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jhullaert
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[*] posted on 27-8-2009 at 06:03
starting a organic home lab


Hi everybody,

I need some advice about starting my own organic home lab.
After I found a good location, I'm now thinking of which glassware I need.

- A reflux condenser NS 29. Is lenght very important?
- A magnetic stirrer with hot plate. speed up to 1250 rpm and temp up to 330°C.
- Round bottom flask. this is the hardest to choose. What do you guys think? three neck or two neck? extra neck(s) NS14 or NS29? and volume? 250 mL 500 mL or even 1L?
- thermometer temp rang -10 to 250°C. NS14
-Liebig condenser NS 29 Would you use this for refluxing too? a reflux codnenser is not cheap but looks more accurate than this.
- Which glass joints do I need? One on top of the reflux condenser where I can put my liebig condenser on for destillation?

Another question. Should I inform the police? I know it sounds very silly but I really don't want to lose everything because they are suspicious for drug making etc.
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watson.fawkes
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[*] posted on 27-8-2009 at 08:39


Quote: Originally posted by jhullaert  
Another question. Should I inform the police? I know it sounds very silly but I really don't want to lose everything because they are suspicious for drug making etc.
That depends a lot on where your lab is. If you'd like informed assistance with this question, please say.
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Saber
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[*] posted on 27-8-2009 at 08:42


1. Generally the longer the condenser the better. It gives the vapour longer to condense. Go for things like graham condenser as opposed to liebig becuase they have more S.A but are more expencive.

2. I have a selection of flasks, 3 one neck (in 50, 100 and 1000ml sizes), 1 1000ml two neck and 1 1000 ml 3 neck, all in 14/23. The size of the flasks depends on quantities you plan to use. I use small flasks in organic synthesis becuase i have smaller quantities of product/material to work with ect... but when you are purifying litres of crude solvents its best to have a litre (or more) flask.


3. I would get one thermometer for low temps -50 to +30. one for normal temps -10 to 110 and one for higher temps (for use in oil baths ect...)

5. As in 1. i used to own a liebig but when i got a graham i found they were infinitly better and have stayed away from liebigs since. They are useless for condening solvents like ether but yes they are cheap!

6. As in 4. The size joint depends on the scale you wish to work with. the higher the joint size the more expencive it gets (margionally)

7. Not sure i uderstood 'One on top of the reflux condenser where I can put my liebig condenser on for destillation' that but i think i know what you mean. You must purchase a still head which is used for distillations.


The final question is a good point. As soon as i started making my lab i got a 'lab license' which basically entitles me to own any chemical (within limits- i cant own over 10kg of cyanide at any one time ect...) To get this license all my purchases were monitored for half a year and my lab was randomly spot searched for a year. Now i have it however everything i do is completly legal and in the name of science.
If you dont get a license though there is a very small chance something bad may happen. As ong as you dont store chemicas badly, keep listed chems (red P. Iodine ect...) you should be fine!
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Saber
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[*] posted on 27-8-2009 at 08:42


Sorry for some reason my post doubled

[Edited on 27-8-2009 by Saber]
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DJF90
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[*] posted on 27-8-2009 at 09:33


Saber: I agree with your comment about graham condensors being superior to liebigs. Although sometimes a liebig is much easier to clean. Also worth mentioning is the need for an air condensor, if you intend on distilling anything with a bp ~>150C. I would like to know more about this lab license you have, especially as you reside in the UK? How did you go about applying for one? Is there any restrictions on where the lab is (i.e. not in residentual areas)?
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jhullaert
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[*] posted on 27-8-2009 at 09:43


Watson.fawkes that would be great. thanks.

That lab license is very intresting. But are even iodine and red P listed chemicals? What would they say when they see my bromine? :P

Saber, I use small quantities (+/- 10 grams) So I guess a 250 mL would do the job?

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[*] posted on 27-8-2009 at 10:20


I thought an Ahlinn condenser was a refluxing condensers. Aren't they far cheaper than Liebig?

