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Author: Subject: H2S intoxication
Klute
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[*] posted on 10-5-2008 at 03:53
H2S intoxication


I'm just recovering for an H2S intoxication.... Things are getting better now, but it was scary...

I was performing an Zn/HCl reduction of a Bunte salt (alkylthiosulfate), which evolves H2S along with H2. I will post details of the reduction latter on. Two scrubbers in series were attached to the reaction flask, a 30% NaOH and 10% NaOCl. Theses were very efficent, though at one moment the first NaOH got plugged by what seemed to be sodium (poly)sulfides, so the bleach washbottle was attached first. It turned yellow over a few minutes and sulfur particules appeared, it didn't change appearance before, so the NaOh seemed to handle the H2S pretty well. I wore a gas mask at all times, one that is efficient at protecting from things like SO2, HCl, organic vapors. The cartdriges weren't new though. When I had to refill the addition funnel, i got a slight smell in the gas mask, so I went to take some fresh air, and did so regularily after. I was working in a garage with the large door (the one to let the car in) wide open, and a normal door on the opposite side wide open too. It was very windy.

The reaction finished, it was letf to stir over night. A current of argon was passed for a few minutes, expecting it to chase away remaing H2S. The grey sludge was transfered to a seperating funnel, and extracted 3 times. The smell was pretty strong when I took the gas mask off, so I spent as little time as possible in there, just the time to seperate layers and add more solvent.

Then i started to get dizzy. I realized i didn't sense the smell in the gas mask at all, though a relative passing by was disgusted by it. My hands started to shake, my heart beat raced, and I felt wxeak. I closed the sperating funnel immediatly, and went outside. The symptoms weren't going away. I advised my relative I wasn't feeling well, and that if things didn't get better soon, they would have to take me to the hospital. I had a bad taste in my mouth, and dry saliva.
I checked the dosage for sodium nitrite, which I had on hand, and finally decied on injecting 50mg in 1mL. I was lucky enough to manadged to inject myself with my hands shaking. My heartbeat suddenly increased as the nitrite came up. The arm was a bit painfull at first, i had stings and needles for 5min, but them the symptoms gradually decreased. My hands stopped sahking, and I am generally feeling better now. I am waiting to see how things evolves, and am considering seeing the doctor or hospital, been concerned about delayed pulmonary oedema. I will have to got and clean up the lab at a moment, but prefer waiting until most of the smell is gone. I will neutralise the sludge with Ca(OCl) or large amount of NaOH, taking in acount that over 350mL conc HCL is present.

Any advice on neutralisation is welcome, aswell as any experience with this kind of poisoning, particularily the delayed effects.

I would recommend anyone willing to handle H2S out of a proffessional environment to SERIOUSLY reconsider. I was very lucky this time. If i had stayed a few minutes more, I could have fell unconscious, at which point I would have put my life and the one of my relatives at serious risk.

I don't understand how the authors of the publications I have read proceeded to do the workup, even in a fume hood, without being exposed to the gas.

[Edited on 10-5-2008 by Klute]




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[*] posted on 10-5-2008 at 05:24


Wow, Klute, that is quite an experience you've had! And your writeup of your experience is very good!

If something like that were to happen to me, I definately think I would go to see the doctor! Pulmonary Oedema might not be evident after as long as two weeks!

For now, take care :)

EDIT:
PS: I surely hope it won't come to this, but if it should:
When you inject the NaNO2, do you inject it sub- cutaneously, intramuscularly, or intravenously?

[Edited on 10-5-2008 by ScienceGeek]




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[*] posted on 10-5-2008 at 06:06


IV injection. I would definatively advise to get proper medical dosage, I did this out of panic, sodium nitrite is a poison itself. Boy did i feel weird opening a reaent bottle and preparing a shot with it...
The correct dosage are:

Sodium Nitrite (3 % IV solution):
Adult: 10 ml at 2.5 to 5 ml/minute, or 0.35 ml/kg IV push
Child: 0.2 ml/kg not to exceed 10 ml.
source

Not having a catheter, and not wanting to put one anyway, i did a push injection (all in 1 go), but only 50mg instead of a 63mg (i weigh just under 60kg), not wanting to making a too concentrated solution. It was painfull.

