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deltaH
Dangerous source of unreferenced speculation
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I may well have goofed up the calculation, so feel free to check it, but the problem is that the hydrate has a lot of water intrinsically associated
with it. There also seems to be some confusion as to what the empirical formula of the hydrate should be, different sources give different ratio's. I
trust the one I used a little more because it came from a paper which determined it's crystal structure from XRD.
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Little_Ghost_again
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Thats ok Delta H, I dont have a clue yet how to work these things out, but I am trying to learn. I want to try as many methods as I can, so it dosnt
matter too much about yield. I am more interested in seeing if any of the bleach making methods improve chloroform with IPA and if/what side products
are made.
Rain has stopped play for the moment, I dont fancy having have electrical stuff outside in the pouring rain  , but it gives me a chance to read some the pdfs posted
Dont ask me, I only know enough to be dangerous
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Bot0nist
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TCCA has been praised as a great and efficient material for use in a chlorine generator. A quick search of the forum should provide countless
discussions and setups. IIRC, woelen dished out some great advice and experience about it in a couple places. As always, UTFSE, and be safe. As I'm
sure you know no, making large amounts of chlorine can be a bit troublesome for your, and others help.
Good luck, and keep us posted.
U.T.F.S.E. and learn the joys of autodidacticism!
Don't judge each day only by the harvest you reap, but also by the seeds you sow.
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Little_Ghost_again
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excuse the ignorance is TCCA Trichloroisocyanuric acid? I dont have any if it is. 
Dont ask me, I only know enough to be dangerous
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Little_Ghost_again
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Safety could be an issue, so major glass cleaning operation while the rain is bad! I intend to try and keep things as closed as I can, might be
overkill but with limited equipment I figure glass rods and any joins done with PTFE wrapped over the joins and held tight in place with heat shrink
tubing.
Dropping funnels and 3 neck flasks, 3 way glass valve so if needed I can dump excess chlorine to thiosulphate was bottle, its new and has a glass frit
so i didnt fancy using hydroxide in it for the first outing lol.
Aquarium air pump to push any excess chlorine from generator into wash bottle, I havnt figured the ice slush yet but probably crystals in a flak and a
drop funnel for adding the hydroxide, 3 neck again to wash bottle if chlorine is evolved and gets out of hand.
I will also set up a mini chloroform run the way i tried before and this time try and weigh things more accurately, i have a good temp data logger I
can leave on the side of the flask and track the temperature over night.
Dont ask me, I only know enough to be dangerous
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Little_Ghost_again
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Unfortunately Trichloroisocyanuric acid is pool shock? I live in Scotland and I doubt there is more than 2 home pools in the whole of Scotland!! Apart
from living in a very rural area I think it likely only one or two cities here would even have a pool supply shop.
I will look online and see how much ebay wants to fleece me for some, failing that anyone got any other ideas for producing chlorine?
Looks like potassium permanganate and hydrochloric acid, I could clean up some manganese dioxide from some of the old cells I have but I dont trust
the contaminants.
This is a real PITA, I was hoping to have a easy way with what I had at home, I would use electrolysis but that means making something to stick the
electrodes through so I can seal the container.
Anyway lunch is over the parents are out and the kitchen is free , so best I
catch up on the glassware cleaning.
[Edited on 4-10-2015 by Little_Ghost_again]
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Bot0nist
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Sorry, I took for granted that TCCA is readily available and cheap in my area. A few pool shock pucks of TCCA could probably be had cheaply online. I
have seen them in little foil packets. Or get a 5 gallon bucket of the powder if you need a lot of chlorine.
U.T.F.S.E. and learn the joys of autodidacticism!
Don't judge each day only by the harvest you reap, but also by the seeds you sow.
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Little_Ghost_again
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1kg is about £16, not too bad but cleaning up battery gunk is free (ish) and I have 7ltr conc hydrochloric acid. I also have permanganate.
