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Topic: Easy Anhydrous AlCl3 production equipment  (Read 16460 times)

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Offline Archer

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Re: Easy Anhydrous AlCl3 production equipment
« Reply #15 on: May 10, 2014, 03:40:28 AM »
Because it doesn't give off copious quantities if hydrogen gas, it is a little safer. Chlorine is dangerous to say the least, but so is HCl.  408.

In what way is chlorine gas is safer than hydrogen? If you vent hydrogen appropriately then the risk are very low. Chlorine cannot simply be vented outside.

Sudden accidental inhalation of chlorine is fatal at around 10 ppm the LEL of hydrogen is way in excess of that.
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Offline Zyklonb

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Re: Easy Anhydrous AlCl3 production equipment
« Reply #16 on: May 10, 2014, 10:31:36 AM »
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In what way is chlorine gas is safer than hydrogen? If you vent hydrogen appropriately then the risk are very low. Chlorine cannot simply be vented outside.
Yes, but as I said, I did it mostly because I can isolate chlorine cheaper than I can generate hydrogen chloride. Safety wasn't my biggest concern. I've done many more reactions which used much more toxic gasses, chlorine is jut another.  Obviously this wasn't done outside, [Meant inside] it was done in my lab and outside during different stages of the reaction. All of the gasses were also scrubbed, but even this wasn't needed, as the leftover chlorine was "dumped" far away from any people. 
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Sudden accidental inhalation of chlorine is fatal at around 10 ppm the LEL of hydrogen is way in excess of that.
Care to provide a ref. for that statement?
The first time I made measurable quantities of chlorine, I was stupid, and inhaled some. I'm pretty sure I got more than 10 PPM, but I could be wrong. I did thro up afterwards though...   
« Last Edit: May 10, 2014, 12:09:22 PM by Zyklonb »

Offline Archer

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Re: Easy Anhydrous AlCl3 production equipment
« Reply #17 on: May 10, 2014, 11:32:35 AM »
Safety wasn't my biggest concern.
 

Well it should be

Quote

The leftover chlorine was "dumped" far away from any people. 

Dumping any chemicals without a licence is extremely irresponsible, no matter where it is

Quote
Quote
Sudden accidental inhalation of chlorine is fatal at around 10 ppm the LEL of hydrogen is way in excess of that.

Care to provide a ref. for that statement?

http://toxnet.nlm.nih.gov/cgi-bin/sis/search/a?dbs+hsdb:@term+@DOCNO+206

   B)  The OSHA time-weighted average permissible exposure limit
       (TWA PEL) is 1 ppm, and the NIOSH immediately dangerous
       to life and health (IDLH) level is 10 ppm.

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The first time I made measurable quantities of chlorine, I was stupid, and inhaled some. I'm pretty sure I got more than 10 PPM, but I could be wrong. I did thro up afterwards though...   

I am very pleased to hear that you did not seriously injure yourself.
“ I love him. He's hops. He's barley. He's protein. He's a meal. ”

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Offline Zyklonb

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Re: Easy Anhydrous AlCl3 production equipment
« Reply #18 on: May 10, 2014, 12:08:15 PM »
Ok, well what I should have said is safety wasn't something I was exceptionally worried about. I also failed to mention I was wearing a gas mask, which make a big difference.
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Dumping any chemicals without a license is extremely irresponsible, no matter where it is.
I made a total of 4 grams of AlCl3. Theoretically, this requires  ~.67 liters of chlorine. Because this is the theoretical yield, I generated ~.75 L Cl2 to compensate for inevitable losses. This means ~89% of the chlorine was used up. Which means only 0.0825 L of Cl2 escaped the reaction chamber. Because it was scrubbed out, I highly doubt any sizable amounts of chlorine went into the atmosphere.
Nice link, quite infinitive.
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I am very pleased to hear that you did not seriously injure yourself.
Thanks, I guess. I don't know why you are underestimating my safety procedures. This reaction is nothing compared to some of the more elaborate reactions I've done. 
[EDIT]All of the reactions I do are with all safety precautions in place, I know what I'm doing.

Mod edit: Offensive language removed. Dan
« Last Edit: May 10, 2014, 02:33:40 PM by Dan »

Offline Archer

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Re: Easy Anhydrous AlCl3 production equipment
« Reply #19 on: May 10, 2014, 02:57:34 PM »
Obviously you don't know me but I am being genuine that I am glad that you were not seriously injured by gassing your self with chlorine, presumably you did not have your gas mask on at the time of the incident.

