Author Topic: very dry isopropyl alcohol  (Read 485 times)

XBee

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Re: very dry isopropyl alcohol
« Reply #20 on: August 05, 2010, 12:32:34 AM »
Regarding drying of alcohol - ethyl, that is... I've found that 3A adsorbs a significant amount - VERY significant.  The adsorbed alc was reclaimed by heating the mol sieve used to 10-15c higher than bp to drive off the alc... my hygrometer said the recovered alc was c.a. 98%!  GOOD STUFF!  It's not a GREAT hygrometer, but you can reliably read the density within 0.01 of true value ;)
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Prepuce

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Re: very dry isopropyl alcohol
« Reply #21 on: August 05, 2010, 02:30:47 AM »
Great information on dehydrating IPA, Lugh. I knew about salting out a lot of the water but quit doing it like that because of the residual salt.

Even though it's a good substitute for ethanol in a reaction, as a solvent there are some significant differences. Two big ones are the toxicity and the odor. It's often used in removing water/salt from phosphonic acid but once mixed I'm not sure it isn't impossible to get rid of the odor.

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hypnos

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Re: very dry isopropyl alcohol
« Reply #22 on: November 14, 2010, 06:11:38 AM »
I have some IPA that is clear, evaporates cleanly,... and is 640mm per liter..it has a slightly sweet slightly soapy smell...what is the rest most likely to be? water? I dont have a thermometer, but am curious.how might I find out other than frational distillation...it came from a pharmarcy but is not called rubbing alcohol... just Isopropyl alcohol 64%...
« Last Edit: November 14, 2010, 06:15:51 AM by hypnos »
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Vesp

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Re: very dry isopropyl alcohol
« Reply #23 on: November 14, 2010, 07:28:17 AM »
Do an MSDS search for the name/brand, etc etc of the product.
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hypnos

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Re: very dry isopropyl alcohol
« Reply #24 on: November 14, 2010, 03:27:48 PM »
Quote
Do an MSDS search for the name/brand, etc etc of the product.
Yeah I did but  all I got was a load of bullshit besically stating its between 50-70%, IPAv/v,, and water 20-40%v/v

 Tell me something I dont know!
     I love google but there is sometimes sooo much shit to wade through, I am still learning a lot abou 'refining' my searches',, however until I can, I rely on the help and the kind buzz of my fellow hivebuddies in cutting through the crap..all and any ideas would be appreciated..Maybe HPLC might be the go for the final extraction

  In order to share the "collective wisdom and practical experience"  and to inspire the up and coming "home organic chemist" rehashing some topics in the most informed way possible..e.g. the current  A/B extraction thread..I have never personally done any PE extractions and follow ups. however it is a subject I have found intereting to watch the enormous amount of "variations on the theme"
 I must say, in reading that thread i have gotten a fairly good  "overview" of the situations/obstacles many have faced over the past decade, which I have found most interesting (even though I have no intentions whatsoever, at any forseeable time in the future, to be doing this procedure, I still find it interesting to see the ingenious ways members have conquered these obstacles, and are still attempting to..  
        
            Now swih is attempting to extract the 'leftover' fentanyl from some 'Mylan' type  patches that 'suggest' that at 50mcg per hour (alledged) delivery, over 3 days,(which I get a total of 3600mcgs absorbed) but the patches alledged to contain 8,4mg which suggests there may be a few mg's available for recovery...and 90 IPA seems to be the solvent of choice-the fentanyl being dissolved in a silicone based oil, nothing too exotic really:
  
      here's the guff:              
Quote
DISCLOSURE OF THE INVENTION

The invention is a solid-state laminated composite for administering fentanyl transdermally comprising:

(a) a backing layer that is substantially impermeable to fentanyl and defines the face surface of the composite,

(b) an adhesive-drug reservoir layer that defines the basal surface of the composite during use and comprises:

(i) 1 to 5% by weight fentanyl;

(ii) 1 to 10% by weight propylene glycol monolaurate (PGML);

(iii) 85 to 98% by weight of an amine resistant pressure sensitive adhesive polymer having a diffusivity to fentanyl in the range of 10-8 to 10-11 cm2 /sec and a solubility for fentanyl in the range of 1.5 to 5 mg/ml,

said composite exhibiting a steady state fentanyl skin flux in the range of about 2 to about 10 mcg/cm2 /hr and administering at least about 75% of the fentanyl in the composite during approximately the first day of use.
Quote

Prior to use the composite includes a release liner layer that covers said basal surface of the adhesive-drug reservoir layer and is adapted to be removed from the device to expose said basal surface and permit the composite to be adhered to the skin.