I really do not advise anyone to do what i did, only if there are no other options. I'm not a doctor, and have virtually no knowledge in the area. Nitrite treatment can be hazardous itself. And injecting yourself in such a situation is very delicate. In good conditions, someone who never injected himself will have difficulties, so doing so when your hands are shaking and your are in panic, would be near impossible. I (un)fortunaly have experience with injection so managed to do so correctly and quickly.

For the moment, i feel that i have completly recovered. Just a salty taste in the mouth from the injection. I will see a doctor and tell him what happened, i know both H2S and NaNO2 can cause some disorder in blood equilibrium and such. For the moment i have no problems at all with breathing, so I'm crossing my fingers.

I have clean most of the glassware and neutralized the solution with Ca(OCl)2 conc solution. I was surprised at the amount of sulfur it deposited, meaning there was a pretty large amount of dissolved H2S...

I will go back at using S2Cl2 for futur sulfide synthesis now, it nearly seems like a harmless compound compared to H2S!

Once again, i was very lucky. I have to insist on warning anyone out there considering a reaction involving/generating H2S. The thrill is nothing compared to your life. I don't give a fuck of the end product now, even though I've kept the extractions and washed them with brine to remove most of the dissolved H2S. I will never risk my life for a reaction again, and never under estimate the toxicity of a compound, or over estimate the safety conditions I work in at home.




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[*] posted on 10-5-2008 at 06:26


Thank you for the details on injection! I hope I'll never have to use any of the information you gave me!

Regarding your experience with dangerous procedures, I'm glad to hear that you won't do it again! To me it seems that you took all the necessary precautions possible for a home chemist (maybe a fume- hood would have done a better job in removing the H2S), but still!

Good luck in the future involving dangerous procedures! I hope this experience haven't put you completely off syntheses involving some degree of risk! :)




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[*] posted on 10-5-2008 at 06:45


Woa that is pretty impressive :o sad to hear about this :(

I hope you fully recover well!
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[*] posted on 10-5-2008 at 07:36


IIRC H2S does not cause pulmonary edema, but nevertheless, it is good to see a doctor. You have had good luck that you realized just in time how dangerous the situation was. I, however, in your situation probably would have gone outside and lay down in the grass or something like that, far away from the H2S, in fresh air.

Fortunately I never encountered really dangerous situations in my home chemistry experiments, I usually work with very small quantities.




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[*] posted on 10-5-2008 at 07:47


Instead of the difficult and hazardous IV injection if sodium nitrite, would inhaling some butyl or amyl nitrite have the same effect?
Amyl nitrite is recommended as a first-aid antidote against HCN in my OC book, along with intravenous NaNO2 later by the doctor.

So would making a small amount of an alkyl nitrite before working with H2S or HCN be as good or better (because of the ease of inhaling it versus having to do an injection of NaNO2) than keeping a shot of NaNO2 ready?




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[*] posted on 10-5-2008 at 08:01


why dont you all just use a fume hood...even if you have to invest some time, money and work, what is this compared to your life?



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[*] posted on 10-5-2008 at 08:19


I definitevely want to build a fume hood. I just thought i could manadge this reaction without it, but that was underestimating H2S.

Taking fresh air is the first thing I did, the time i got less dizzy and considered the situtation. A certain number of MSDS i have consulted claim H2S exposure causes delayed (from a few hours to days) pulmonary edema. I have contacted my local anti-poisoning cneter, explaining them what happened, they said as far as all symptoms are gone there sin't anything to worry about anymore. They did advise me to see a doctor if i feel some disconfort while breathing. They obviously told me to consult a doctor immediatly when this happens, and to never inject any antidote by myself again, even if it is a known one.

Amyl nitrite is said to work waiting for a NaNO2 injection, but can't suffice alone, at least from what I've read. But i guess it's the best thing to do while waiting for proper treatment. The quicker after the exposure, the better.


I'm very glad I got out of there as soon as I felt something was wrong, but feel very stupid of even getting to that point. I am seriously reconsidering improving the security conditions before doing any other reaction, in case of un-planned events.
Indeed, a few hundred euros a few weekend's work are nothing compared to life, or even health. And that smell.. brr...




