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geezmeister
(Hive Addict)
07-17-02 21:16
No 333934
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Extraction
Technique: Waterless A/B
(Rated as: excellent)
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Waterless A/B extraction of pseudoephedrine from tablets
Abstract of procedure:
reduce pills to powder form
soak 12 hours in non-polar solvent
rinse with acetone
boil in acetone
dry thoroughly
add base
add basing medium (OH, acetone) mix thoroughly
extract with non-polar solvent
gas or extract with aqueous HCl
rinse or acetone flash
recrystalize with ISO OH
Standard Procedure:
1) If using 30 mg pills with red coating, remove the red coating. Grind pills
to powder form. Use a morter and pestle after coffee grinder; texture should
be a fine powder and few coffee grinders get the pills fine enough by
themselves.
2) The powdered pill mass should first be soaked in a non-polar solvent.
Choice of solvent is dictated by the presence of povidone and/or polyethylene
glycol. If povidone is present, mineral turpentine is the solvent of choice;
alternatives include xylene, tolulene, mineral spirits. Suggested time:
twelve hours. If povidone is not present but polyethylene glycol is
present, soak in non-polar solvent for at least six hours. Recommended
solvent: xylene, tolulene, mineral spirits. Decant non-polar solvent.
3) Rinse pill mass with dried acetone, discard acetone. If the pills contain
an antihistamine, place pill mass in pyex dish, cover with two to three times
its volume in dried acetone, bring temperature up slowly with hotplate to a
steady gentle boil with constant ventilation. No open flame or ignition
source may be used. Stir boiling acetone continuously for five minutes,
remove from heat, decant acetone. Spread pill mass and allow to dry to
complete dryness.
4) Weigh out one gram of NaOH for each gram of available pseudoephedrine in
the pill mass. Weigh out one gram of NaCl for each gram of available
pseudoephedrine (rock salt is recommended). Combine and grind in coffee grinder
to fine powder. Take care to avoid inhalation of powdered NaOH! Mix the
combined salt and sodium hydroxide with the dry pill mass and stir with a
glass rod until the mixture is evenly and thoroughly mixed.
5) With the pill mass/ sodium hydroxide/ salt mixture in a pyrex beaker of
sufficient depth to allow the addition of three times the pill mass volume of
non-polar solvent, add very dry isopropyl alcohol in small quantities while
mixing the mass with a glass rod; continue adding alcohol and stirring until
the pill mass has the consistency of a thin paste. The pill mass should heat
slowly during this step. At no time should the mass become too hot to hold
comfortably. If the heat rises quickly and beyond comfortable
temperature to hold, add non-polar solvent immediately. As long as the
temperature does not make a quick surge, work the pill mass for at least ten
minutes to insure all portions of the pill mass have been exposed to the
base. You will observe the color change of the pill mass, most usually to a
medium yellow or light tan/brown shade. This is expected. Dark brown
indicates the presence of excess water but will not impede the process.
6) Add three times the volume of the pill mass with non-polar solvent. Xylene
is recommended. Mix this with the paste very thoroughly, recommended for at
least fifteen minutes. Allow to settle, decant the non-polar solvent. Repeat
this step twice. The amount of mixing and the time period may be shortened
for the last two non-polar soaks. Combine the three volumes of non-polar
solvent used to extract the freebase pseudoephedrine.
7) Wash the non-polar solvent with warm distilled water wash, cool distilled
water wash, and a third warm water wash. Continue washing until the washes
are clean. After the third wash, monitor the pH and do not allow it to fall
below pH 9. If necessary to remove excess sodium ions, do a NaOH wash of the
nonpolar with a 20% NaOH solution.
8) Extract the pseudoephedrine from the non-polar solvent by gassing or by
aqueous HCl addition and evaporation to near dryness, followed with an
acetone "flash."
9) Rinse the collected pseudoephedrine in dry acetone. Dissolve in hot dry
isopropyl alcohol and recrystalize with dry acetone as a second solvent.
