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tina_craig
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Joined: 07 Feb 2005 |
Posts: 26 |
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642.42 Points
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re: Straight to BEE III - The Pickled P
Wed Jul 06, 2005 9:48 pm |
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Switc can vouch for that observation as well about the multiple passes. Second passes usually yields maybe a 1/20th of a gram, the first volume of Naptha extracts the majority.
Also, as far as yields:
KOH boiling with modified reagent amounts (4x KOH/2x alky with multiple additions of KOH): 70%
STB3 following WM/VE's latest modification(100mlBrine-1/2vol. Naptha): 80%
Both procedures have yielded ready to react PSE with nothing but white during basing of reaction fluid and at least 70% yields in a 2 hour P/P type reduction.
STB3 is by far the best to date and the most efficient. |
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loki
guinea pig
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Joined: 09 Mar 2005 |
Posts: 391 |
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14167.88 Points
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re: Straight to BEE III - The Pickled P
Mon Jul 11, 2005 8:23 pm |
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i thought i should relay this message that was scribbled on a sheet of paper which strangely flew into my backyard:
Quote: |
videoeditor=god
36x120mg pseudoephedrine/loratadine pills were boiled in 150ml of brine containing 52g of rock salt, 22g of citric acid mixed with white vinegar. took about 40 minutes to come to the boil at the end point the little barrier shells from the pills were floating around in a vinegar smelling milky solution.
the solution was filtered in a combination coffee filter/charmin filter, stacked one on top of the other, conveniently the coffee filter funnel sat nicely on top of the funnel below. a clear, dense looking golden liquid came out of the solution. crystalline sodium carbonate was added slowly until frothing ceased then concentrated sodium hydroxide solution was added slowly after putting 50ml of shellite on top. probably too much was added, the solution went past white to orange.
as the solution was heated it turned brown and then black with a frothy looking orange layer atop the aqueous with the shellite on top (this darkening was assumed to be caused by the citric acid caramelising). this was heated for 15 minutes, extra shellite was added as the volume decreased by half in the process. the two phase solution was poured into a separatory funnel and the bottom layer was separated from the top, and the top layer put in a small jar.
a second pass was done because only 50ml volume was possible in the solution. meanwhile crystals started to precipitate out of the small jar. the second pass was again separated and added to the first pass and a small amount of distilled water was used to remove the orange froth which managed to end up in the solution.
the solution was sealed and put in the refrigerator, it was already forming dense mats of crystals around the top and on the bottom and somewhat on the sides as well. the first time ever that the experimenter experienced the phenomena of a solution which literally was crystallising right in front of him, when a dropper bottle was used to agitate the solution when washing it the dropper became almost clogged with crystals.
the end product was not weighed but looked easily in the vicinity of 3 grams of off-white crystals. the yellow colour was assumed to be from the antihistamine in the preparation and had been seen before. the experimenter lacked a grinding device (and at the time, acetone too) so the pills were not pre-soaked in acetone. the colour of the crystals was better than he'd ever seen before from this pillstock however.
the entire extraction process from start to finish took about 5 hours and there was enough time during the initial boiling to be able to process 50 matchbooks and 150ml of 2.5% tincture, the final stages of washing the phosphorus and drying the iodine was performed while waiting for the crystallisation.
the completed clean reagents were premixed and cooled in a freezer until the crystals were ready to go in. when the pseudo was mixed in at first nothing happened but the crystals gradually turned orange. the reaction vessel was placed on the heat and watched carefully because this was the experimenter's first freebase reaction and he didn't want to have a flask fire. the reaction got a bit crazy at first, and the vessel was on and off the heat for the first little while. the white vapour, assumed to be hydriodic acid gas, persisted and mostly went away once extra water was added to the reaction. the experimenter allowed a faint vapour to remain because he wanted to ensure that the reaction stayed at just above concentration for the duration. the reaction vessel was a small 50ml lolly jar which was sealed for the reaction.
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sadly that was all that was written on the piece of paper, maybe i'll be lucky and find the other half later on. |
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re: Straight to BEE III - The Pickled P
Mon Aug 01, 2005 10:57 am |
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Well well, Swip must say that this method works so far.
Swip followed instructions to double the brine salution with 1.800gms of avalible pse,
So far for swip everything has happend just as the write up sais, Now swip went and used *camp fuel* for his nonpolar and now has a jar plus colmens plus what looks like little splinters of glass, HHMMMMM.
From there swip is scared to do anymore incase he looses all the pse , But then again this is a dream test run, LOL.
