Author Topic: MM Nitro/Al-Hg variation: No HgCl2  (Read 7187 times)

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isohuman

  • Guest
MM Nitro/Al-Hg variation: No HgCl2
« on: January 31, 2002, 07:48:00 AM »
ISO-SWIM decided to try a new twist on the Methyl Man Nitro writeup.  ISO-SWIM decided that instead of using HgCl2, he would try Hg(2?)I2 instead(mercury blobs dropped into I2 tincture, ala unnilhexium).  The batch was done at a half scale, 12.5g ketone, 10ml MeNO2 and 13.7g aluminum foil.  The tincture, .24g Hg from a thermometer dropped in a 30ml 3% I2 tincture 1 week earlier, was dissolved in 400ml MeOH, and dumped into a 2L RB flask, to which the aluminum and a 2.5 inch stirbar had already been added.  Amalgamation took approximately 35-40 minutes, and once complete, the ketone/nitro was dripped in.  Do not wash the aluminum after amalgamation, this was tried and resulted in a failed run, without ever heating up appreciably during the addition.  The ketone was dripped in over the course of about 15 minutes, and the reaction proceeded as expected, and reached an impressive reflux.  The rest of the procedure was carried out as MMs writeup, and yielded 10.9g of the hcl salt.  Just in time for the weekend 8)

PoohBear4Ever

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #1 on: January 31, 2002, 08:39:00 AM »
Thank you for trying this:  :)  :)  :)

Props go out to unnilhexium,

PB

TranceMe

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #2 on: January 31, 2002, 08:20:00 PM »

The tincture, .24g Hg from a thermometer dropped in a 30ml 3% I2 tincture



:o Oh my, oh my!! And that's it? Life keeps getting easier and easier ;D


Chemically enhanced.

goiterjoe

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #3 on: January 31, 2002, 08:53:00 PM »
um, won't mercury in the elemental form amalgate aluminum?  People just tend to use the chlorine salt form because it makes the reaction run faster and clean up easier.

If Pacman had influenced us, we'd run around dark rooms eating pills and listen to repetitive music

Rhodium

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #4 on: January 31, 2002, 11:16:00 PM »
joe: The amalgamation would not be even and dead slow. Compare the area of 0.1g dissolved HgCl2 to the area of 0.1g solid Hg. Big difference, right?

TranceMe

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #5 on: January 31, 2002, 11:50:00 PM »

(mercury blobs dropped into I2 tincture, ala unnilhexium)



Can you please point me to this post? I can't find it UTFSE.


Chemically enhanced.

bicepules

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #6 on: February 01, 2002, 09:14:00 AM »

     Yes, yes I to would like to see a little more here to.  Came up with nothing UTFSE. 

"No I'll tell you what insanity is, insanity is majority rules"

noj

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #7 on: February 01, 2002, 09:27:00 AM »
I believe it came from TSII. Do a search on "HgI2" if you need information. BrightStar mentioned it being the least desireable of the Hg salts for amalgamation, but that was in relation to water solubility. Hellman had a thread on it several years ago, but it has been purged.

Real men cook naked.

isohuman

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #8 on: February 01, 2002, 03:59:00 PM »
I guess TFSE isn't working properly, I couldn't find the post, but it was on a thread about peracetic acid, where unnilhexium made mention of his amination technique using I2 tincture.  I don't know if that was a unnilhexium original or not, he was just the first bee I saw posting about it.  Anyhow, for those of you worried about side reactions, the residual I2 seems to form some kind of alu-halide, as the red color leaves the solution during the amalgamation.  Also, the tincture adds about 15ml of water to the reaction, which should keep Osmium off your case ;)   BTW, it important to periodically shake the tincture bottle, to break up the mercury blob so that it can react.  Also, make them as far in advance as possible.  They can be made weeks, months or years in advance, IT'S JUST TOO EASY!!!!!!!!!!!!!  Isn't that so much nicer than making or buying HgCl2?

mushhead

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #9 on: February 01, 2002, 05:06:00 PM »
Wow!  If this works as advertised, SWIM will be a very happy person.

By UTFSE, I found a couple of posts from hellman.  He didn't give much detail but insists it works. 

Here's a couple of posts

Post 104506 (missing)

(lost in the sauce: "Re: HgI2", Chemistry Discourse)

Post 106043 (missing)

(hellman: "Re: HgI2", Chemistry Discourse)


noj

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #10 on: February 01, 2002, 06:42:00 PM »
Seems like a waste of I2 if you ask me. HgCl2 is pretty cheap to buy. But if you have the elemental Hg I guess this would be nice.

Real men cook naked.