Repeat the recrystalization.
Notes and comments:
1) Pill selection: this process was developed with generic antihistamine
tablets with 60 mg pseudoephedrine and 2.5 mg tripolidine. It also is
effective with pseudoephedrine sulphate antihistamine tablets with
cloropheneramine maleate, and changes the form to the salt form for the
reaction. Name brand and generic 120 mg and 240 mg time release
pseudoephedrine tablets may be extracted with the process. Yields for the
above average 60- 66 percent of available pseudoephedrine hydrochloride by weight.
Extraction process yields very clean pseudoephedrine HCl. If the pills are
dry matrix formulation such as the time release 120 mg caplets, it is very
important that every solvent used be as dry as possible and that the pill
mass not be exposed to excess moisture or allowed to remain exposed and
uncovered.
2) The presoak in non-polar solvent is to remove povidone and mineral
turpentine is recommended. Alternatives are soaks in xylene, tolulene,
mineral spirits. Minimum twelve hour soak for any solvent but mineral
turpentine. If povidone is not listed and you are familiar with the pills and
have not encountered povidone in them even though unlisted, a soak in any of
the other suggested non-polar solvents is done to remove polyethylene glycol.
Six hours is sufficient; shorter times may be effective but have not been
tested by the author. PEG should be soluble in any of the nonpolar solvents,
but if the pills are the 120 time release formulation (or the "dry
matrix" formulation) the author strongly suggests xylene be used.
3) The acetone rinse is to rid the pill mass of the non-polar solvent.
The following acetone boil is to remove tripolidine or chloropheneramine
maleate. If there are no antihistamines present in the formula, the acetone
boil is unnecessary and should not be done. Do not boil the pill mass with
the solvent, or with the solvent and acetone combined. Rinse the solvent and
then use fresh acetone to boil. Yield seems to be better is the entire pill
mass is allowed to dry thoroughly before the addition of base. Drying in the
microwave on less than full power is effective, although not particularly
recommended. Drying in an electric oven at low temperature, not to exceed 150
degrees F if also effective to dry the pill mass.
4) If the pill mass is in the least clumpy or hard, grind it to powder again
before proceeding. NaOH may be used to base. Gram per gram is probably an
excess of NaOH, but it does effect the basing. Sodium carbonate has been used
with good success and it provides fewer contaminants to the non-polar solvent
that need to be washed out. Baking soda baked completely dry-- 350 degrees
for thirty minutes in a shallow dish should be sufficient, yields sodium
carbonate. pH Down at the pool store is sodium carbonate and may also be used
for the process. Salt is recommended as an addition to the lye as it provides
a moisture absorbing substance to help prevent the lye from absorbing
moisture immediately on powdering. Lye can be used without grinding it;
powdered NaOH seems to give better performance.
5) The selection of solvents to mobilize the HCl is one of choice. On the
antihistamine type pills, MeOH may be used, but is not recommended. Very dry
ISO alcohol is one recommendation, although dry acetone seems to work very
well. If the pills are time release or dry matrix formulation, dryness is
essential to yield. Dry acetone is highly recommended. The addition of the
solvent should be a little at a time, working the pill mass until a slightly
thin paste is achieved. Water, including moisture in alcohol or acetone, will
tend to speed the basing process up and if NaOH is used it can become hot too
quickly and damage the pseudoephedrine. Care should be taken to select dry
solvents. Working the mass thoroughly is thought to be important to yield.
Too much alcohol can impede the a/b process, and the amount used should be
carefully tailored to avoid making the pill mass runny and diluting the
non-polar solvent with alcohol.
6) Xylene is the author's preferred non-polar solvent for extracting the
freebase pseudoephedrine as it is unlikely to contain any significant amount
of water straight from the can, or even after having been used. It is
considered to be the solvent of choice for dry matrix formulations. Tolulene
and Mineral Spirits have been used with equivalent success. Naptha is not a
recommended solvent for this purpose.