  *****     An adhesive backing containing 2.0% silicone oil (100 centstokes, Dow Corning Medical Fluid) and 92.5% amine resistant polydimethylsiloxane (Dow Corning X7-2900) dissolved in trichlorotrifluoroethane (freon) to provide a 35% solution was prepared. The adhesive was then laminated onto a film consisting of 25 micron thick polylester film (3M, MSX-630) such that the polyester film would provide the outer backing-subassembly (L1).

A fentanyl-containing pressure-sensitive adhesive composition was prepared consisting of 1.8% fentanyl base, 4% PGML, 2.0% silicone oil (100 centstokes, Dow Corning Medical Fluid) and 92.5% amine resistant polydimethylsiloxane (Dow Corning X7-2900) dissolved in trichlorotrifluoroethane (freon) to provide a 50% solution. The drug-containing pressure-sensitive adhesive composition was cast using a 150 micron gap Gardner wet film applicator onto a fluorocarbon-coated polyester film (3M, 1022) and the solvent was evaporated to provide a 75 micron thick contact adhesive layer. A porous layer consisting of 25 micron thick Cerex film (a nylon spun-bonded nonwoven fabric obtained from James River Corp.), was laminated onto the other side of the film of drug-containing pressure-sensitive adhesive composition to form a second subassembly
Quote
said composite exhibiting a steady state fentanyl skin flux in the range of about 2 to about 10 mcg/cm2 /hr and administering at least about 75% of the fentanyl in the composite during approximately the first day of use.
 this somewhat "contradicts" the statement on the pack about a steady state 50mcg per hour  ???:-\

apparently...
Quote
The matrix system is designed to hold vast concentrations of medication ;D, far more than its counterparts ;D 8) ;D. The acrylic in a matrix solution serves only one function, to deliver a large amount of drug in a relatively small patch. In a matrix patch, the drug, adhesive, and polymer matrices are all combined.

“It allows you to bypass the ‘middle man’ so to speak, because you are incorporating the drug right into the adhesive,” explains Mantelle
  and also,,,
Quote
The matrix system is designed to hold vast concentrations of medication, far more than its counterparts. The acrylic in a matrix solution serves only one function, to deliver a large amount of drug in a relatively small patch. In a matrix patch, the drug, adhesive, and polymer matrices are all combined.

“It allows you to bypass the ‘middle man’ so to speak, because you are incorporating the drug right into the adhesive,” explains Mantelle

OK now back to the IPA ;D

 Now I have read of 'salting out' the IPA, to improve its purity
 
  Would this be a good simple method to bring the purity up to say 90% without too much fuss?


Quote
Product Code 9320 9403 UN number Solution not classified 6th code
Product Name Isocol Rubbing Alcohol DG Class not classified Packing Code not classified
Other Names isopropyl alcohol solution Hazchem Code not classified
isopropanol solution Schedule not scheduled

Product Use Rubbing alcohol, Skin Sanitizer, personal care solutions External use only

Physical Data
Appearance Clear solution, characteristic sweet odour
Melting Point not applicable
Boiling Point oC approx 92
Vapour Pressure Not determined; above 4.4kPa @ 20 o C
Specific Gravity 0.878 @15 o C
Flash Point oC 24 estimated
Flamm. Limit % U.E.L. N/D L.E.L. N/D
Solubility in Water completely
Other Properties

Volatile Component < 70 %
Auto. Ignition not determined
Vapour Density not determined
Ingredients CAS 67-63-0 Proportions 50 – 70 % [v/v]
CAS 7732-18-5 20 - 40 % [v/v]


Health Effects

Acute
Swallowed Harmful May break into a foam if patients vomits. Aspiration into lungs may lead to chemical pneunmontics
Acute-Eye Mildly irritating
Acute-Skin May affect sensitive skin - broken skin, prolonged contact may cause dermatitis

Acute-Inhaled Not applicable under normal use.


93209 9403…. 2

First Aid

Swallowed If swallowed DO NOT induce vomiting, give a glass of water to drink
Eye Wash with copious quantities of water for 10-15 minutes
Skin Wash with copious quantities of water
Inhaled Remove to fresh air. Keep calm and warm. Seek Medical advice
If any unusual reactions to the above occur seek Medical advice
Poisons information phone 131126 -- Australia wide

Advice to Doctor Treat as for branched chain alcohol solution

PRECAUTIONS FOR USE

Exposure None specified TWA above 983 mg/m3 400ppm Worksafe
Limits None specified STEL above 1230mg/m3 500ppm Worksafe

Personal Protection

[1] Eye Protection Not necessary in small quantities supplied and used
[2] Gloves Not necessary in small quantities supplied and used
[3] Covering Not necessary in small quantities supplied and used

Flammability
Fire Hazards product is Flammable Alcohol solution may burn with a pale flame

SAFE HANDLING INFORMATION

Transport No need to mark as Dangerous Goods in small packages supplied according to ADG code 6th addition
Storage precautions Flammable, Store away from ignition sources naked flames, oxidizing agents, chlorinated compounds.

