Other experiments on OPs
Found the following on the "7" train and scanned it in. Could probably be simplified.
ACRONYM KEY:
VFP = Very Fine Powder
IA = Isopropyl Alcohol (100%)
OAS = Open Air Siphon
CWE = Cold Water Extraction
ml = Milliliter
fl oz = Fluid Ounces
SS = Stainless Steel
IR = Instant Release
UV = UltraViolet
led = Light Emitting Diode
RECOMENDED OR NEEDED EQUIPMENT:
-100% pure orange oil or 100% lemon oil (bit less common, found at specialty stores like “Fruits & Passion” but easily found & sold on internet. Relatively expensive 0.5fl oz for about $19)-
[editor's note: Pure Orange Oil be available much more cheaply, like that price given, but for a pint - look for pure d-limonene, too ]
-100% Isopropyl Alcohol (less common but readily available to many people, cheap 12fl oz for $5 )-
-Separatory Funnel (less common but readily available on internet for $20. Possibility of using funnel or cone shaped container but unknown. SF is highly recommended & needed at this time.
-Pasteur pipette (or long eye dropper) (a cheap & effective way to make a long eye dropper is to buy 3 very common two piece medicine droppers or kid eye droppers. Simply stack taper end of first tube in back end of another tube and replace suction ball on last tube. No tools required, cost about $1 each.)
-High power UV led flashlight (common, available in specialty stores such as Spencers. Also readily available on the internet for about $10-$15. Also very common this time of year for “Halloween”)
-Pedi Paws, battery powered pet nail trimmer (very common, available at retail/drug stores like Walgreens/Target/CVS for $9.99)-
-Ziploc freezer bag (extremely common, any super market $5)-
-(2) small SS Coffee Scoops (very common, available at Target Store/Wal-Mart, in kitchen supplies $2.99ea, made by Chefmate)
-set of SS small measuring cup set (very common, available at *same as above, comes in set of 4 different sizes on one ring, only $1.99
-set of SS small measuring spoons (very common, available at *see above, comes in set of 4 different sizes on one ring, only .99 cents (under a dollar)
-Vibrator Pad or Shaker (less common; $100+ lab equipment but can be easily made from parts, certain toys or old cell phone for under $10 or free using old parts)-
-Heating Pad or Coffee Warmer (very common under $20, available at Target/Wal-Mart/Super markets. Very Hot water could be used instead but could destroy experiment if any got into the solution)-
Step 1:
Take one item, pulverize into very fine powder (this is a key step and time much be taken to ensure that powder consistency is as fine as “talc”, or as close as possible)
Use a “Pedi Paws”. It is much preferred over a Dremel tool, due to the Pedi Paws “catch cap” on the “Pedi Paws”.
Hand filing is NOT recommended, as it does not refine the powder to “talc” consistency.
This catch cap is extremely efficient at retaining as much product as possible. Even when using a Pedi Paws, one should place the entire tool (Pedi Paws) into a “Ziploc freezer bag” and work within this bag. One will be very surprised at the amount of very fine powder that becomes air born but is conveniently trap in the bag which easily collected after pulverizing item.
My note:Friend, please take no insult to these “important notes & key steps”, as they are already written in and I’m only repeating it exactly as it is read. This data seems to be written for those who may not have proper equipment or understanding and is not direct at you per say
Important Note: Use a container which is as small as possible. It should hold no more than 15ml or about 3tsp.
Also keep in mind to select a container that can be easily manipulated and cleaned to retain residual product that may be left on the inside walls of the container.
Small SS Coffee Scoop (15ml max), works perfectly and should be used if proper lab glassware is not available.
Step 2:
Place VFP in small container (container #1). Pour 5ml 100% IA (or just enough to saturate and just cover powder completely)
Important Note: (Use only 100% IA.
Common 70% 91% or even the less common 98% IA will NOT work.)
Place container #1 on vibrator pad for 8 hours.