7) The washes will rid the non-polar solvent of any color they aquire from
the pill mass and excess sodium ions. Wash until clean. Save the water washes
to check for pseudo freebase that may hitch a ride in the water. It can
happen.
Advantages: works with most pills; safer than solvent boiling
techniques; fewer solvents used; less odor; pseudoephedrine HCl obtained is
very clean and has fewer impurities that affect the reaction, contaminate the
red phosphorous, or contribute to yield loss.
Disadvantages: complex for those unfamiliar with a/b process; risk of
damage to the pseudoephedrine during the basing process; low yields if done
improperly or too much alcohol used; may allow polyethylene glycol or
povidone to be extracted with the pseudoephedrine if proper soaking is not
done; some report limited yields with the process.
Known to be effective with pills containg the following ingredients:
Pseudoephedrine HCl 60 mg
Tripolidine 2.5 mg
corn starch
Flavor
Hydroxypropyl Methylcellulose
lactose
Magnesium Stearate
Polyethylene glycol
potato starch
povidone
sucrose
titanium dioxide
patent no. 5098715
210CA01
__________________________
Pseudoephedrine HCl 60 mg
Tripolidine 2.5 mg
Hydroxypropyl Methylcellulose
Magnesium Stearate
Polyethylene glycol
starch
titanium dioxide
may also contain:
cellulose
Dioctyl Sodium Sulfosuccinate
Hydroxypropyl cellulose
lactose
Polysorbate 80
povidone
powdered cellulose
pregelatinized starch
silica gel
silicon dioxide
sodium starch glycolate
stearic acid
_______________________________
Pseudoephedrine HCl 60 mg
Tripolidine 2.5 mg
carnuba wax
corn starch
flavor
Hydroxypropyl Methylcellulose
lactose
Magnesium Stearate
Polyethylene glycol
povidone
sucrose
_________________________________
Pseudoephedrine Hcl 120 mg
Candellia Wax
Hydroxypropyl Methylcellulose
Magnesium Stearate
Microcrystalline Cellulose
Polyethylene glycol
povidone
titanium dioxide
Pseudoephedrine Hcl 240 mg
Candellia Wax
Hydroxypropyl Methylcellulose
Magnesium Stearate
Microcrystalline Cellulose
Polyethylene glycol
povidone
titanium dioxide
Brand names:
withheld pending further notice regarding board policy
An
education is what's left when you've forgotten what you learned.
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Aurelius
(Hive Bee)
07-17-02 21:39
No 333944
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basification
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how does the NaOH (presumed base) react with the HCl salt if no water is
present? is there enough surface contact to cause a solid state
reaction? just wondering here. (or perhaps the NP solves enough
of the base little by little to react with the HCl.
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Aurelius
(Hive Bee)
07-17-02 21:42
No 333946
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should
read
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sorry, should have read the actual procedure first. the alcohol solves
the base for reaction.
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raffike
(Hive Bee)
07-17-02 22:31
No 333964
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But
how one does A/B with acetone and NP.
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But how one does A/B with acetone and NP.NP is usually miscible with acetone
and alcohol
A
friend with speed is a friend indeed
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jacks_addiction
(Stranger)
07-18-02 01:04
No 334005
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Extraction
Technique
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Thanks Geez - You rock! Exactly what I was needing!
I am
Jack's addiction... Jack gets me drugs, I keep Jack happy...
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Hematite
(Individual)
07-18-02 01:23
No 334014
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The
suggested addition of iso/acetone after ...
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The suggested addition of iso/acetone after mixing of the pill powder(now
completely dried) as I read it, was only as a medium for the base to come in
contact with all the desired product and prepare it for an effective
extraction into the non polar solvent then added. If I understand this
correctly then being miscible with the non polar solvent would in fact be
advantageous.
Regards,
Hematite.
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BenWiFFen
(Line Monitor)
07-18-02 04:59
No 334095
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geez
what a nice job.