Either way, I got my Ahlinn for $10 at an Indian lab store :D
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jhullaert
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[*] posted on 27-8-2009 at 11:20


I don't think you can get an Allihn condenser with NS 29 joints for 10 bucks. :P The one you mention is probably one without a glass joint but it can be usefull though.:)
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DJF90
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[*] posted on 27-8-2009 at 11:20


You can get anything for $10 if you look hard enough and get lucky :D Unfortunately I'm not quite that lucky :(

[Edited on 27-8-2009 by DJF90]
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donlaszlow
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[*] posted on 27-8-2009 at 11:41


Even for less than 10 bucks. A few times I went trough the glassware and chemical trash of a clinical lab, and got some good stuff that I could either clean or get repaired :) Don't get into the biohazard one though ;)
The flea market is sometimes a good source for glassware, thermometers and some of the most unusual stuff ;)
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Saber
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[*] posted on 27-8-2009 at 12:11


@DJF90 - I do indeed own an air condenser but i use my graham as an air condenser when needed (just dont have any water input). I again find it more effective. Actually i found a good use for my straigh air condenser (of which i have 2). Fill it with small pices of boro glass (form smashed beakers TT ect.) and it make a awsome fractionating colum!

As for the Licence. I live in England yes, in the countryside so i have no problems with nosy neigbours :P
I went to my local police station and asked for a 'Research laboratory registration form' and filled it in. Its like a gun license (any one else have one?) but it asks questions like what kind of research are you doing? how many people will work there est... You then hand it in and they do 3 random spot checks within the year. They are rather scary but i have nothing to hide! they walked in on me synthesising some ibuprofen once which went down very well for my 'Pharmaceutcal Research' point i put in my registration. They told me they checked all orders i made from my credit card for one year but my supplier said nothing and i didint get any comments about it so i guess all was good! Then after one year i got this letter saying my licencing is complete ect... and there was a big list of what i must not own (>10kg K/Na/H CN, >15litres of phosgene ect..)
I am glad i did it but i took forever and like i say the spot checks take you by surprise. two men in white lab coats :P

Yep Ahlinn condensers are fine, they are fairly similar to liebig but they have bulbs making them more effective (higher SA ect...)
Ebay is a great place to find cheap quickfit glassware! things like plain beakers are a rip off though, £5 for one 50ml beaker... WTF!
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[*] posted on 27-8-2009 at 12:19


Hmm, well the narrow end of my Ahlinn condenser is a little chipped, any idea what I could do with that?

Any idea where I can get all the other stuff (excepting the condenser)? I want to make and distill some HNO3 and HBr.
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[*] posted on 27-8-2009 at 12:44


chipped as in cant fit it in the socket of the reciever anymore or chipped as in small insignificant chip?
Well i dont know any suppliers around Oregon but im pretty sure your Ebay will sell a lot of decent quickfit. They very often carry sets.

Can i just give some advise, before you start distilling HNO3 and HBr, do a couple of distillations of simple things like start with Sodium chloride solution, move on to ethanol/butanol mix then you can move on to the more hazardous stuff. The reason i say this, is i have seen it all to often in uni, naive people new to quickfit distilling hazardous fuming substances, heating the fask to quickly, only in one point ect.. and the flask breaking, spilling fuming acid (or whatnot..) everywhere. If you are doing this with Br2 then not only have you wasted expencive bromine but you have also filled you lab with a lot of bromine (however good your hood is it cannot handle 50ml of bromine, vaporised at 100degC. Spilling conc Nitric is not a laughing matter, especially if you are working on a wooden surface :O
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entropy51
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[*] posted on 27-8-2009 at 14:01


Saber, please tell us more about your license. It sounds like a police thing. Was the fire department involved? A member in Canada posted the following regulations:

https://www.sciencemadness.org/whisper/files.php?pid=159476&...

These regs require one hour fire separation from the rest of the building and require hood ventilation to outside the building. But apparently you have a ductless recirculating hood; I take it this was not an issue? Were you required to have a special storage cabinet for flammable liquid? At least two fire exits? Is your lab in a residential building?

I once helped set up a commercial lab and the interactions with the authorities were much more complicated than those you described. We had to use explosion-proof wiring and electrical equipment and it took forever. But congratulations! You may be the only legal mad scientist.

Edit: Did you have to make any special arrangements with your fire insurance company? We had a separate inspection by the insurance company, more involved than the fire marshall's inspection.

