posted 08-31-99 07:44 PM         

What is the density of mircocrystalline cellouse? Is it more or less than water? More or less than naphtalene? More or less than toluene? Etc, etc?

This would be very helpful because, to my knowledge, the cellouse isn't soluble in anything. If you knew the density you could create a two phase system such that the cellouse would position itself for easy removal.
For example, if MircoCrstaline cellouse was less dense than water you could have the ephedrine salt in an aqueos phase and the microcrstalline cellouse would be floating in it. Then you could add an organic solvent with a density between that of the water and the mircocrstalline cellouse so that you could skim off the mircocrstalline cellouse with a cup (or you could just use a sepatory funnel to drain the ephedrine bound layer).

The advantage of useing the above sceam is that you wouldn't have to wait forever for a solution to drain through a filter and you wouldn't have any particles leak through the filter either.

posted 08-31-99 08:21 PM         

==========================

From a more confident position (direct testimony of a near and dear friend) i can state that if the product is just contaminated with this, getting around it is really easy, as i described in "filter flask for otc's". (originator darf)

You can get pure freebase by extracting in an alcohol "(I sure like blenders), sand filter followed with alcohol wash, add only NaOH (or equivalent) to the alcohol to around pH 12.5, (no water!), xylene, decant, xylene wash, decant, evaporate warm or leave in the sun.

Truth is you do not even have to decant the xylene: just put the whole mary ann in a tray and any more junk (mostly in alky level) will be distributed across the tray and the FB will roll into the corner if the tray is inclined.

If'n you have other crap in there, like povidone or wax: the freezer will in 24 hours agglomerate the povidone and allow selective siphening of the wax free material.

I had hoped that cold filtering would get rid of the wax entirely but 'twas not to be.

For serious filter freaks I recommend investing in a 10 year supply of #60 grit sand from your neighborhood sandblast supply store: $20 or so for 50 lbs.

You may use your expensive low pass and high pass 200 mm filter paper again one day, but not fer this process, I betcha.

posted 08-31-99 10:54 PM         

Got some data downloading.............
DESCRIPTION: SANCEL is purified partially depolymerized ALPHA CELLULOSE. It is White to off white, Odourless, Tasteless, Free from Organic and inorganic Contaminations. It is insoluble in Water, dilute Acids, and in mostly all organic solvents. Practically insoluble in Sodium Hydroxide solution. SANCEL, which has now become a synonymous name in pharmaceutical industries, is a must for quality as well as quantity products.

It is seemingly insoluable..............

"mostly all organic solvents"

its real small..........70um-30um

Good luck with the filter idea guys!

posted 09-01-99 01:56 AM         

Certainly most of us have tried the flter paper idea, or the original "filter through two compressed cotton balls for 24 hours or so" (I paraphrase, to be sure: ) and have been more or less disgusted pissed off or at the least impatient at the progress or lack of it with these processes.

The people who put this microfiber in the mix I am sure principally had the idea of foiling the filtration process: and although it does indeed work well for fouling filter media of the common type, the three dimensional sand filter structure is very effective in ridding the blend of the fibers.

I do not doubt that each fiber might in fact be in the micro or nano or pico or whatever smallness range "per each", but either thru polarity, or charge, or some other characteristic it agglomerates or otherwise configures itself into removeable masses.

This is so easily found through simple and cheap experiment that I am perplexed on your "good luck with the filter idea guys." comment.

If you have tried it you know it works. If you have not your theoretical considerations like I said are worthy of note but fly in the face of direct experience I and others have had.

I implore you to give it a try and then critique and improve the process.

Your other concerns expressed elsewhere about foreign inclusions modifying the structure of the molecule are of interest to me: if you have some evidence or facts about that i certinly stand by to be educated in that regard.

Thanks for your creative broad form input on so many ideas, FMAN: on this one I disagree with you.

posted 09-01-99 05:27 AM         

It shrinks when dry to very small.
Small enough to get thru the coffee filters.

So it is not that MCC dissolves in acetone, but that acetone does not dissolve ephedrine Yet still has the mechanical effect of a rinse.
Acetone is easy to work with.

The Micro crystaline cellulose appears as tiny white spects floating near the bottom of the acetone wash, given a bit of time it grows spidery legs, given even more time it forms a pulpy slime on the bottom of the acetone.
So if the pills are washed with acetone when dry, when the MCC is small, then it slides through the filter into your trap

posted 09-01-99 10:59 AM         

I have no further interest in the freebase once the extraction is made: the joy of obviating the cloying effects of the pill manufacturers brings transcendent radience to my visage: and both brightens my day and lightens my step as I carom through my daily chores.