Most of the IA should be evaporated by this point (8h) of coarse depending on room temp, conditions & amount of IA first used but early evaporation (exposing powder) should NEVER be allowed.
Powder should be fully cover & saturated by IA over the 8 hours. IA evaporates relatively quickly at room temp (78f) but at 8 hour mark mix until dry.
(Important Note: Heat can be applied to help assist evaporation of IA but this can be EXTREMELY dangerous if you are not familiar with 100% IA. Open flame should NEVER be used. If one must, place container on heating pad or coffee warmer (coffee machine heat element can be used).
If you decide to apply heat, constantly mix & stir until IA is fully evaporated and powder becomes dry. Do not heat powder further, doing so will greatly degrade end results. Over heating powder at this or any stage will help bind unwanted elements over to the next steps.
Step 3:
Add 10-15 drops of 100% pure orange oil or 100% lemon oil to container #1 holding dry powder. These oils can be costly, so use only enough to fully cover powder. Adding extra will not help but will hinder during separation stage.
(Important note: Pure 100% orange oil or lemon oil is a must.
Do NOT substitute with “extracts” or products containing “evaporated cane juice” (form of sugar), simple “juice” or anything containing “water”. The slightest water or sugar from these type products will destroy outcome. )
Take container #1 with oil covered powder and place on vibrating pad for 8 hours.
Prepare for OAS during this wait. A second container (#2) will be needed for capture the drain off of oil from container #1. (using the second SS small coffee scoop might be useful at this point)
A truly well written description of a proper OAS:
(
[URL="http://www.drugs-forum.com/fo...m.com/forum/showpost.php?p=892099&postcount=8[/url])
Step 4:
Open Air Siphon (OAS) until powder is almost dry and siphon has nearly complete.
Just before OAS is completed (when liquid IA is almost drained out of container #1 but while powder is still wet), quickly wash down sides of container with a few extra drops of 100% oil.
Instructions to “Wash down” sides/walls of container #1; Take small eye dropper and fill with 100% orange or lemon oil.
Use very sparingly, only a few drops of oil from eye dropper will be needed to wash down sides of container #1. This should take no more than 4-5 drops if used correctly.
Take eye dropper and drip a single (one) drop while at the same time using a wiping motion. This wiping motion is simply like drawing a short line on the inside wall of the container as you are releasing a drop of oil. Let this wash down the walls of container #1 into wet powder.
The OAS collection container (container #2) which is now holding oil from first container #1, can be disregarded (This will NOT be used again in this experiment).
Fear not, this oil does NOT contain any wanted product.
You will have second thoughts about discarding this oil but since you are trusting in these instructions to this point, there is little logic in doubting them now. The science of “why” the target ingredient did not siphon out with the oil can be research and it is recommend that you do so in order to better understand but for now please follow to next step)
Wait until OAS has fully stopped and powder is as dry as possible (should take less than an hour)
Step 5:
Take 125ml separatory funnel and pour powder from container #1, into it.
Add 70ml 100% IA (about 1/3 cup)
Shake very vigorously by hand for 4-5 minutes
Step 6:
Suspended Sep. Funnel from stand or position properly (vertically & level).
Take a long piece of aluminum foil and wrap it around sep funnel (shinny side facing in).
Tear small hole in aluminum foil (about half way down) place high power UV led flash light through this hole so that the UV light is shinning directly at the IA liquid in sep funnel. (the aluminum foil should hold the UV flash light but you may need to add a few piece of tape or wrap another piece of aluminum foil also around flash light. The point is to directly bath IA solution in direct UV light. The Aluminum foil makes this very easy to incase sep funnel and hold UV flash light at the same time. It is much easier than it sounds. The reason behind this is that it helps separate & oxidize small partials from the AI solution. Tests back this claim and it is considered a must at this point)
Set aside like this (with UV light on) for 10 hours
(Note: It may be possible to use a container other than a separatory funnel but be warned, doing so has not been tested and is considered uncharted waters, so to speak. If you decide to attempt this, use a container that is as close to funnel or cone like, as possible.)
