: 36.46.
Percent Composition: Cl 97.24%, H 2.76%
Line Formula: HCl
Literature References: See also Hydrochloric Acid. Produced industrially by the interaction of NaCl and H2SO4; from NaCl, SO2, air and water vapor; by controlled combination of the elements; or as a by-product of the synthesis of chlorinated hydrocarbons: A. C. Cumming, Hydrochloric Acid and Salt Cake (Gurney and Jackson, London, 1923); N. A. Laury, Hydrochloric Acid and Sodium Sulfate (Chem. Catalog Co., New York, 1927); Maude, Chem. Eng. Progress 44, 179 (1948); Faith, Keyes & Clark's Industrial Chemicals, F. A. Lowenheim, M. K. Moran, Eds. (Wiley-Interscience, New York, 4th ed., 1975) pp 454-461. Prepn of pure HCl for research purposes: Hönigschmid et al., Z. Anorg. Allgem. Chem. 163, 315 (1927); Kemp, J. Chem. Ed. 37, 142 (1960); Schmeisser in Handbook of Preparative Inorganic Chemistry vol. 1, G. Brauer, Ed. (Academic Press, New York, 2nd ed., 1963) pp 280-282. Toxicity: K. I. Darmer et al., Am. Ind. Hyg. Assoc. J. 35, 623 (1974). Reviews of prepn and properties: Addison, Lewis in Mellor's Comprehensive Treatise on Inorganic and Theoretical Chemistry vol. II, suppl. I (originally published as suppl. II, part I) 402-475 (1956); Downs, Adams in Comprehensive Inorganic Chemistry vol. 2, J. C. Bailar, Jr. et al., Eds. (Pergamon Press, Oxford, 1973) pp 1280-1329; D. S. Rosenberg in Kirk-Othmer Encyclopedia of Chemical Technology vol. 12 (Wiley-Interscience, New York, 3rd ed., 1980) pp 983-1015.
Properties: Colorless, corrosive, nonflammable gas. Characteristic pungent odor. Fumes in air. d 1.268 (air = 1.000). d 1.639 g/l. mp -114.22°. bp760 -85.05°; bp100 -114.61°; bp10 -137.77°; bp1.0 -154.37°. Critical temp 51.4°; critical pressure 81.6 atm; critical density 0.42 g/ml. nD20 (liquid under pressure) 1.256. Heat capacity at constant volume (15°): 0.1939 cal/g/°C. Heat capacity at constant pressure (15°): 0.1375 cal/g/°C. Heat of vaporization at -85°: 3860 cal/mole; heat of soln (infinite dilution) -17.88 kcal/mole; heat of formation of gas at 25°: -22.063 kcal/mole. Dielectric constant (gas at 0°) 1.0046; dipole moment 1.07. Soly in water (g/100 g H2O): 82.3 (0°); 67.3 (30°); 63.3 (40°); 59.6 (50°); 56.1 (60°). Forms a const boiling mixture: 20.22 g/100 g soln; see Hydrochloric Acid. Soly in methanol (g/100 g soln): 54.6 (-10°); 51.3 (0°); 47.0 (20°); 43.0 (30°); in ethanol: 45.4 (0°); 42.7 (10°); 41.0 (20°); 38.1 (30°); in ether: 37.52 (-10°); 35.6 (0°); 24.9 (20°); 19.47 (30°). LC50 (30 min) in mice, rats: 2142, 5666 ppm (Darmer).
Melting point: mp -114.22°
Boiling point: bp760 -85.05°; bp100 -114.61°; bp10 -137.77°; bp1.0 -154.37°
Index of refraction: nD20 (liquid under pressure) 1.256
Density: d 1.268 (air = 1.000); d 1.639 g/l
Toxicity data: LC50 (30 min) in mice, rats: 2142, 5666 ppm (Darmer)
CAUTION: Potential symptoms of overexposure are irritation of nose, throat and larynx; coughing, choking; dermatitis; direct contact with solutions may cause eye and skin burns; direct contact with liquid may cause frostbite. See NIOSH Pocket Guide to Chemical Hazards (DHHS/NIOSH 97-140, 1997) p 166. See also Patty's Industrial Hygiene and Toxicology vol. 2B, G. D. Clayton, F. E. Clayton, Eds. (Wiley-Interscience, New York, 3rd ed., 1981) pp 2959-2961.
Use: In the manuf of pharmaceutical hydrochlorides, vinyl chloride from acetylene, alkyl chlorides from olefins, and arsenious chloride from arsenious oxide. In the chlorination of rubber, as a gaseous flux for babbitting operations. In organic reactions involving isomerization, polymerization, and alkylation. For making chlorine where economical.