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[*] posted on 10-5-2008 at 08:26


Well, this is the first forum-declared case of H2S poisoning that I've ever come across. Scary... especially as I've been around the gas quite a few times. Al/S or Al/CaSO4 boosted thermites of SiO2, TiO2 (and potentially others) that I routinely use, all produce rapidly hydrolyzing sulfides like Al2S3 and CaS and the smell of rotten eggs coming off the slag (even when freshly fused, thus 100 % dry) is often intolerable. I dispose of them usually by soaking in bleach, prior to binning.

It's to avoid the terrible smell I developed S-free booster packages, based on KClO3 or nitrates. But I still occasionally use CaSO4/Al (--->CaS + Al2O3) because it's so powerful as well as cheap as chips.

It kind of begs the question: what's the concentration of H2S at dangerous levels and how to pre-emptively detect it?

And it makes you wonder how many cases of this kind of poisoning must have occurred when the Leblanc process for the production of soda was still in use: it produced hundreds of thousands of tons of CaS watery slurry (the so-called galligu)... :mad:


Quote:
Originally posted by stoichiometric_steve
why dont you all just use a fume hood...even if you have to invest some time, money and work, what is this compared to your life?


If concentrations reach danger levels, spewing the stuff into open air in a residential area is hardly considerate... Some kind of scrubbing/incineration would be advisable.
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[*] posted on 10-5-2008 at 08:32


One could just feed the exit of the apparatus into the air intake of a bunsen burner, this will efficiently take care of the H2S without the need for additional chemicals.
Also install some backdraft protection, like stuffing a piece of steel wool into the pipe, to avoid igniting a H2S/air mix inside the apparatus.




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[*] posted on 10-5-2008 at 08:57


But then wouldn't you have sulphur dioxide to contend with? Which I find quite unpleasant. :(



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[*] posted on 10-5-2008 at 09:07


SO2 is not nearly as toxic as H2S. SO2 is tolerable up to 10 ppm or so, H2S is very dangerous already at 1 ppm. The only trouble with SO2 is that it can induce astmhatic attacks in allergic people, but normally it is not that toxic.



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[*] posted on 10-5-2008 at 09:10


Garage chemist, if you lead it into a Bunsen burner though you're going to get acrid sulfur dioxide instead, safer but still a pain in the butt.



That's a picture of my wash bottle from reacting carbon with sulfur. It made plenty of H<sub>2</sub>S. At first it was just NaOH (aq) in there to absorb any incidental generation (didn't think there would be much) but my grandmother came out and told me she smelled rotten eggs. I couldn't smell a thing, so, panicking somewhat I dumped some aqueous copper sulfate into the solution to see to what degree it was saturated (I expected most of it to just turn into blue precipitate) and instead of what I expected it turned into a fine black powder seen in the picture. Anyway in retrospect I may have been experiencing some tremors or weakness but not to the extent you mentioned. Still, it was surprising that it killed my sense of smell, I might have caught a hint of it, that was it.




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[*] posted on 10-5-2008 at 09:49


NaOH solution seems very effective at handling H2S, but you need to plan on using alot of it. As mentionne dearlier, at one moment, the tube going down in the solution got clogged up with some white solid, surely sodium sulfides. I'm not sure if it's better to use a >30% solution of NaOh, for maximum absorption, or a more dilute one that will dissolve more sulfides.
The bleach scrubber was pretty efeective too, it turned yellow after a while with fine solids in suspension. No clogging up at all.
Both were pretty hot (>40°C) from the large flow of H2S generated.

the best way of getting rid of it in a fume hood would be to avoid release some as much as possible, using washbottle and such, and maybe use a solid Ca(OCl)2 "screen" in the evacuation tube.
I think H2S get's oxidized pretty quickly in the atmospher anyway, the smell didn't stay long once all the solution/glassware were neutralized.




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[*] posted on 10-5-2008 at 10:57


In response to some of the NaNO2 injection and akyl nitrite inhalation questions I have done much research on the subject. The alkyl nitrite inhalation may save you if you inhaled a small amount. It's to keep you from passing out (or dying) before the more involved injection can be done. It wears off within a few minutes so the subsequent injection is almost always done.