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The part about recrystalizing with acetone. How'z that going to happen? It
doesn't dissolve in acetone.
Give me
libreum or give me Meth
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geezmeister
(Hive Addict)
07-18-02 06:04
No 334105
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notes
2
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Hematite: correct on the miscibility of the medium used to base. In fact, it
can be allowed to dry before the non-polar is added. Its use is to facilitate
the mobilization of the salt from the pseudoephedrine molecule, and once
freebased the molecule will remain that way whether the powder is still damp
with the basing medium or not.
Ben: the acetone is the second solvent used when recrystalizing the
pseudoephedrine in isopropyl alcohol and gives contaminants a fluid to
migrate into as the crystals form. This is standard dual solvent
recrystalization.
An
education is what's left when you've forgotten what you learned. Standard
dual solvent recrystalization.
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BooWho
(Hive Bee)
07-18-02 10:38
No 334190
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Hot
Damn!!!
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Way to go!! Excellent posting!! Will be used extensively.
boo
Three
or more days of meth, no sleep, no food, and dehydration invites a psychotic
episode.
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SQUIDIPPY
(Hive Addict)
07-18-02 12:33
No 334224
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Forget
12 hours
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If pills are brought to almost a boil in mineral spirits, and then rinnnnsed
with acetone, long oal periods are not necessary, at least as far as povidone
is concerned.
I'm keeping my eye on you !
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dwarfer
(Hive Addict)
07-18-02 14:54
No 334271
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NaOH
plus acetone or OH
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I was unaware that you could basify acetone enough
to get the salt undone, but if you can, it is bitchin'.
(I've never tried, like I said: what pH does indicator
paper show the pH of sat. 'tone to be????)
I know that NaOH saturated ISO-OH has some advantages
in some situations because it will not "overdo" the
basing for some situations.
Good job, Geeze.
I appreciate the new info..
dwarfer
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platcat
(Stranger)
07-18-02 21:01
No 334422
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povidone
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Is Ibee understanding correctly; povidone is included but not listed
sometimes???And if so how whould Ibee know without wasting too much time and
solvents unnessessarily. Also- is the red a big problem to leave in if it
leaves in the A/B ?What about TCE?? No longer needed??This tired bee goin to
bed.Time management problems.Gnite bee's.tomorrow is another day in the
life. LOL
"The
crux of the biscuit is the apostrophe"FZ
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geezmeister
(Hive Addict)
07-19-02 06:35
No 334574
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acetone
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Dwarfer: Acetone works very well. Former_chemist recommended it and SWIG
tried it with sodium carbonate to good result. VideoEditor suggested
powdering the NaOH and adding salt to absorb moisture--as powdered NaOH does
grab moisture from the air, it seems. SWIG has not replaced the sensor on his
pH meter and assumes it is defective and has done the basing by measurement
and watched the color change and temp release to know he's there. You aren't
really using the acetone for anything but a medium to get the NaOH in contact
with the pseudo. Another tip from VideoEditor about drying the pill mass
after basing seemed to work well, also, and the yield increased by six
percent. Note that the NaOH is added to the dry pill mass, and both are in
powdered form and mixed well before the acetone or alcohol is added. Minimal
amounts of acetone or alcohol are used, the exact quantity used depends on
how much it takes to make a fairly thin, mixable paste of the gups. The
dryness of the basing medium is of partiuclar importance on the time release
version of the pills.
Platcat: This particular technique does not rely on TCE, and at least with
the non-polar pre-soak seems to bypass the gakks TCE was employed against.
An
education is what's left when you've forgotten what you learned.
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dwarfer
(Hive Addict)
07-19-02 14:16
No 334733
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sounds
good to me
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Well, it does not matter what the pH is, since it works.
Did I read correctly that NaCarbonate would also work??
If it does why do you use NaOH, with it's (slight) problems??
I know that drying things in the micro, including GUPS,
has made a significant difference:
I also have been doing an A/B process with dry feedstock
and NaCO blended in the coffee grinder, and then touched with alcohol.