The Worlockian methodology herein understood by me for the 1st time, to wash away the unexpanded nauseuum prior to its absorbtion and expansion of polar substances, through filters, using a solvent that does NOT take up the ephedrine or pseudoephedrine, is clear now.

This is significantly different than what I had said of my understanding of this technique in my first response to Chem Man above: thus once more demonstrating the inappropriateness of trying to speak for another person anent their patented, or at least copyrighted, extractive methodologiess.

in truth, (well, kinda ) i thought Worlock's trek into the Sonoran Outback in search of botanical specimens would keep him out for several weeks: thus I had the termerity to speak of his method.

posted 09-01-99 12:08 PM         

Anyway, as compared to sliding through the microfibers 'afore they expand, in contrast my procedure expands the bejesus out of them in alcohol, and filters them: and then washes the filtered fibrs with more alky to be sure none of the pre-nectar gets entwined in the sand/fiber mass. Frankly some fibers do get through although in very small amounts with the 60 mesh sand.

But then in basifying the alcohol and extracting with xylene (and I've tried salting the alcohol but could not note additional productivity) there ain't nothin' in the evaporated xylene 'cept clear amber-yellow oil in a damnsite better yield than I've ever gotten thru any other technique.

I have not tried the Wor-mans technique: I think you get the .HCl usually. I presume the laborious act of removing the powder from the filter paper, with it's myriad interstices, must be undertaken: (sigh!) once more resort to the camel hair flagellae he uses so frequently is politic.

Just kidding: the artful brushes he uses I'm sure have other employment as well: the next great southwestern landscape painter may be a'borning amongst us even as we metaphorically speak.

I propose an experiment to be done by someone with decent scale: perhaps by Worlock himself: whose lizard like scales are known to eczema experts around the...: wait:: I digress.

I propose an experiment, mayhap by Worlock, whose veracity is unbesmirched by innuendo:

wherein he obtains maybe 20 of the 24 hour MCC laden specials, and following pre-publicized protocols extracts value from the puck shaped perforated plastic [Oh my god: plastic!! Hope it isn't {gag} the dreaded
p o l y c a r b o n a te !!] pills, measures the results, applies equivalence conversion factors to the freebase/.hcl dichotomy, and lets us know which is bestest.

in that manner, truth will manifest once more.

And should his technique edge mine out through some slight of hand or may be (unlikely) because it IS better, then you can be sure that I will immediatly revert to true form, and whine about how much easier my technique is, and cheaper too, avoiding as it does the exorbitant cost of the filter paper and camel hair brushes.

A feeble solace it may provide me to seek shelter under these winsome excuses: but dwarves are small, and it takes little break to shield them from the glare of the brightened sun.

posted 09-03-99 04:42 AM         

So I only offer this as a slap to the silly grin I see coming from the D section.

I am awaiting the delivery to a remote location of a 50 ml burette with an attachement that acts as a stopping valve.
The long thin design of the burette is adventageous to the sand filtering process,
One must understand the difficulty of adding additional equipment, cleaning, and operating.
There is also a certain reluctance to bring raw dirt into the lab.

Add an inappropriate fear of getting any polcarbonate dust and goos into the product.
One day the sand filter will become the device of choice.

The support of the device is shakey and
I'm too lazy to go scoop up the sand.
The clean up afterwords is a sin

posted 09-03-99 03:17 PM         

As regards the burette: hell, I've got an extry one I'll send to you just cause like I said you'se is a nice guy.

Maybe I'll swap you for one of your hoes??

Believe you know my addy should you wish to part with a hoe.

Just kidding I don't need no stinking hoe: Its yours fer the askin.

(PS: Have to get yer own burette brush. )

posted 09-03-99 03:21 PM         

(PS: they have been in intimate contact with the adjacent polycarbonate containers, so may have picked up some bad habits.)

posted 09-09-99 04:19 PM         

Any practical experience here? What does your sand filter look like, dwarfer?

Worlocks method seems a little sketchy though. He says that the MMC expands when acetone is added, but then he says that the MMC in acetone passes thorugh the filter because it doesn't expand. ?

posted 09-09-99 07:56 PM         

I didn't think "chromatography column" had the same ring as common old sand filter.