[Edited on 27-8-2009 by entropy51]

[Edited on 27-8-2009 by entropy51]
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DJF90
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[*] posted on 27-8-2009 at 14:23


Saber: can you please provide explicitly what you are regulated for? Like what chemicals are listed and quantities, and also other requirements you must adhere to (eg. emergency measures in place - eye wash station, emergency shower, fire/CO alarm, etc etc). I just searched the local police force's website and there is no mention of this form when I search for "research" or "lab", and only one hit (for alcohol) under "licensing". Perhaps its a regional thing (Thames Valley is the police force here)?
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Saber
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[*] posted on 27-8-2009 at 15:16


I am allowed to own any chemical i desire, as long as it is under the correct quantities and as long as storage is suitable. Here is Britain our H+S are surprisingly light on storage of chemicals. I got a requested visit from a H+S lab expert and he said by law i do not need to store things like acetone, hexane ect. in a flammable liquid cabinet. only solvents such as CS2 must be or solids such as white P (i own 500g of WP sticks :) )
I own no radioactive substances so that makes life a lot easier!

I am currently in the USA but when i get back i will scan in a copy of my chemical wheight limits.

Here is the list of safety features my lab has;
Emergency shower/eyewash
Foam,water and CO2 fire extinguisher
fire blanket
Sand bucket
Clear signs(fire escape ect.)
2 CO alarms, one near my hood, one on the ceiling.
Smoke alarm
Fire door

My H+S adviser said that is more than enough, the shower was overkill...

As to the firefighters, nope they were not involved. I have insured my lab but it costs a fortune! My H+S expert gave me the fire concerned safety precautions,
My recuirculaitng hood was deemed safe and proper. I see Picric-A was getting worried as to their effectiveness but i find them better than ducting, they look neater, you can move them and are cheaper (in the short run!)

Honestly at first i thought the license was regional but then i have been in contact with another privatly owned (but not home chemistry like us- this dude is proper) lab and he told me he went through the same procedure...
@ DJF90 lets chat by U2U and i can give you more personalised advise onto this matter


Being a legal home chemist makes me feel safe in the eyes of the law. It means i can stock I2, HI, red P and others which i would be scared to use otherwise. HI is a invaluable reagent (cleaving of ethers ect..).


Because there is only me and my lab partner (who uses this account aswell as me, rather like Ozonelabs i hear) i only have to have two doors. there are not many regulations i must follow (i follow them lazily i guess)
I will scan in the forms and stuff relating to this matter.

[Edited on 27-8-2009 by Saber]
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entropy51
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[*] posted on 27-8-2009 at 15:33


Saber, I find your stated timeline somewhat odd. Less than one year ago you said:
Quote: Originally posted by Saber  
Hi i am new here and i am new to home chemistry.
For my fist post i wanted to ask a simple question:
What glassware should i buy or can i use things like jam pots ect..?


And less than one year after asking about jam pots you say that you have passed the one year probationary period for your research lab license and that you have a hood and emergency shower. Quite an amazing evolution!

I have little knowledge of legalities in Great Britain, but in the US the fire marshall would have been extremely involved in inspecting your facilities. 500 g of white P would have raised eyebrows.

Not to put too fine a point on it, but I suspect you are putting us on.
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entropy51
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[*] posted on 27-8-2009 at 15:51


Quote: Originally posted by Saber  
If you are doing this with Br2 then not only have you wasted expencive bromine but you have also filled you lab with a lot of bromine (however good your hood is it cannot handle 50ml of bromine, vaporised at 100degC.


The aroma of skatole becomes stronger, Saber. The boiling point of Br2 is 59.5 C, which you would have known had you ever distilled any Br2.

And your spelling sux.




Better to remain silent and appear a fool than to open your mouth and remove all doubt.
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Saber
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[*] posted on 27-8-2009 at 15:58


Yep the time i was using glass pots was the time i didnt want my stuff to be raided by the british equivelant of te DEA. I then got registered and here i am now.
I think i have made my lab sound more impressive than it actually is.
Emergency shower is not hard, just a shower head attached to the wall from one of several extra water fittings i have under the sink. the wall under it is a platic shower base which runs off to the drain, simple! there is only me and my lab partner working in the lab so i have no problem stripping off in an emergency for the shower without a curtain and so you dont need a fancy shower... i will take pics soon in tour my lab.
As for the glassware ect, when you have friennds who work in labs it is easy for you to get accounts from fisher, griffin, phillip harris ect and form them i have attained all my glassware and chems.
The fume cupboard cost me £2000 from a friend of a friends lab (dont ask) and so i got that cheap!
They dont know i own 500g of white P but it doesnt matter!
Please be patient, stop pointing the finger for one week until i can scan in my docs to prove you wrong.

my final note to sum this thread up is its not difficult AT ALL to set up a lab at home as long as you have a)the money b) the contacts.
Just because i managed it in under a year and you didnt doesnt mean i am 'putting you on' that is a strong accusation without any proof.