This would work even better (your technique )
I think, with acetone..
=============
Your tech. also improves what I had been doing
in your measuring out the gram to gram ratio
between NaOH and pseudo, as I had been rinsing the
base
with water to remove the large excess I was using.
(why, I don't know,actually "":<( )
Anyway, I am of the opinion, but maybe wrong,
that adding the NaCl won't take it (the water) out
of the (potential) reaction, and would suggest warming
the NaOH by heat or micro. (but if NaCO works, that would be
"groovier"..)
former_chemist is a good addition to the mix, for sure.
":<)
dwarfer
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Scottydog
(Hive Bee)
07-19-02 16:09
No 334802
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Sodium
Carbonate and MS as the NP
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Yes Sodium Carbonate works great!! In theory when mixed (equal weight) gram
to gram with pseudo feed-stock upon adding the ISO IPA.. Theoretically one
can look down into the preferred glass container and watch it bubbling away
doing its thing. 
By adding 1 teaspoon of NaOH to the thin paste with additional stirring the
ph will go up to 12+. No real need to even take a ph reading at this point.
The (top layer) NP can be syphoned, rinsed with dh20, and HCL titrated with
fresh water and evapped and crashed with tone... Thereby liberating pristine,
rhombic needles. 
Swis has found that pre-soaking with Mineral Spirits and later using the MS
as the actual NP in this waterless a/b extraction technique works great as
well.
Many soak with it, but how many bees have actually used Mineral Spirits as
the Nonpolar?? Cheapest NP around...(IMHO)
___________
Refuse/Resist
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acid_egg
(Hive Bee)
07-19-02 17:11
No 334827
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Getting
the PEG out
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[extract from merck index]
7729. Polyethylene Glycol.
Clear, viscous liquids or white solids
which dissolve in water forming transparent solns. Sol in many organic
solvents.
Readily
sol in aromatic hydrocarbons. Only slightly sol in aliphatic
hydrocarbons.
Do not hydrolyze or deteriorate on storage,
will not support mold growth. Solvent action on some
plastics. Polyethylene glycols are compds of low toxicity: Smyth
et al.,
J. Am. Pharm. Assoc., Sci. Ed. 39, 349 (1950). Toxicity data
(PEG 400): W. Bartsch et al., Arzneimittel-Forsch. 26, 1581
(1976).
Mineral spirits are suggested for step 2 and although this has been discussed
before,it appears there is confusion about what is what(mineral
sprits,mineral tupentine,turpentine).According to this extract from merck,
aromatic hydrocarbons are what you want to take out the PEG so toluene and
xylene are obviously good but if you go OTC ensure your solvent is an
aromatic and not aliphatic based solvent.
You should determine which is which for where you are.
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Scottydog
(Hive Bee)
07-19-02 20:42
No 334910
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Changing
composition of "Paint thinners"
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With the United States largest retailer changing the composition of their
"Paint Thinner" product from 100% Mineral Spirits to Petroleum
Distillates (Naptha?) in Swis' area... Or was it nationwide? This is some
very good advice acid_egg!
Read your labels bees! Make sure you are truelly purchasing the solvent that
you want/need.
This retailer went from a 1 gallon white plastic container to a see-through
clear plastic container.
But then again with kerplunking this "supposed" new substitute will
also work! Jokes
on them... God I'd hate to work in that paint dept. The employees just got
through pulling the old composition from the shelves. Swis has a strange
feeling that they will be pulling the new composition from the shelves as
fast as it was stocked.
Either that or the corporation will not meet their quarterly projections
concerning generated profits, the product will sit on the shelves forever and
they can thank the feds that they are so obviously cooperating with...LOL
With the new headquarters for the "Northern Command" Homeland
Security being in close proximity, (Effective April 19th) they must not be
too happy about tweekers running amuck.