If you plan on making up an injection kit use USP (or whichever Pharmacopia grade you have in your country) NaNO2. That's what is used in the professional antidote kits. If you prepare the solution before hand adding .075% (by weight) sodium benzoate and 1% w/w citric acid will make the solution bacteriostatic (a must for anything entering your body, especially IV). ALWAYS use sterile water (if you don't have access to this at a hospital you can order it online or sometimes use eyedrop solutions THAT CONTAIN ONLY SODIUM CHLORIDE can be used if it says it is sterile). MEASURE OUT THE NaNO2 CORRECTLY. USE LESS RATHER THAN MORE (50mg). Also, this is for other drugs and not specifically NaNO2. Also, make sure the pH is neutral! Benzyl alcohol can also be used in place of sodium benzoate but it can be harmful. Apparently they had to take it out of infant medicine because it was causing deaths. It's still used, though. Actually, it's probably more common than benzoate. DO YOUR OWN RESEARCH. THESE ARE JUST SUGGESTIONS.

EDIT
After some research I now recommend BnOH. If you need BnOH USP (it will be repacked under non-USP conditions but it will be clean) I have it. I also have sterile water.
Quote:
Bacteriostatic Water for Injection, USP is a sterile, nonpyrogenic preparation of water for injection containing 0.9% (9 mg/mL) of benzyl alcohol added as a bacteriostatic preservative. It is supplied in a multiple-dose container from which repeated withdrawals may be made to dilute or dissolve drugs for injection. The pH is 5.7 (4.5 to 7.0).
From: http://dailymed.nlm.nih.gov/dailymed/fda/fdaDrugXsl.cfm?id=1...

I would do this even if you don't need to make multiple extractions simply because the environment inside the home is not "clean". Also, NaOH and HCl are used to adjust the pH of parenteral solution. DO NOT USE A POTASSIUM BASE.

Like Klute pointed out doing an IV injection without experience, ESPECIALLY ON YOURSELF, is damn near impossible so, if you are really concerned with poisoning, learn how to do it very well or teach someone else that will be in the area how to do it. I mentioned this and was told that my girlfriend would leave me if I told her that ;) Actually, I did tell her about it and she said it was good that I was taking every possible precaution (even with a fume hood and SCBA gear, accidents happen).

I used to sell hypodermic needles (legally and not to "junkies", I hope) so if you live in a state (I don't think I want to ship something like that overseas where it might be illegal) that won't sell them without a prescription (or if you don't want to be seen buying them) I will send you some. I would actually ask you to reconsider the experiment first but if you're set on doing it, I'd rather help you out with the supplies than not.

P.S. Check your state laws. In most states, simple possession is not a crime even if they require a prescription to buy. Drug paraphenilia can (usually, I'm not sure now with the state of this fucked country) only be claimed if you have drugs. Just don't carry them in your car! Duh! I have to do it but they are all in the packages and I have no drugs so... Also, IV injections are not as finicky and unforgiving as everyone believes. BE CAREFUL, but also don't believe all the hype.

Anyway, I'm rambling now. Just everyone be safe and take every precaution. If you don't feel comfortable having to do something like this, don't do the experiment. This can be dangerous. Do your OWN research and do not rely soley on mine. You should always do that, by the way.

Also, I was unaware, until now, that nitrites were an effective H2S antidote. Interesting.

EDIT
You should let the hospital or doctor do the injection. However, if you think you can do it properly, the sooner the better. The poisoning is WAY more likely to kill you than the injection (it's pretty unlikely, really). I would actually be scared to go to the doctor. Can you imagine the questions? I mean, I called the poison control center once to ask about iodine poisoning. They WOULD NOT give me any information without taking my full name, phone number and address down. Naturally, I declined (and called from a payphone). They kept asking, "How did you get exposed to iodine? What were you doing? Where was the iodine located? (asking for an address). I called a few weeks later (out of curiosity) about mercury and they asked no such questions. God I hate the meth scare. Now you can't even get medical assistance anonymously if you are messing with chemicals that could be meth precursors (I know H2S is one on some list somewhere, along with almost every other common chemical).