SPILLS AND DISPOSAL

Spills and leaks Extinguish ignition sources, naked flames. Use absorbent material/ sand
to soak up liquid.
Disposal Follow State or Local Authority regulations / guidelines for disposal of waste.

Fire/Explosion Hazard
Fire/Explosion. Flammable liquid, clear flame
Extinguishing Use foam Carbon Dioxide, dry chemical, water fog.
Media
Other Information

This information relates only to each individual material referred to herein. Such information is to the best of our knowledge based on present technical data believed to be accurate and reliable. No representation, warranty or guarantee is made as to its accuracy, reliability or completeness. This information is not intended to be used or substituted for any other product. It is product specific information. It is the user’s responsibility to satisfy himself as to the suitability of this information 93209403
« Last Edit: November 14, 2010, 03:31:19 PM by hypnos »
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letters

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Re: very dry isopropyl alcohol
« Reply #25 on: November 14, 2010, 05:32:09 PM »
4a mol sieves work great for drying isopropanol. usually the problem with mol sieves arises with drying ketones (such as acetone for example), since most mol sieve batches are slightly basic, prolonged exposure can and will trigger a self aldol condensation.
with isopropanol, ive had no such problem, even when letting it stand for 2 days at r.t. (due to lazyness). best bet for when buying not lab grade isopropanol is to distill straight out of the bottle into a dry flask which contains mol sieves. after a short time, the distilled isopropanol can be gravity filtered from the mol sieves or just decanted.
works well everytime.
if you wish to dry ethanol and methanol with mol sieves you should use 3a size.

hypnos

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Re: very dry isopropyl alcohol
« Reply #26 on: November 15, 2010, 08:24:50 AM »
 her do you get your molecular sieves? as in what type ?  thanx for the idea
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Re: very dry isopropyl alcohol
« Reply #27 on: November 15, 2010, 10:34:11 AM »
the bottle im looking at right now is from alfa. 4a molecular sieves, 1-2mm beads. but in general i guess any decent company can supply you with quality mol sieves.

hypnos

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Re: very dry isopropyl alcohol
« Reply #28 on: November 17, 2010, 10:55:00 AM »
thanx  good to know, I have never used any molecular sieves, but I think I am about to do some experimenting with them, if they are not too expensive....
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iknowjt

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Re: very dry isopropyl alcohol
« Reply #29 on: November 30, 2010, 11:06:23 AM »
Thanks lugh for the info.  In particular:

"The product obtained mixes with eight volumes of carbon disulfide, xylene or petroleum ether without the slightest trace of turbidity." 

That sounds like a brilliant test to see if alcohol is anhydrous.
Seems like it should work for acetone as well.





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Re: very dry isopropyl alcohol
« Reply #30 on: November 30, 2010, 12:16:37 PM »
They use Mol. Sieves in some double glazing type installations as well, look around there are all sorts of interesting chemicals close by.
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Re: very dry isopropyl alcohol
« Reply #31 on: November 30, 2010, 03:33:30 PM »
4a mol sieves work great for drying isopropanol. usually the problem with mol sieves arises with drying ketones (such as acetone for example), since most mol sieve batches are slightly basic, prolonged exposure can and will trigger a self aldol condensation.
The basic impurities can be removed to a great extend by washing the molsieves with PLENTY of water, at least 10-15 times. Don't use it sparingly, but as much and as often as possible. The wet sieves can be regenerated in a household oven at maximum temperature for >10 hours. If you can afford a vaccum oven - even better!

Molsieve 4Å is usually a bit cheaper than 3Å and suitable to dry almost everything except MeOH, which requires 3Å. You can dry liquids, but also most kinds of gas! Very useful if you need for example anhydrous HCl gas but don't want to spent precious sulfuric acid.

Molsieve can be regenerated easily by first washing with PLENTY of water. This is important because the water needs to replace the solvent molecules before the drying step. If you try to dry molsieve in an oven when it is still impregnated with solvent then your oven might go BOOM!
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