____________
Refuse/Resist
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foxy2
(Distinctive Doe)
07-20-02 09:00
No 335083
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yes
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Mineral spirits (aka charcoal lighter fluid)
Xylene/tolly
dry tone
That is the correct order to purchase your solvents.
Hmmm
What goes along with charcoal lighter fluid?
Why matches, OF COURSE!!!
Stealth mode...........
Those
who give up essential liberties for temporary safety deserve neither liberty
nor safety
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BenWiFFen
(Line Monitor)
07-20-02 17:07
No 335267
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Always
ready to learn
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I've always used acetone to wash my gear. Then let it dry. Before useing
something else to recrystalize it. Is this what you're calling a dual
solvent? Never have tryed to leave the impression of a chem trained
Bee. I think one of the best things about the Hive is it's a place were a self
taught and a school taught person can exchange ideas and methodes. 100.000
eyes are better then two.
Help
i'm a Rock. Frank Z
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geezmeister
(Hive Addict)
07-20-02 18:04
No 335300
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does
work
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Dwarfer:
Sodium carbonate does work, it brings the pseudo HCl right to the needed pH
level. (Being unable to be moderate in most anything, basing included, I
could never resist the urge to add those few extra point with a little NaOH.)
NaOH works every time, but as you note it has its risks and its drawbacks. IF
I had a jug of sodium carbonate on the shelf, I'd use it, and I may buy some
the next time I go to the pool store, which I don't do anymore, since I sold
the place with the pool because of the neighbor with a badge and a good nose.
The NaCl is used when powdering the NaOH to keep the NaOH from absorbing
moisture in the air. It tends to do that right now in my experience.
It is a precaution, and that is all.
Dry acetone worked and has worked each time I used it for this purpose. I
think the two choices are dry acetone and dry ISO alcohol. MeOH would work
but even in the yellow bottle it tends to have enough moisture to hurry
things up too much.
I also agree with your note on former-chemist.
Platcat: On the question about the 30 mg red hots. SWIG has never tried
running the name brand red hots through this process without deredding. He
cannot answer as to its success. He has run the generic, dull red coat red
hots as part of the batch without removing the red, with no noticeable
problem. He could not say this result would be true if they made up the
entire pill mass. He lacks the actual hands on, been-there-done-that
knowledge to answer the question.
Ben-- the principal solvent in the recrystalization is dry alcohol. Some dry
acetone is added to the saturated alcohol and the crystals form in the
alcohol/acetone bath. The crystals will crash out of straight alcohol as it
cools, but if there is much trash and dirt in the powder you want to grow
crystals from, having a second solvent in the mix gives the trash a place to
go other than the first solvent or the crystal itself.
An
education is what's left when you've forgotten what you learned.
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geezmeister
(Hive Addict)
07-20-02 19:17
No 335333
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PEG
and turps
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Acid-egg: The mineral turps that SWIG uses is a xylene based solvent with
turpenes added, sold by America's biggest retailer as turpentine substitute.
It will get the povidone out, and it will also pull the PEG. In SWIG's quest
to avoid povidone, he shifted to pills with PEG, skipped the turps soak, and
got hammered by the PEG. The note about mineral turps refers to a
xylene-based solvent with turpenes.
An
education is what's left when you've forgotten what you learned.
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platcat
(Stranger)
07-20-02 20:56
No 335358
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get
the red out
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Thanks Geez, after 24+ hrs soak most of the red is dull to gone.
Seems like 2 different batches from identical boxes.some were shiny and very
hard. No povidone was listed. Just PEG,carnauba wax,hydropropyl
methylcellulose,dicalcium phosphate,magnesium stearate,microcrystaline cellulose,polysorbate
80,silicon and titanium dioxide and the FD&C red#40.These reds were
generic (big)store brand.The tone seemed to be saturated with red so
swip changed it and put it back to soak after shaking the crap out of it for
the umteenth time.First soak was 400ml. maybee swip is stingy with his
solvent?Was approx 125% volumn of reds .Should swip bee concerned about
the extended soak time.Swip is a patient bee.Good honey is worth the
wait.