[Edited on 5-10-2008 by MagicJigPipe]




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Klute
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[*] posted on 10-5-2008 at 13:46


In my country it's totally legal to posses injection equipment. Sterile equipment is distributed freeely by harm-reduction associations, one of which I am a member.
Although sterile water and filtering was sued, the sodium nitrite was far from USP, being a technical grade. I wasn't going to do a fuss about that at the time. Considering it's 90% minimum, that's 5mg impurities maximum, mostly sodium nitrate, so I'm not too concerned.

You are right to point out that no potassium salts should be used IV. This can cause immeadiate heart failure.

Again, i wanted to share my (bad) experience, but do not advise doing this in case of hydrogene sulfide poisoining, unless there absolutly no other solution. Only a trained medical personal can decide on nitrite treatment, and taking charge correctly of such an intoxication.




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[*] posted on 10-5-2008 at 14:32


Thanks for posting that Klute, the safety measures you have - gas mask, breeze throgh work place, frequent trips outside, conc. NaOH scrubber (I never bother with 2) sound very similar to mine, which I thought effective. So this could have happened to me, and serves as a good warning.

The one difference I have is a fume hood, but its not all its cracked up to be - you still have to open it to wash precipitates, dismantle apparatus, and especially in the cleanup, thats when you get exposed. Even if you do all that in there, the protection is then only 50% effective.

Gas masks we use are not war gas masks, if you wore them during a phosgene attack, you'd die. Thats because the switch mechanism from in- to exhale is a trivial diaphragm, you still get up to 10% of your gas from outside. So thet offer protection up to 10x allowable exposure - bot no more.

It is possible, though not a relief, that the hands were shaking from anxiety once the diziness set in and you realised what happened - thats just some observations ive done on myself
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[*] posted on 10-5-2008 at 15:19


Yes Len, I was pretty surprised myself considering the conditions, and the only rare times I actually smelled the gas. The hands shaking was actually what made me realize this wasn't just dizzyness from keep me breath when opening the apparatus, as I sometimes have. It was pretty spooky, because uncontrolable. I manadge to calm myself pretty well just before injecting the antidote by deep breath and emptying my mind.

I have just finished removing the solvant: the recovered product is neglieable, i guess toluene isn't a good solvant. I risked my life for nothing :D Better laugh than cry about it...
So back to S2Cl2 when the fume hood is up then! :)




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[*] posted on 10-5-2008 at 16:03


I also use the hold-your breath trick at tricky moments, even in a gas mask.

Still Im trying to understand the source of the problem, because I havent completely given up on H2S work, and I consider this work as a mandatory prelude to any work with cyanides.

I am also in a much less enviable position then you. This sort of hobby is very borderline here, much less understood than in europe - I can not afford any serious mistake, one ambulance or fire-brigade call, and thats it. And it'll just reinforce the prejudices of the masses regarding our hobby.

So it would be of help to know the scale of your work - how many moles of H2S got generated?

Also, the error I understand was the clogging of the tube and the momentary disconnect of the traps. Or was most H2S released during work-up?

As I understand a fume hood or a 'professional environment' will really not solve anything - the same thing can happen there. My lab hasnt a hint of smell in it while the reactions are going on in the fume hood. Its beautiful and you can enjoy yourself. But it all changes when the hood opens during workup or cleanup.

Presently I think the essence is this:

the key advantage of H2S, our ability to detect it in tiny concentrations, is a faux ami, it lulls you into a false sense of security. A reliable H2S detector needs to be found and several located in the lab. If thats triggered, a response (other than just fleeing the lab) should be prepared.

[Edited on 11-5-2008 by len1]
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[*] posted on 10-5-2008 at 16:04


Wow, that is really something. I'm really glad you are ok. I got Cl2 poisoning 5 years ago and it was not fun. Took me a month to get better (meaning I could stop worrying that I'd just die in the middle of the night), and about a year to feel completely ok again :(



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[*] posted on 11-5-2008 at 00:54


Quote:
Originally posted by BromicAcid it was surprising that it killed my sense of smell


H2S can only be detected in LOW concentration by the human olfactory sense.

The rule is: If you know you SHOULD be smelling it and you DON'T -> GET THE FUCK OUT!!!




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[*] posted on 11-5-2008 at 05:38


Quote:
Originally posted by len1

So it would be of help to know the scale of your work - how many moles of H2S got generated?



