TheWire
Harmless
Posts: 6
Registered: 27-4-2011
Location: UK
Member Is Offline
Mood: No Mood
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Advice on practising A/B cleaning and methods of dealing with MCC
I need to practise my A/B extractions. When I get enough of the re-agent it will be a HCL mixed with Micro Crystalline Cellulose. Some people seem the
think that getting the HCL from the MCC is easy as MCC is not VERY dissoluble in H20 but it certainly dissolves enough to severely contaminate the
resultant HCL(after simple h20 extraction).
I looked into this and found that MCC is slightly disolvable in just about anything EXCEPT a ph.11 solution, which is why the A/B is more successfully
as to base the HCL you need to use a high ph solution. A/B is ok, but I get bad losses. I put it down to crappy reagents that are slightly wet and not
LG, also I think my simple gassing procedure of just using a syringe to inject amounts of 36%HCL acid creating the HCL in a wine bottle is to put it
mildly, sloppy and in need of vast improvement.
Talking of a gassing set up, say HCL gas, can anyone recommend a lab glassware/equipment that is reasonably economic but patent, releases gas at a
steady flow and of course making sure the gas is dry.
I am asking a lot of things, so to summarize, I need practice extracting a HCL and cleaning it via the various washes, dual solvent crystallization,
etc. the end result I am looking for is to produce clean crystals that if you guys felt necessary would go through several dual solvent
re-crystallisations and a final clean using something like H20/MEK..... of course the crystallisations would be engineered to be slow,about a week to
2 weeks per one, I want VERY clean base product.
On another project I will be turning the base back to HCL and may not do an A/B at all.
I would like suggestions of cheap products(not reagents) that I can practise my extractions, cleaning, gassing, A/B so when it comes to the real thing
I don't mess up(hopefully).
Also,any help on a good gas make-up, with lab equipment/glassware and produces steady(leak free!) gas and is a solid working piece of equipment. Any
pointers on gassing welcome.
Sorry if I sound like a complete noob, I am desperately searching for chemistry courses but fear I will have to travel 50 miles for a course that
would be at the right level for me and part-time. I have been reading, reading forums, doing all the research I can. I have utfse and am familiar with
lots of advice but I am looking for specific recommendations where I could not find any in these specific areas.
I wished I got into this earlier in life, I am a hardware/micro-electronics/micro-processors/assembly language geek! I can certainly reciprocate your
help if you have any questions in those areas..... I am just about getting my head around Linux ready for my 2 servers to arrive!
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smaerd
International Hazard
Posts: 1262
Registered: 23-1-2010
Member Is Offline
Mood: hmm...
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HCl gas is not really practical in this application I wouldn't think. Are you making it from printer paper?
What do you mean your HCl was contaminated? Isn't that the goal in general for this procedure? To wash away undesireable compounds from the cellulose?
The way I have gassed HCl was by drilling a small hole in a rubber stopper and inserting a 18 gauge needle through it(snuggly). This was placed ontop
of a vacuum filtration flask(loaded with dry CaCl2 granules). I then attached a hose to the vacuum out-let and lead the hose to the solution to be
gassed. When everything was ready and the apparatus was OUTSIDE I fixed a 10mL syringe with concentrated HCl(~31.45%) and pulled the plunger down
several mL's and walked far away. The gas will evolve over a large period of time, and this isn't safe by any means... Pretty ghetto really, probably
shouldn't have recommended it. When gassing anything be aware of suck-back and plan for it, especially with hazardous/corrosive gasses such as HCl.
There is a lot of information on this subject available here on this forum though.
Anyhow, hopefully something here was useful, best wishes.
[Edited on 5-8-2011 by smaerd]
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