Its a tough one because I have a limited budget but then again I want to give this a good shot. if I can find a way to make the container then
electrolysis of Brine would seem the best way. Wikipedia dosnt mention oxygen being off at the Anode but other sources mention it.
I didnt get to do much today, I had a great deal of backed up glassware and still more to clean. Since being banned from the kitchen I have got lazy
with cleaning, I also dont have hot water in the outbuilding I have been kicked out into.
I confess with some of the thicker walled really dirty glassware I washed out best I could then added water and some sodium hydroxide, instant hot
water lol, its cleaned the glass nicely.
I didnt leave the solution in very long though. I am going to read all the info I have been given before going further, I really want to get this
right. I found a 2 ltr flask with the waste from a chloroform run, I used alot of IPA and the top layer smelled like a solvent but not IPA or acetone.
Now it smells closer to acetone, I will distill it and see what the boiling point is. I also found a few bits of glassware in a box that I have no
idea what they are for, I might post pics later and see if anyone has any idea what they are.
Thanks for the help, its really appreciated. I doubt anyone is going to take it seriously but the very first run of chloroform I did with IPA
bleach,salt and sodium hydroxide worked really well and I started at room temp, I didnt get very hot temps and I think most of that was actually from
the hydroxide.
This time I will document it, the bleach is kind of a side project from that.
I can do much as its getting dark but I might try and draw what I have in mind, I did think sulphuric acid and salt would give me chlorine but that
didnt work too well
[Edited on 4-10-2015 by Little_Ghost_again]
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Little_Ghost_again
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I started reading the PDF and the bit near the start where it talks about absorbing chlorine gas into dry calcium hydroxide caught my eye, it says
upto 70% chlorine is possible, I doubt I would go anywhere near that and I dont have calcium hydroxide. BUT in the back of my shed from long ago is an
old 10 ltr carboy with hydrochloric acid in and dissolved seashells, I was making calium chloride that I then reacted with sulphuric to get calcium
sulphate.
To be honest I forgot all about it until tonight.
I then found this video online https://www.youtube.com/watch?v=MdIHl2JnD-I
In it the guy makes calcium hydroxide by reacting calcium chloride with sodium hydroxide, I have a shed load of sodium hydroxide as I make soap. My
calcium chloride is a bit erm rough, the pics make the vessel look small but I had to take the picture with a lamp as the container is in a shed with
no light.
It dosnt look like it but the white powder under the dirty layer is very white, the solution still dissolves sea shells so I assume its still pretty
acidic. Now its all settled out I could hoover out the dirty layer with a large glass tube connected to a vessel and vacuum pump, then hoover some of
the clean powder and wash it.
From that I could mix with sodium hydroxide and get my calcium hydroxide?
Its hard to tell from those pics but there is a fair bit of powder in there, also if I drip some of the liquid into sulphuric acid I get a white
precipitate form, so I am assuming I do actually have calcium chloride in the main vessel.
Thoughts welcome as always.
The bit I got it from in the PDF in this thread says the following about it....
In 1799 C. Tennant and C. McIntosh developed a process for the production of bleaching powder by absorbing chlorine onto dry calcium hydroxide. This
bleaching powder was
much more stable than previously obtained
bleaching products. In 1906, G. Pistor succeeded in producing highly concentrated bleach-ing powder with more than 70 % available chlorine.
It dosnt say exactly how you get the powder to absorb but I havnt read it all yet. in some ways this would seem safer, but I dont want to go too far
as obviously making chloroform with it for the first time will be small scale.
Just as a side note the shells were mainly razor clams and had alot of organic crap around them, I heated the shells in a pan on a open fire to try
and heat alot of it off. Thats where I think the dirty layer comes from, the powder thats white settled pretty quickly after fizzing and left a dirty
solution, but over time the solution has cleared alot and the fine crap layer has settled on top
[Edited on 4-10-2015 by Little_Ghost_again]
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hyfalcon
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Do you have access to pickling lime? If so, you have calcium hydroxide, or calcium oxide which upon adding to water...