Step 7:
Examine separatory funnel at 10 hour mark , upon careful inspection you will notice that the IA is much clearer and a small oil layer floating on top of IA. (you may also notice a small cloud like layer just above bottom powder)
Separate off oil layer to the best of your ability.
Drain off powder & IA solution (and cloud) layer into another small container (container #3). This container (#3) should now be the repository for everything BUT the oil and oil layer (which is a small brown mix layer just under the surface)
This new container (#3) should also be small as possible, a small 1/3 or ½ SS measuring cup will work. You may need to use a pasteur pipette (or long eye dropper) if drain becomes clog. If separatory funnel’s bottom drain successfully drained-out powder & IA solution, skip to step 8.
If clog, read following notation:
Notation for clog: The powder will likely clog most small separatory funnel drains. If this is the case, don’t despair as this will be the norm due to most smaller sep. funnels do not come with larger particle drains.
At this point, do NOT pour out IA & powder solution through the top of separatory funnel, as this would contaminate and remix the oil residue (located on the walls of the funnel) back into the IA & powder solution. If this happens, you would have to redo step 5 from the start (10 hours prior) and waist 10 hours.
Make sure that as much oil as possible is taken off top of IA and the sides of funnel. To do this, use a suction tool and paper towel. Slowly manipulate paper towel to just touch the oil floating on top of IA, it will instantly absorb oil once you touch it, as well as a small amount of IA. Don’t be overly concerned with this IA being absorb with the oil into paper towel, as it will be negligible and not avoidable.
You will find that most common “eye droppers” will be to short to reach either the bottom or the middle of a 125ml separatory funnel. If you do not have longer lab pipette (this is basically a long, thin eye dropper), simply use two or three common eye droppers connected together. Here’s how; almost all common cheap eye droppers have tapered ends and a suction ball that comes apart for easy cleaning. Due to the tapered ends on the eye droppers/medicine droppers, they will easily & very simply fit into each other. Press together two or three until required length. Then place one of the suction ball on the last tube as if you would a single unit and your done.
Be careful when using any suction tool or dropper. If you use to much suction, it will splash up on the sides and taken in unwanted oil. Use suction very slowly and sparingly, you will thankful in the end.
If using a suction tool/eye dropper on powder clog, be sure NOT to use the same dropper that you used to separate the oil or make sure to properly wash/clean dropper(s) between steps or you will contaminate oil back into the powder IA solution and waste many hours of work.
Step 8:
Wash-out separatory funnel. Be sure all oil residue is gone and sep. funnel is thoroughly clean.
Step9:
Redo above steps 5 thru 7 one last time. Do NOT cut any corners (This is a long process but it was found necessary to get rid of the oil/chemicals from usable powder.)
Step 10:
Container #3 should now have the solution of powder & IA.
Evaporate IA from powder by employing a non flame heat source. This will greatly speed things along (see above note on heating IA correctly & safely).
If heating, make sure that temperature never surpasses 110 degrees F. Stir & mix while heating to help evaporate off IA. This will not take long, as IA evaporates quickly when even a small amount of added heat is applied. (Note: the author has decided to keep this a low(er) heat extraction process but one can adjust this in order to balance time-to-outcome during future trial & error. This solution may be too long as written but as it stands now, it has been vested... although refinement is for the bold & welcome)
Once powder is completely dry, you are almost complete.
Step 11:
CWE by employing OAS. This will help wash out any left over chemicals. Make sure that all the water used is continually kept ice cold, no more than 34F degrees and that filter/string is wet with ice water before starting extraction. (to help manger ice cold temperature during OAS, recommend placing the top container in a type of "double boiler" set up but using ice & water)
Recommend using three pieces of Oral-B superfloss string(s) for the OAS and reusing the two (15ml) SS coffee scoops once again during this OAS, CWE. (Of coarse wash & clean SS scoops first. Also note: Oral-B string has a coating which should first be washed off as well)
Use as little ice water as possible, less than 8-10ml. Use small eye dropper to wash down walls of container, again using only a drop or two during a wiping motion, in order not to waste any wanted product.