"The
crux of the biscuit is the apostrophe"FZ
Are we there yet?
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former_chemist
(Hive Bee)
07-20-02 23:30
No 335393
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Acidifying
Acetone
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Dry acetone won't dissolve the sodium hydroxide so the solution isn't really
basic. BUT and this is the kicker. Acetone will dissolve pseudo
HCl slightly (less than 1%) so that it reacts with the base. In a well
mixed powder this works well. Acetone containing pseudo base dissolves
pseudo HCl better so it kind of feeds on itself. It isn't really basing the
pseudo HCl, It is acidifying the NaOH. Freaky way to think of it but it
works.
Thanks for the kudos guys 
After a little research, Toluene and Xylene both have limiting moisture
contents close to .01%. The solubilities are very similar which is to
be expected since they are similar chemically. Moist toluene seems to
absorb amine salts better than xylene though (no quantitative available).
Soaking with the solvent you intend to use for base removal will ensure that
almost no nasties are left that will follow the base. Triprolidine and
Chlorpheramine are exceptions here since they are amine salts.
Incomplete soaking will leave stuff naturally. And other things may be
pH sensitive.
One good reason to use a little lye at the end of the basing with sodium
carbonate is that amines can form carbonates. Mixing sodium carbonate
and an amine HCl isn't a good way to make amine carbonates so it isn't a heavy
side reaction but a little lye seems likely to increase yields.
Has anyone come across polymethyl methacrylate copolymers yet? I have
seen literature but no actual box labels with these things. After a
little research, these things should be soluble in acetone even in a hydrochloride
state. Since this nasty isn't showing its head around here actual data
is sorely lacking.
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platcat
(Stranger)
07-21-02 13:50
No 335542
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red
out
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Thanx bee's, Swip was pointed to a old post(2001) about a couple ml's of H2O
to help get the red out and it does as claimed. This bee humbled. thanx
again.
"The
crux of the biscuit is the apostrophe"FZ
Are we there yet?
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dwarfer
(Hive Addict)
07-22-02 14:24
No 335897
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Thanks
former-chem
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You can see my ?? about NaOH basifying acetone, but my capitulation to the
fact that "if it works, screw what I
think.."
so you have provided a melding rationalle for the conundrum's resolution.
":<)
Not that I totally understand it, but I'll give it a try.
sounds like the acetone acts as a "transfer agent",
asissting in the reaction that way, although I really thought you had to have
both components soluable, and
some hydrolysis or ionization of the carrier media
to be effective: thus you can understand my continuing confusion...??
It's difficult getting acetone truly dry (and keeping it that way), so that
could be a factor, maybe, too?
If it's acidifying the NaOH, then seems to me adding NaCL
also
would tend to restrict the basing operation.
Also, will NaCl dry NaOH??
Poly methyl methacrylate?? Makes the particles
stick to each other, in super fashion??
=============
Povidone separtes and dissolves, or is destroyed, in dry acetone
at 100C.
==========
dwarfer
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grokstar
(Newbee)
07-22-02 21:55
No 336031
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Groks
2 cents
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I love the sound of this waterless A/B. G always phuckz up adding
NaOH, his hydro ph meter phreaks out. He has suffered yields of
around 50% with CM sulphates, so picking up that extra with less
mess, less fuss, looks very promising indeed!! And the
people at the 24hr supermarket always look funny at me buying bottles of dh2o
at 3 in the morning.
F.Y.I.
Acetone boiling :- Put your flask in a pot or something filled with
boiling water. Remind you of anything???
rockin
the hive with the Jungle Rhythm flavour
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former_chemist
(Hive Bee)
07-22-02 22:18
No 336038
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Dual
phase reactions
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Dwarfer: As long as one component of the reaction can be 'mobile', the second
component doesn't have to be. It certainly speeds the reaction if one
product precipitates out. Reaction products can 'poison' the
reaction. In this case the NaCl product is not any more soluble than
the NaOH so you don't have that problem. If the amine prevented further
solution of the amine base that would prevent it from working but the
opposite effect actually happens.