When a chemistry hobbyist is found dead or very seriously injured, the fist question the police ask is regarding the manufacture or attempted manufacture of controlled substances.

When this has been ruled out the coroner or the hospital occasionally seeks counsel as to whether there is a possibility that the injuries sustained were accidental or intentional.

For reasons best known to themselves coroners rarely pre-warn you that there are graphic images in the file.

Maybe if you had seen a persons face who has died from acute exposure to toxic gasses you may understand my concerns over unsafe practices in any lab, whether it be in a kitchen or a fully kitted out state of the art industrial facility.
« Last Edit: May 10, 2014, 04:44:37 PM by Archer »
“ I love him. He's hops. He's barley. He's protein. He's a meal. ”

Denis Leary.

Offline Zyklonb

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Re: Easy Anhydrous AlCl3 production equipment
« Reply #20 on: May 10, 2014, 03:39:26 PM »
I am glad that you were not seriously injured by gassing your self with chlorine, presumably you did not have your gas mask on at the time of the incident.
I appreciate your concern, and you're right, the first time I made isolated chlorine, I wasn't wearing a gas mask. Please understand this was a long time ago. Long before I had much experience.
I was just browsing this forum for the first time, and saw this thread, seeing that nobody had actually experimented with the procedures mentioned, I decided to give my 2 cents worth since I had already done the reaction. I don't understand why you felt like you needed to derail the topic. I know chlorine is toxic. Of course you didn't know that I knew that.
I understand that this board is more for beginners, but I thought you guys would be interested in somebody's personal experience rather than just idea's floating around. 

Offline Borek

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Re: Easy Anhydrous AlCl3 production equipment
« Reply #21 on: May 10, 2014, 03:54:52 PM »
I thought you guys would be interested in somebody's personal experience

We are.
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Offline Archer

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Re: Easy Anhydrous AlCl3 production equipment
« Reply #22 on: May 10, 2014, 04:01:11 PM »
I thought you guys would be interested in somebody's personal experience

We are.

Indeed

I have prepared anhydrous aluminum (III) chloride from chlorine gas and aluminum.(2 Al + Cl2  :rarrow: 2 AlCl3) Because it doesn't give off copious quantities if hydrogen gas, it is a little safer. Chlorine is dangerous to say the least, but so is HCl. The reaction (as one would expect) is self sustaining, and further heating is not required. Everything was done in a SS setup, and the heat generated was used to distill the product.
I hope to try the zinc chloride and aluminum reaction as it will probably be much easier, and certainly safer.
The main reason I used chlorine is because at the time I didn't have much concentrated sulfuric acid, which I would have used to make HCl(g). The chlorine was isolated as such: Ca(OCl)2 + 4 HCl(aq)  :rarrow: CaCl2 + 2 H2O + 2 Cl2. BTW, I am very new to this forum, but that doesn't mean I'm a beginner, I'm very active on the Sciencemadness forum, as linked above by 408.

I wasn't intending to derail the topic, I intended to highlight to the OP and all of the other amature chemists on here the hazards involved in this process of making chlorine.

Some people will take the information above and just give it a go, having done absolutely no risk assessment.

It is best not to assume experience, knowledge, or a general appreciation of self preservation on Citizen Chemist. This is only my opinion but I am sure that others agree.

“ I love him. He's hops. He's barley. He's protein. He's a meal. ”

Denis Leary.

Offline Zyklonb

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Re: Easy Anhydrous AlCl3 production equipment
« Reply #23 on: May 10, 2014, 09:35:39 PM »
Ok, well thanks for the explanation. Either way, there isn't much more to say about the synthesis. I would enjoy reading other people's accounts on the subject though. I might try a safer method which requires neither chlorine or hydrogen chloride. Direct combination of the elements is by far the cheapest method and is used industrially. 
My next attempt will probably be the so-called ''Chlorothermal reactions'', using zinc chloride to oxidize aluminum as mentioned here https://www.sciencemadness.org/whisper/viewthread.php?tid=30150. I ran out of zinc chloride recently, but it's fairly easy to make or buy http://www.ebay.com/itm/ZINC-CHLORIDE-ZnCl2-800G-ASSAY-99-0-HIGH-GRADE-/201084391150?pt=UK_BOI_Medical_Lab_Equipment_Lab_Supplies_ET&hash=item2ed1904eee.

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