VIP Note:
Unlike prior OAS (under step 4), the bottom or target container (which we will now call container #2) will NOT be discarded or thrown away. This target (bottom) container #2 will retain all the wanted product.
You may also notice that the top container #1 will not have much, if any, left behind material or powder after OAS is complete. This is to be expected. You may also notice that the siphon string(s) might be light brownish in color and have a slight sent of orange/lemon oil, this is ok. As long as you completed the wall wash with a few extra drops of ice water. Do not attempt to pintch the string and squeeze this out.
Step 12:
Take container #2, sprinkle a very small amount of fine powder ox_co_one (talc?), less than a pinch, into container #2 and stir. If none is available, move on. (this method was used in all tests due to a well placed suggestion and discussion to help end results. It may make zero difference but was used in all tests)
Place in oven at 180F degrees. Do NOT boil. As water evaporates, lower temperature to 130 when most of the water has evaporated. Check constantly at this point, until fully dry. Once fully dry, take immediately out of oven. Excess heat is unwarranted.
Step 13 (END)
Very important to take your time and scrap down entire area of SS container. You will finally have product ready to be ground/cut into desired choice method.
This entire method can be refined with experience but works as is. Once experienced & familiar with above method and with one‘s own devices, one should figure out methods best to refine & speed-up the entire process.
NOTE: This is for information and theoretical purpose ONLY, rather than real world practical considerations. The term "vested", as used in this informational article implies vested in theoretical science. Do NOT use this in a real world setting or to violate any laws. NEVER take out of the theoretical setting or discussion. Do no harm.
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Editorial comments are below, but can't get them to originator of method:
Comments:
Comment 0: Whenever I see the acronym IA, the first thing I think of is "Iowa". Better to use "IPA", which is the standard acronym for isopropranol.
Comment 1: If you have or can borrow a scale that measure to the hundredths of a gram, or better to the milligram, it would be useful to measure what you have at the beginning and end of each step. Before starting, you would weigh each of your containers. For example, if you were using dried epsom salts to purify Isopropanol, and you knew what the weight should be of the water that's in the amount of impure IPA you were purifying, you would weigh your dried epsom salt before and after purifying. If the epsom salt had increased in weight by the weight you expected the water to be (and your isopropanol decreased by the same weight), you would have a good indication that your purification had been successful. Of course you would need to subtract the weight of yor container(s) before jotting down the weights.
Ideally, this data will make it possible eventually, for each step to indicate what it's inputs are, specify the transformation it performs, and then indicate what it's expected outputs are. Until then, just speculation will have to suffice.
Measuring the weight of everything affected, both at the start of the step, and at the end of the step can help to pinpoint exactly what is happening at every step, which may help to streamline the procedure, speeding it up.
Step 2 is mildly agitating the mixture for 8 hours. All I can think of is that this is applying minor shear forces to the PEO. Manufacturers such as Purdue are given instructions (by the makers of PolyOx aka PEO) to use certain motions, when mixing the raw PEO powder, to minimize "shear forces" which "degrade PEO".
Step 4: Comment should note that "oil should contain the anti-oxidant PEO". I wonder if there is any test to compare the amount present beforehand vs afterwards.
The API (active Pharmaceutical Ingredient) is still probably bound to the PEO, which has not yet been degraded by oxidation and shear force (which probably degrade PEO in different ways.
Steps 5 and 6: It probably would be best to agitate while exposed to UV light and then let stand to separate out into layers (probably still under UV light. Also, see Question after comments.
Step 7a: A separate siphon string presaturated with oil should repel water, and only siphon oil from the top (or do I misunderstand orange oil?).
Step 7b: Why not drain mostly from the top? You could use a long siphon wick running through an opening in the rubber bulb of a cheap glass dropper (squeezed tight while inserting through oil layer, so no oil gets on wick). Due to then length possibly needed, you might need a different material for the wick. A thin slice of a thin chamois worked nicely for ethanol. It should also work well for isopropanol.