Any other bee use *camp fuel* at all, and after collecting the free base crystals and cleaning them, Could it bee used in a rp/I2/E reaction ????? |
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Sektor
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Joined: 22 May 2005 |
Posts: 103 |
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3105.26 Points
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re: Straight to BEE III - The Pickled P
Wed Aug 10, 2005 2:39 pm |
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can swim use Toulene instead of Hexane? |
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Sektor
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Joined: 22 May 2005 |
Posts: 103 |
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3105.26 Points
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re: Straight to BEE III - The Pickled P
Sat Aug 13, 2005 7:37 am |
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or *camp fuel* instead of VMP Naptha? cheers |
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re: Straight to BEE III - The Pickled P
Mon Aug 15, 2005 10:07 am |
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no and yes |
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Sektor
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Joined: 22 May 2005 |
Posts: 103 |
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3105.26 Points
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re: Straight to BEE III - The Pickled P
Mon Aug 15, 2005 11:37 am |
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Note:
Do not substitute for VM&P Naphtha. Shellite, white gas, petroleum ether and lighter fluid are NOT VM&P naphtha. VM&P Naphtha is a combination of aliphatics, xylenes and ethyl benzene and has an unmistakable smell of naphtha (moth balls). Some Oz Bees have reported the same success with Shellite but since I cannot verify this, I cannot guarantee it will work.
^^^ can swim use *camp fuel* instead of VM&P Naptha? |
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loki
guinea pig
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Joined: 09 Mar 2005 |
Posts: 391 |
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14167.88 Points
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re: Straight to BEE III - The Pickled P
Mon Aug 15, 2005 12:06 pm |
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i have used it with shellite, works a treat |
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re: Straight to BEE III - The Pickled P
Tue Aug 16, 2005 9:18 am |
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swip has used *camp fuel* with no problems |
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Sektor
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Joined: 22 May 2005 |
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3105.26 Points
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re: Straight to BEE III - The Pickled P
Tue Aug 16, 2005 9:48 am |
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sweeet, cheers p2e3r4f5e6c7t8, say... do you know u98chq0134 by chance? thanks again |
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re: Straight to BEE III - The Pickled P
Wed Aug 17, 2005 8:37 am |
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It is swip's plesure to help any fellow bee, Seeing as tho swip had a tone of help at THE HIVE when he first become interisted in this sort of hobby.
So now swip will try to repay the favor as best he can with dreamers. |
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Sektor
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Joined: 22 May 2005 |
Posts: 103 |
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3105.26 Points
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re: Straight to BEE III - The Pickled P
Tue Sep 06, 2005 10:30 am |
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swim has recently done this, problem:
the brine wash that was mixed and boiled with pill mass was green/bluey
lots of sedement in filtration(after many at that)
the stage where naptha(swim used *camp fuel*) is added to neutrilised solution and heated to simmer whilst adding base fluid, the bottom layer went really dark/caramel/orange, whilst there was little top layer left-so swim added xtra *camp fuel* and swirled then seperated, swim will report of what has become when the top layer has finished cooling(in freezer right now) |
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Sektor
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Joined: 22 May 2005 |
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re: Straight to BEE III - The Pickled P
Tue Sep 06, 2005 11:57 am |
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fuckin BOOYAH!, dunnit! success, false alarm on the problem post of above, this is a great method, strange though, apparently tripolidine hcl is meant to taint the pfed blue, swims was beutiful brilliant crystals(not blue) and if anything most of the shit was green up to the stage where swim added the *camp fuel*+basing and boil, then canted of top layer then froze, excellent! |
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loki
guinea pig
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Joined: 09 Mar 2005 |
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14167.88 Points
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re: Straight to BEE III - The Pickled P
Tue Sep 06, 2005 1:35 pm |
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yeah swim saw it turn first to a rich orange then after that, more rapidly it went nearly black. two passes of half volume were extracted, the second amount of naptha was literally dumping crystals right in front of swim's eyes once separated.
swim was having a problem with the particular pills however. they are known to contain loratadine, which upon investigation seems to be a relatively insoluble bastard... and so the nature of a bright golden yellow contaminant is thus unknown. the pillstock is known to also contain rosin and vegetable oils... it is sticky and not water soluble whatever it is, and more soluble in naptha than pseudo.
perhaps a defat beforehand (either a soak of the dry powdered mass or a wash of the acidic brine solution) would do the trick? it really depends on whether the contaminant is alkaloid or oil/phenol/alcohol/whatever. it does seem to rinse out fairly well acetone. what is the solubility of pseudo fb in acetone? |
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Sektor
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Joined: 22 May 2005 |
Posts: 103 |
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3105.26 Points
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Re: Straight to BEE III - The Pickled P
Tue Sep 06, 2005 2:50 pm |
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Filter the mixture through a Charmin plug in the bottom of a large funnel into the other boiling flask. All the collected liquid should bee crystal clear.
^ though swims collected liquid was not crystal clear at all... still worked though |
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