Plus, it does act as a filter with other materials, such as the infamous dark green grunge associated with plant fiber extractions.

When the top gets plugged, as it will, you just mechanically stir the top inch or so: probably the equivalent of 20 or 30 standard filter changes.

I suspect that the MC is polar and that is why it hangs in the interstices longer.

I always wash the filter with a couple hundred ML of solvent: alky or xylene: and even the fresh system flush does not get the MC "stain" anywhere close to the bottom.

The "funnel" is a 2 liter polycarbonate 7-UP bottle with the plastic protruding "ring around the collar" removed, and with about 20 small drill holes in the cap.

The bottom end is removed.

Because the ring is removed, it can be inserted in a larger mouthed polycarbonate bottle and be stable.

The column height of the sand is about 6 to 8 inches from upside down lid to the top of the sand: and it will hold I estimate 500 to 600 CC above that.

You can see the filtration/chromatograpy percolation process thru the clear side of the bottle: based on that, I would really say that 6 or 8 inches of sand is "overkill": but sand is cheap....

I know it has changed my life for the better: I'm getting significantly increased yields.

Usta spend 2/3 of the time getting the stuff ready for an experiment: now it's trivial.

the two best improvements for me were:

1. The sand filter
and
2. Getting away from gassing of the precursor: waste of time IMHO and mostly you wanna have the FB anyway.

and if I was to list #3 it would be avoidance of using water.

and if I was to list # 4 it would be understanding the value of the freezer in some separations.

Jesus: this was gonna be a short answer.

Toolate.

posted 09-10-99 11:52 AM         

Dr. Faustus,
_____________
The glass beads, any idea on the grain sizes and purity, especially lack of salts. I would think that they must be fairly salt free, depending on the type of glass used to make them.

I have an idea that is at least close to kewl stuff that
FMAN kicks out, check this out.
________

Not being familiar with the reaction I only offer this to you to consider if it has a possible application, zinc lithium ammonia reaction just consider a burette packet with glass wool then a dry chemical, more wool a second chemical , wool , and zinc on top.
Through a funnel HCl is introduced to the top of the buret, allowed to react and pass into the next chemical and so on, with un reacted HCl passing out the bottom, a drying solvent is then run through to clear out this or that , ammonia then run down the buret to complete the reaction, toss in a couple of electrodes, a very small distillation unit and nay be a vacuum chamber .

CHEM GUY
__________
Your appraisal of the MCC removal technique presented is a fair rebuke of the method.
What's wrong, you feeling OK, no innuendos no hypothetical scenarios, your being too good, maybe you have a slight fever or something. Don't worry you get back to the old self soon enough.

The MCC( Microcrystaline Cellulose) hypothesis(laced with facts) is this.
1) microcrystalline cellulose predominantly coarse particulate aggregates, typically having a mean size range of about 15 to 40 microns.(it will pass through a coffee filter.)

2) In nature, several microcrystals are hinged together and surrounded by amorphous cellulose to form a cellulose microfibril. If the amorphous cellulose is removed, the resultant product is called level off DP (Degree of Polymerization) microcrystalline cellulose.

3) A long chain of glucose molecules 250 in length is similar to a starch or a little bit like cellulose itself except cellulose is highly branched. MCC does not necessarily have the same solubility.

4) solubility in a solvent and ability to adsorb molecules on the surface of a molecule are quite similar concepts, but solubility is indicative of a molecule being inseparable from its solvent, at least via filtration mainly because of its ionic relationship with the solvent.

I suggest that perhaps MCC is very much like cellulose, except the chain is smaller, and that although not very soluble in most solvents (like cellulose it will adsorb molecules including solvents upon its surface ). The effect of this is to expand the chain and allow two or more MCC's to hook up. At this point it is no longer microcrystalline but Macro Amorphous Cellulose(MAC). The purpose of which is two fold,
1st) plug up your filters when water is present (adsorbed easily)
2nd) to hopefully make it through the filtration process and get into the E and reaction process gumming up the RP, reducing yields, and adding an unwanted impurity to the final product.

I have seen the dang thing when the powdered E is initially soaked in boiling acetone for 20 minutes or more and then filtered, the lower levels of the filtrate contain a fine particulate that over time expands, coalesces into a branched structure thinner than a hair , each straight subsegment is 2-4 mm in length and connects to the next subsegment at an obtuse angle. until 5 to 10 of these subsegments form a small chain. After a period of time these chains disappear and a bottom layer develops in the acetone that has the appearance of paper pulp. A rather slimy looking amorphous mass loosely bound together to form a white slime.