Not certain if moisture actually has to be present for NaOH to react with
HCl. NaOH is VERY hydroscopic so it probably contains all that it would
need. The kenetics strongly favor salt and free base. Adding a
drop or two of water to the acetone might speed the reaction but some of the
other nasties might start acting up.
I don't know for sure but you could probably detonate ammonium chloride mixed
with lye. Doesn't sound like a safe reaction to try. Anyone up
for one of those Darwinian Awards? 
How about we start a forum of all the things we wonder about but would really
rather not die from.
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dwarfer
(Hive Addict)
07-23-02 14:10
No 336218
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How
about THIS, apologies to Flinger
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If I had the time I'd look up what post of amethystium,drudge,flinger or
which-whomeverit was that
made me conjure up this thought question,
but here it is..
============
Would the process work with calcium hydroxide?
I'd never have thought about it, being close to insoluble
in water, but it comes as a nice white finely divided non
deliquescent non-amide compound forming material which, if it can be
"acidified" thru the same mechanism, may have some advantages.
Hmm: but CaCl is hygroscopic... so if it were to work it should be done in a
sealed containter.??
speculation, the mother of invention?? and disappointment.. 
dwarfer
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foxy2
(Distinctive Doe)
07-23-02 14:19
No 336223
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Step
further
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barium hydroxide
Those
who give up essential liberties for temporary safety deserve neither liberty
nor safety
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dwarfer
(Hive Addict)
07-23-02 19:47
No 336339
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sounds
enema-ish to me
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ewwww
dwarfer
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former_chemist
(Hive Bee)
07-23-02 22:32
No 336386
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Other
compounds to acidify
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CaCl2 will lock up the alcohol if you use Ca(OH)2 and
alcohol. Shouldn't be a problem with the acetone though. Dunno about
the barium hydroxide.
Calcium hydroxide is used in canning foods (pickling lime) so it is easy to
get USP grade. Might be good to try sodium carbonate from baked baking
soda and pickling lime instead of lye. The lime has a much higher
affinity for the CO2.
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grokstar
(Newbee)
07-30-02 23:17
No 339267
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Waterless
A/B thumbs up!! Beautiful Colours
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With a little trepidation I tried out this waterless A/B.
Without going into too much detail -
blue 60 mg CM sulphates
Turps soaked 12 hr. Washed with tone.
2 tone boils(by putting open jar in a pot of boiling water)
Dried and crushed the pill mass. Still seemed to smell slightly of
turps but whatever.
Crushed up Rock salt, then NaOH, then crushed together.
Mixed all this in good and proper to the crushed pill mass.
Now, the scary part -> slopped in a bit of iso and mixed.
Nothing much happened. Poured a bit more and mixed. hmmm not
much. Then poured enough in all at once to form a thin paste. The
pillmass started turning deep mauve. Did I add too much I
wondered. Panicked and slopped in some dry tol.
After stirring, pill mass and tol turned bright pink!!!
Quite impressive(but a little scary). Anyway, let settle,
decanted. Repeated twice more. By the end the pill mass had
turned yellow/orange, and the extracted tol was an orangy pink colour.
Washed the Tol with dH20.3x cold warm cold. The wash water came
out a lovely deep purple. My wife was suitably impressed as purple is
her favourite colour. You know you have washed enough when no more
colour appears in the tol or the wash.
Then did the HCl thang.
After evapping and tone crashing there where needles galore,
and being impatient I poured out the tone into a different dish after about
an hour in the fridge so I could admire these crystals. Kind of
boiled the tone off the other dish a bit then crashed it again to yield a
heap more pfed.
Haven`t yet weighed it, but seems to be better than usual.
And, the best thing ->
I only used 1 filter paper for the last drips of the 3rd tol extraction of
the orig pill mass.
Spirits
of earth bring unto me
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