Looking back on it, the amount i have learnt in the past few years is incredible, :)
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Saber
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[*] posted on 27-8-2009 at 16:01


Quote: Originally posted by entropy51  
Quote: Originally posted by Saber  
If you are doing this with Br2 then not only have you wasted expencive bromine but you have also filled you lab with a lot of bromine (however good your hood is it cannot handle 50ml of bromine, vaporised at 100degC.


The aroma of skatole becomes stronger, Saber. The boiling point of Br2 is 59.5 C, which you would have known had you ever distilled any Br2.

And your spelling sux.


Yep im dislexic im afraid, you are just going to have to get over it!

yes but when your distilling out Br2 you are boiling water too and im not sure about you but i dont set my heating mantle to exactly 59.5degC, do you? NO, you set it up to boil it off and water and whatever else, depending on you method of production. JESUS! are you actuallt that retarded?
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entropy51
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[*] posted on 27-8-2009 at 16:44


Quote: Originally posted by Saber  
They are rather scary but i have nothing to hide!


Really?

Quote: Originally posted by Saber  
They dont know i own 500g of white P but it doesnt matter!


Kid, I have nothing against you personally. I don't care if it gives you an erection to troll about your fantasy license for your jam pots.

But some poor kid may believe you and go down to the local police station and say "Can I get me one of them licenses for my chemicals?" And the result might be less pleasing to that kid than your fantasy is to you.

I'm dyslexic too, but I'm not a lazy teenager who uses it as an excuse not to learn how to spell and use the shift key every now and then. Your mum must have filled out the police paperwork for you since you can't seem to string a simple sentence together.



[Edited on 28-8-2009 by entropy51]

[Edited on 28-8-2009 by entropy51]
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[*] posted on 27-8-2009 at 21:03


Quote:
If you are doing this with Br2 then not only have you wasted expencive bromine but you have also filled you lab with a lot of bromine (however good your hood is it cannot handle 50ml of bromine, vaporised at 100degC.


50mls of bromine vaporized ALL AT ONCE is about 44 liters at STP.
How big is your fume hood? I can imagine some fumehoods handling that, especially if the vaporization is not simultaneously, which it wouldn't be in this situation.

Quote:

yes but when your distilling out Br2 you are boiling water too and im not sure about you but i dont set my heating mantle to exactly 59.5degC, do you? NO, you set it up to boil it off and water and whatever else, depending on you method of production. JESUS! are you actuallt that retarded?


Why are you calling him retarded? you are the one that claims a mixture of bromine and water will distill at 100*C. Also the temperature that something boils has nothing to do with the temperature you set your heating mantle at, as you have made it seem. Do you think maybe the bromine would distill off as an azeotrope with the water at a different temperature then 100*C? I sure do, but what do I know? I'm probably retarded as well.


Also what is the point of distilling bromine if you are also distilling "water and whatever else"?





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[*] posted on 28-8-2009 at 07:58


Even if you set your mantle to heat to 100*C to distill water, when the tempertaure reaches (well before you switch it on actually) you will get Br2 distilling! At 60*C next to no bromine would be left in bromine water and at 100*C well... unless you changed your receiver... you'd get more bromine water!

I asked a policeman today about licensing a research lab, to his knowledge, he had no idea what I wastalking about but said he would enquire and get back to me!

I recall a glassblower I know being insepcted by the police when he first started up, and they told him what he had to watch out for. But not licensed and it was a suprise to him that they came out to check what his company was.




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[*] posted on 28-8-2009 at 13:25


I can give a damn about his safety shower or white phosphorus, I want to see his version of the Contact Process. I and a friend built one and documented it, and I've repeatedly asked to see photos of the one he claimed to have built. If he can show me that, he's got me convinced.



Neither flask nor beaker.


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entropy51
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[*] posted on 28-8-2009 at 13:47


Fleaker, he posted a pic of himself operating it earlier:

http://www.careers-scotland.org.uk/upload/rag5-d.jpeg

I'll eat every microliter of acid he can make as syrup on my pancakes.:P
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