I have done a denatured extraction, dried the filtrate, followed up with the acetone extraction and come up with nothing in the acetone. However when the acetone extraction is performed initially this structure is present in the clear acetone filtrate.

The MCC is thought to be freed from its matrix as the acetone saturates the fillers and waxes.
The MCC has not had time to expand fully when it is run through the filters. The filtration process depends upon mechanical action of the solvent flushing thru the filters(since MCC is insoluble). Hence decanting and filtering the supernatant is not going to do any good. The solids are mixed with the solvents and poured into the filters en masse. otherwise the MCC will sit in the bottom with the larger filler particulates safe from the mechanics of filtration. DIG.

Over time the MCC expands especially since the solvent absorbs water in the form of humidity to form MAC.

The acetone wash was initially developed in hopes of catching waxes that were assumed to be present, and this is what was captured instead.

A nasty little creature.

Considering the controversy, I intend to filter and evaporate the acetone filtrate when it is convenient to isolate the MCC free of solvents, then play with it for awhile. However that seriously cuts into my play time in other areas and is low priority.

In the process of extracting E from the blue labeled O.T.C.B. brand pseudos, 60mg, 120 tabs/bottle, lot # 322199.
The powdered tabs were extracted with methanol(not Heet) I have become suspicious of the Heet product in the last month or so of containing water and/or isopropynol.
The filtrate evaporated and dried completely
powdered again and soaked in hot acetone for 25 minutes and fltered as described above.

There are large amounts of particulates in the acetone filtrate, assumed to be MCC.
Much more than I have previously seen.

posted 09-10-99 01:58 PM         

What is important is this !!!---
-------------------------------------
They made it through the methanol extraction. the powdered pills were soaked in methanol(not heet) for 8 hours.
filtration incorporated decanting of the supernatant,
Indicating that theses structures did not expand in methanol, and most probably are soluble in in methanol.
-0--------------------
and are now growing in an open carafe of acetone,

If they are adsorbing water which seems to be the case, then the product Heet may be tainted.

Results of a prior extraction performed
______________
a few days ago.
The previous extraction used methanol from Heet, the powdered pills soaked for several hours before filtration, the filters plugged up very quickly, I had to resort to multiple filters in addition a slime made it through the filters.
On the second filtration( the filtrate was filtered a second time), the rate of filtration was so slow, it was totally scrapped and sand filtering was incorporated.

The entire filtrate from the above mess was re-filtered using the diabolically clever Dwarfian Sand filter and produced a clear filtrate in a rapid fashion.

So
Without the acetone prewash,
Using methanol from Heet,
Standard filtering techniques,
were ineffective and slow to the tune of two hours soaking and a totally dead filtration rate after 2 more hours using three separate funnels all were plugged up. this was with red and white NL brand 60 mg /100 tabs

The, sand filter once again kicked the holy shit out of the crud within 15 minutes.

The paper filters had hours of dismal results.

Dang Dwarves the whole damn family is gonna show up, all gonna be so smug, after this gets around,
Shit I don't need this, I can not deal with gloating dwarves.

yuk yuk
I sure do appreciate the sand filter Dwarfer.

BEWARE
--------
The insolubility of this stuff is a farce.
Would like to know where you come by your insolubility knowledge Chem Guy.
Inaccurate information can happen.

quote:

---

The data of real importance is the density.

What is the density of mircocrystalline cellouse? Is it more or less than water? More or
less than naphtalene? More or less than toluene? Etc, etc?

This would be very helpful because, to my knowledge, the cellouse isn't soluble in
anything. If you knew the density you could create a two phase system such that the
cellouse would position itself for easy removal.
For example, if MircoCrstaline cellouse was less dense than water you could have the
ephedrine salt in an aqueos phase and the microcrstalline cellouse would be floating in
it. Then you could add an organic solvent with a density between that of the water
and the mircocrstalline cellouse so that you could skim off the mircocrstalline cellouse
with a cup (or you could just use a sepatory funnel to drain the ephedrine bound
layer).

The advantage of useing the above sceam is that you wouldn't have to wait forever
for a solution to drain through a filter and you wouldn't have any particles leak through
the filter either.

Anyone with the relavent data?