That seems to be the crucial question to me here. Many of use will come into contact with H2S during various experiments, it's a frequent by-product of sulphur chemistry but few will suffer adverse effects like Klute...

For that reason it would be interesting if Klute could estimate, even roughly, how many moles of hydrogen sulphide were generated during the course of that job. Generating H2S as an unwanted by-product is one thing, using it as a reagent quite another and would, IMHO, require different types of precautions...
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[*] posted on 11-5-2008 at 05:45


The reaction itself liberated 0.2mol of H2S, most of which were completly neutralized by the scrubbers. The
2 times I had to open the setup (recharging the addition funnel with conc. HCl and swapping the scrubbers, I just got the bad smell and nothing more, no disconfort at all.
The intoxication was noticed at the third extraction of sludge, contained in a large seperatory funnel, always leaving the place between washes and letting time to settle, so i wasn't in there for more than 2-3min at the time. The beaker used to contain the sludge when sperating the toluene was left in the air, which was probaly a mistake, as it offered a good surface for desorbtion. The flask was immeidatly washed with dilute hypochlorite after transfering the sludge out, so I guess the gas came from the seperating funnel, and much more when emptying it in the beaker.
I'm sure an efficent hood would have minimized exposure, but you would need a vey high flow and the sash way down, as the gas is heavier than air... Although it was very windy in the garage (can't leave a piece of paper not pressed down by an object, even a empty PP mesuring funnel had to be placed on the floor as it kept on falling), the geometry, and the furniture must have prevented a efficient evacuation.

The form of the garage is basically like this:
with a shelf in the middle, and the two doors on the sides. The wind was comming from the small door (on the right)

________bench______
|............||||||||||||........|
<...........||.....................|
<...........||.....................|
<................................<<<<
|__________________|



Funny you mention not sleeping at night, this happened to me, I felt that if I would go to sleep I would stop breathing, and I had arythmy (Sp?) when your heartbeat suddenly slos down then speeds off in a irregular way. I only had a few hours sleep. Now things are better, so I guess there was a part of anxiety. If this happens again tonight, I will talk to the doctor.

Actually, if I didn't call the medics when not feeling well, it was mainly for the same reasons as Len. Plus, i didn't want to leave a potential source of H2S unattended with relatives around, or with a medical team comming: they would have sent HAZMAT team (or the equivalent here). Legally, i don't think it's a problem having a small lab, but the insurrance wouldn't be happy of learning there are solvants and chemical stocked in the garage, albeit in small quantities. And the cops would surely think explosives or drugs and make a full investigation. i don't want to take the risk of falling on a cop that considers that if I have iodine and HCl, I'm surely making meth, if I've got diethylamine and methanol, I'm surely making LSD, nd if I've got H2O2 and acetone I was surely planning on high-jacking a plane so they might just aswell put death penalty back up...
Bref...

I'm starting my plans for the fume hood now, and I actually kept the syringe that possibly saved my life :) I don't think I'll show it to my granchildren if I have some though :D

[Edited on 11-5-2008 by Klute]




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MagicJigPipe
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[*] posted on 11-5-2008 at 08:15


Arythmia is irregular heartbeat. The slowing down of the heart below 60bpm (which isn't always bad, I've often had heatrates below 60bpm while I was in shape) is called bradycardia. Tachycardia is the opposite (above 100bpm, this is at rest and not while you are "applying yourself" physically).

All can be extremely dangerous if they are caused by a substance. Especially arythmia which can lead to a very bad type of arythmia called ventricular fibrilation (V-fib) which is basically when the electric signals that keep the heart in rythym get screwy and cause the heart to "tremble" rapidly instead of beat regularly.

V-fib is scarey shit. Seems like a horrible way to go. I even hate talking about it. So I'll stop.

[Edited on 5-11-2008 by MagicJigPipe]




"There must be no barriers to freedom of inquiry ... There is no place for dogma in science. The scientist is free, and must be free to ask any question, to doubt any assertion, to seek for any evidence, to correct any errors. ... We know that the only way to avoid error is to detect it and that the only way to detect it is to be free to inquire. And we know that as long as men are free to ask what they must, free to say what they think, free to think what they will, freedom can never be lost, and science can never regress." -J. Robert Oppenheimer
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