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Little_Ghost_again
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Quote: Originally posted by hyfalcon  | | Do you have access to pickling lime? If so, you have calcium hydroxide, or calcium oxide which upon adding to water... |
Never heard of it but a trip to the super market will reveal if we can get it .
If not do you think the method I outlined above will work?
I know its a long route but in case I cant get the pickling lime....
I might ask mum about it she would know if pickling lime was in the shops, she does pickling and stuff like that
I know the pics look grotty but the dirty layer is very thin, I can definitely suck up some the white powder and wash it? Oh it just occurred to me I
better see how soluble it is in water!!! If washing is a problem then maybe drying by heating it? the HCL should decompose first shouldnt it?
[Edited on 4-10-2015 by Little_Ghost_again]
Thanks guys I am really having fun with this
[Edited on 4-10-2015 by Little_Ghost_again]
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Little_Ghost_again
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Ok no end of problems!! I need some different tubing for a start, we have two weeks off starting next week so..
The plan is two do small scale Chloroform using IPA and a few variables of the method I used, I will use the bleach I have at the moment and order
some better tubing for the chlorine, if this comes in time I will re run with the new bleach I make.
I thought this would be easier than its proved to be!
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aga
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With charcoal, a short length of steel pipe (fence post) and a hairdryer you can get up to some insane temperatures (1500C ?) albeit briefy.
It's messy as the airflow blows crap all over the place, however i've seen this simple setup melt about 30g of Steel easily.
I was trying to melt copper in a steel pot at the time.
The copper may have alloyed with the steel, lowering the melting point (depressed eutectic !) or something like that - i do not know.
The Copper certainly melted, so that's 1085 C right there, and there was a big hole in the steel pot where it;s metal used to be.
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Little_Ghost_again
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Not sure what went wrong but one of the plastic aquarium airlines just went black and started to leak, so better tubing or the chlorine is going to
get out. My little oven based on charcoal gets pretty hot, a bit like yours but I use a small bouncy castle fan for the air flow.
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Little_Ghost_again
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| Quote: Originally posted by UC235 | Chilled sodium or potassium hydroxide solution is very effective at absorbing chlorine gas until you get close to equivalence. It's easiest to track
chlorine absorption by weight and with NaOH, 12%ish by weight is a good target. It is very exothermic from what I remember so you'll need quite a lot
of ice.
Existing bleach can be made stronger (in fact it will save you a lot of hassle and reagents to do so) by adding cooled conc. NaOH solution and adding
chlorine gas until desired weight gain. Heavily degraded bleach might end up saturated or precipitating salt though, so proceed carefully if that is a
problem. Addition of salt has basically no effect on bleach and it probably contains a fair bit anyway leftover from the electrolysis brine.
[Edited on 3-10-2015 by UC235] |
I mentioned somewhere or rather asked about adding salt.
I originally added salt when making chloroform from IPA, I think the original idea was to see if I could salt out any water from the IPA or bleach.
The information given back was adding salt dosnt do anything. Because the whole point of doing all this is to see what happened when I made chloroform
with IPA I decided to add salt to IPA and in another flask add salt to bleach.
The flask with bleach I added enough salt to saturate and leave a very fine layer on the bottom of the flask, nothing weighed as this was merely a
lets see what happens thing.
This was a couple of weeks ago now and for the first week nada, nothing, no change. Then starting yesterday I noticed that the top of the flask 'MAY'
be a lighter colour, this is very subjective at the moment and the difference is very tiny.
Whats interested me is there are definite vey very tiny bubbles on the top of the salt crystals, these bubbles are evolving at a slow rate and so far
I would say most of the top of the salt layer has these very tiny bubbles.
The flask has been sealed all this time with bubble wrap, upon taking of the bubble wrap the smell of bleach is less. But that makes me think that
maybe this is down to the lighter coloured layer (if it exists).
Now I know there is probaly a reasonable explanation for this but the number of these tiny bubbles makes me wonder what is going on
Dont ask me, I only know enough to be dangerous
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