---

posted 09-14-99 09:20 PM         

If the solution doesn't scatter light, you have a true solution.

posted 09-18-1999 02:37 PM         

When doing the sand filter process- The MMC also filters through, but slower than the ephedrine.

Problem, you want all the ephedrine, but no MMC.

Solution- drain the sandfilter into a container which slowly drains that solution into the final container. Now shine a light through the intermeditate container. In the beginning the solution dripping in shouldN'T scatter the light. But when the MMC finally does make it through the sand filter the light will scatter in this intermediate container. When this happens stop the flow of the solution into your final container with the now MMC free ephedrine solution.

Note 1: I would just use distilled water for solvent.
Note 2: Make sure the sand is clean, so that when the distilled water does drain through the solution won't have any suspension in it that will fuck up the intermediate test for the "true solution".
Note 3: The longer the distance the solution has to travel through the sand filter the better. That way the ephedrine phase is more likely to completely separate itself from the MMC.

posted 09-21-1999 08:42 PM         

If you take some of the sand and put it in a jar with water and shake it up, the water remains clear. And has no taste, either!

I do not know why it always works better (for me) to use the cheapo mixed alcohols (which is mostly methanol, I think).

Perhaps there is something in the blend from the OTC manufacturers that is DESIGNED to work with water: alcohol contravenes it.

As you so rightly pointed out the sand trap is part filter and part chromatographic column.

the first 6" pass through 30 grit sand will still have some particles in it: a second pass can be made (wash the column both times with a couple hundred ML alcohol) and you'll be essentially free of the microcellulose: but truthfully the few remaining after one pass will not make it thru the a/b process anyway, or hamper the efficiency.

My recollection is that the distribution of the particles through a constant diameter column is gaussian. You get the "tip of the leading edge of the curve" with one pass: do it twice and you are probably way less than 1% of the starting value.

In fact I'll guess at less than 1/1000 th.

posted 09-21-1999 08:51 PM         

Are you saying to put the solution back into the sand filter to filter twice? Or are you saying to add two amount of a methanol wash to put the solution through? Also are you saying that the MMC never filters through the sand?

I think that one should use my little test to make sure you get all the "true solution" that filters through before the MMC.

posted 09-22-1999 01:21 PM         

A two dimensional representation of the frequency of particles plotted against distance travelled will show the distribution to be a bell curve.

(I'm leaving out starting conditions and boundary considerations and removal of pores from clogging: but i think I'm more right than wrong) A similar distribution occurs in electrophoresis.

To effect a high percentage of differentiation between things that move at different rates, the media should be chosen appropriately.

In this case the dissolved liquid should shimmy on through, and the microcellulose has all those confusing draggy edges to negotiate.

By time the liquid has 100% drained from the system (- amount on grains wetted surfaces, ) the leading edge of the microcellulose has arrived. (Theoretically some arrives with the first of the liquid, the bell curve being assymtopically (SP) arranged with the axis)

The 100 to 200 ml wash of the drained of liquid filter to wash off the surface tension adhered liquid is probably overkill: it just migrates more mCC trough the system.

But you still get only the very leading edge of the MCC curve: and this is with the 30 mesh sand.(approx 6" deep)

So if you set up another fresh sand trap and repeat, you will get the same distribution curve, but with maybe only 2% of the starting load of fibers.

So if it IS 2%; that's 1/50th

1/50th X 1/50th = (mumble) ?? to hard for me.Where's my calculator??

Chem guy: where's the hole in my logic? I suspect you have more familiarity with chromatographic columns than I.

Thanks

posted 09-22-1999 01:29 PM         

Oh yeah: in the 60 mesh, the "bell curve" is more squashed up, think an inchworm-shape in full retraction moving through the sand.

The wash of the drained-of-liquid filter then produces almost no fibers.

dwarfer

posted 09-22-1999 01:37 PM         

a piece of wadded up paper towel could probably be used, pushed down in the neck to hold back the sand.

But on reconsidering it probably is not a good idea because it may not be well washed by the follow-on plain alcohol rinse: and therefore slightly reduce yields.

So far, at work, I'v done NOTHING but hive: this is ridiculous: I HAVE to makes some money!

OUT!

posted 09-29-1999 01:31 AM         

You may get Raped while your trying to Pillage!!!!!!

I have managed to extract a gwoob of this nasty shit, Visual observations tell me that,
it is insoluble in: H20,acetone,and alkEhol!!