7C: If you have been able to drain mostly from the top, you should not have too much trouble with clogs when you get to the point where you need to drain from the bottom.
To deal with clogs, you could use a long cheap glass dropper with some metal wire poked through the rubber bulb (not a hole, you want it somewhat air tight without effort), and gently manipulate the wire to clear the clog at the bottom.
Step 8: Specify what to use to clean up? An emulsifier like Palmolive dishwashing liquid? A major solvent like MEK? Isopropanol? (IPA worked well for Dow and Colorcom)
Step 10: you could heat the microwave platter ahead of time just by preparing lunch or coffee, so as not to waste energy. The rotating platter should be sufficient for a heat source.
Why the choice of 110 degrees?
Step 11: Why so cold? The procedure for the old OC's used room temperature at this point
Step 12: lactose powder might be good to add as a filler here, as it is fully water soluble, and won't bother the nose when dried.
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Question: What is the output rating of the UV flashlight (in lumens or microcandles or watts)? What is it's wavelength? Both of these should be on the flashlight packaging. Powerful Raw UV Led's are available (I just looked some up, and those that are ultraviet or infrared are rated in milliwatts or watts. It's probably because you can't see them that they arent rated the same way that visible leds are.
superbrightleds.com has 20mw UV "SuperBright" Leds for 1.59 each, but I would not buy a 20mw led any more. They also have 1 watt UV leds for 6.99 each. You could probably get 1/2 watt leds elsewhere for a few bucks apiece and string them all around the funnel.
You'd also need a power supply (that same site has a 15 watt supply for 13.00) unless you want to keep changing D. cells. Staying with batteries would mean, since you can't see UV light, you'd need something that flouresces under UV to tell whether the batteries are still producing much light under load. The one other thing you would need is a current limiting resistor (diodes conduct current very well in one direction (forward) and not at all in the other direction (reverse). If you don't limit the forward current with a resistor, they will suck all the current they can, and burn themself up doing so. (The property of conducting current in one direction and not the other makes diodes ideal for converting alternating current into direct current, but the diodes normally used for this purpose can generally allow much greater currents. They also do not emit light. Every AC to DC adaptor that you plug into the wall contains at least 4 diodes, sometimes packaged in a single casing with four leads)
Note: The entire contents of this message are pure speculation on the operation of one or more imaginary devices intended for use by licensed medical staff, aboard a starship in a science fiction novel.
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More comments:
I was just re-reading "POLYOX Degradation of Water Soluble Resins". Close to the end, where it talks about reaction with oxygen and hydrogen peroxide, it says "The decomposition can be catalyzed by several metal ions such as ferrous, cuprous, cupric and silver. Typically, lower valent ions are more effective catalysts".
My take on this is that one could place two electrodes in a solution of PEO, through which oxygen is being bubbled, and pass an electric current through the solution. This would look a little like an electroplating setup, or like a cell of a wet battery. As you pass current through the solution, electrons are jumping from one atom to the next, creating a flow of ions. The source electrode (called the "cathode", connected to the negative side of the power source) should be as large as possible.
The combination of oxygen exposure, UV exposure, and ion catalyzation should result in a very rapid degradation of the PEO. From another document, shear forces should speed it up further.
The PEO used in the OC tablets has a molecular weight in the millions. After degradation, it is still in the thousands.
Oxycodone has a molecular weight of about 315, and acording to drugbank.ca, an experimental water solubility of 100mg/ml
I couldn't find any information about the water solubility of degraded PEO (how degraded is degraded?), but I recall seeing a reference to an inverse solubility profile, such that it becomes insoluble when heated to a certain point, so if that is also true for the deggraded form,, after degradation, one could perhaps heat a solution to cause sedimentaion of the degraded PEO.
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Finally, Pure Orange oil or it's main component, d-limonene seems to be available for much less than the author indicated, less than an Andrew Jackson per pint