IndoleAmine · Dreamreader Deluxe

No, seriously Wink

:

Maybe try and distill away the acetone from your ibogaine freebase/HCl/H2O mixture, hopefully the acetone will remove the tiny amnt. of H2O azeotropically, and addition af fresh dry acetone will cause precipitation - thats what I would do.
(with making 2C-B.HCl from aequ. HCl, this works wonders!)

nubee · Master Archiver

do the amounts matter ?

loki · guinea pig

i learnt the hard way, in part because this information is not written down anywhere in an explicit exacting form, that hydrochloric acid does not ionise alkaloids very well when it is more concentrated than about 2 moles per litre (it could be a little higher than that i'm not absolutely certain). i think the reason for this is simply because a certain amount of non-acidified water is required to enable these mostly nonpolar substances to dissolve in water, because of the hydrogen - oxygen polarisation that, with insufficient water molecules would interfere with the formation of a surface surrounding the hydrocarbons. I could be mistaken about this but in practice, it has been an ongoing frustration and observation that extracting freebases out of nonpolars does not seem to happen as fast or as completely in concentrated or near concentrated acid, and surface tension (uniform polarisation at the surface of contact between polar and nonpolar substances) seems like the most logical reason behind this, in my opinion.

A solution to this problem is to mix up standardised molarity solutions of HCl (you'll have to do some stochiometry calculations), 0.5M seems to be a good concentration, and then you can get pretty close to accurate ionisation (within a reasonable range) of the alkaloid as a 1:1 salt by using volumes and knowing how much alkaloid you should have there (again more stochiometry). by applying this method systematically i have now learned i can consistently ionise alkaloids into a solution via titration (well, if there's no great concern of a little HCl being caught in it in water caught in a space in the crystal structure one can just estimate and at the end one should only get a brief period of HCl release at the worst)... sounds complicated, i know, but it works SO much better than just throwing a dash of this and a dash of that. this method, possibly with a 0.1M concentration of HCl used instead, could be used to fairly accurately ascertain the yield of alkaloids by progressive small titrations until the pH remains acidic, without using scales (one has to of course convert molarities to milligrams to do this, but cheaper than a scale is a calculator Very Happy

)

edit: oh just two minor points - some alkaloid salts will not crystallise at all no matter what you do (eg, dmt - although lilienthal once said that the oxalate does, and the picrate does too, but totally useless are both for ingestion) and second point some alkaloids break down at the temperatures that would be involved in an atmospheric pressure removal of water. if the alkaloid will not form a crystal you cannot gain anything by attempting to recrystallise it - it will just form a mass of fluffy stuff. there's not much information available as to salts and phase change data on ibogaine either.

edit 2: it would seem logical to me that it probably forms a nice tidy crystalline freebase anyway. consider extracting the freebase into a suitable nonpolar (naptha is probably just fine, although a lazy solvent) then evaporate it down to about 20ml volume (adjust up or down depending on expected amounts of alkaloids) and cover and put in a freezer, should form crystals under these conditions, almost guaranteed to (so long as the alkaloid is in solid phase at the temperature of the freezer, -18 degrees C, and preferably likewise solid at room temperature as well)

IndoleAmine · Dreamreader Deluxe

Loki: this is not much of a problem when you use acetone: everything will mix nicely, water, acid and nonpolar substances...

I can say that large excess of HCl doesn't do any harm when acetone and azeotropic drying are used: but you need to remove the solvent and add fresh one for 2-3 times sometimes until everything crashes out.

..better use only slight excess of HCl 30%, should work well.

If the HCl salt you're planning to make isn't really temperature-sensitive, you could also try to make it by neutralizing with HCl 30%, followed by azeotropic drying with toluene/dean-stark trap (works well with methedrine or MDxA for example)...

i_a