Vibrating_Lights

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #11 on: February 01, 2002, 06:46:00 PM »
use 1 rectal thermometer per 1 oz bopttle of 2%iodine.  exess won't hurt.
VL_

isohuman

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #12 on: February 03, 2002, 01:46:00 PM »
I found it

Post 248601

(unnilhexium: "Re: When substituting GAA for Formic acid...", Chemistry Discourse)


However, it doesn't give too much detail either.
LT/: it's [xxxxxxx] which translates to

Post 248601

(unnilhexium: "Re: When substituting GAA for Formic acid...", Chemistry Discourse)

PoohBear4Ever

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #13 on: February 03, 2002, 08:22:00 PM »
Heh, LT, that took me a second to process...

Time for some sleep, ::)

PB

SuperStar

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #14 on: February 06, 2002, 04:02:00 PM »
I have a few questions. 
One rectal thermometer into 30ml 2% then use 2 of these bottles for 25g Al?  What is the exact ratio of tincture to Al?

If the tincture does not convert all the Hg to salt (excess Hg) what are the dangers of the vapors during reflux?

I am a little slow so details help.

noj

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #15 on: February 06, 2002, 04:16:00 PM »
wow, that would be way too much mercury. You only need 100mg of Hg salt, at most 200mg, for 27g foil.

there must be an answer for everything, if only you knew how to set forth the questions

SuperStar

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #16 on: February 06, 2002, 05:07:00 PM »
Like I said, I'm a little slow  :P .

So how much tincture? (ml?)  I assume approx 250mg Hg per bottle. So is the Hg converted equally to salt?  250mg Hg in equals 250mg HgI2 per bottle, would this be correct?

I guess my big question is how to convert the ml of tincture (using 1 thermom per 30ml) to grams of Hg Salt?

PoohBear4Ever

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #17 on: February 06, 2002, 05:12:00 PM »

So is the Hg converted equally to salt?  250mg Hg in equals 250mg HgI2 per bottle, would this be correct?




No, but from what I've read, using about 0.5g blob of Hg in one bottle is good for ~ 30g Al...

PB

edit:  Hg= 200.59/mol = A;  I= 126.90/mol = B;  HgI2 = A+2B...


cheeseboy

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #18 on: February 06, 2002, 05:16:00 PM »
Come on SuperStar, live up to your name. ;)

May The Source Bee With You....Always.

  - OB1KNoBee

SuperStar

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #19 on: February 06, 2002, 05:30:00 PM »
Work with me, I am trying to get with the program.  Just so you know that was my first post.

So let me sum up.  We are assuming approx .5g Hg per thermometer added to 30ml 2% tincture. Add 30ml of this tincture for ~ 30g Al.  Sounds easy enough.  Oh yea, Shake tincture well and let stand for about a week.

PoohBear4Ever

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #20 on: February 06, 2002, 05:44:00 PM »
Yep, that should work...

PB

BTW, here's what unnilhexium told me: "All aminations were of the al/hg variety, using methanol as a solvent (isopropanol was never used successfully), with ~.5 gram blobs of hg dropped into I2 tincture, allowed to react for a few days, and then used to amalgamate.

Swim recorded an actual amalgamtion time, it took 17 minutes(.5g mercury blob, 30g Al). The basic procedure is to put a plastic dish on the old balance, zero it, and poke at a mercury blob until about .3-.5 grams is weighed out, then dump it into some 2% I2 tincture, the kind you buy at walmart.  I can't verify that HgI2 is formed, but I have successfully amalgamated using this procedure."

Pray for him ya'll, he may just need it  :( !

SuperStar

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #21 on: February 06, 2002, 07:11:00 PM »
Can anyone tell SWIM a good method for breaking one of these thermometers to keep everything contained and not breath too much vapor.  SWIM was thinking maybe in a tall thick glass with rag on top.  Thermom is about 4 - 5 inch long fairly small.

noj

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #22 on: February 06, 2002, 07:17:00 PM »
That's still 500mg of mercury. .5g is 500mg. I would think 1/4 to 1/3 bottle would work, but never done it so can't say from experience.

there must be an answer for everything, if only you knew how to set forth the questions

noj

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #23 on: February 06, 2002, 07:20:00 PM »
swim uses a pair of side dykes (linesman type pliers) and cuts at the base of the silver to glass interphase. Do this over a dish, use tweezers to get the glass shards out. There is no vapor, it is a liquid metal.

there must be an answer for everything, if only you knew how to set forth the questions

SuperStar

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #24 on: February 06, 2002, 07:33:00 PM »
Yea that is 500mg Hg, but actually more like 1130mg of HgI2 if you take into consideration the 2 Iodine atoms right?  If you use figure above you would have HgI2 = 454g/mol.

Is everyone just assuming that extra doesn't really matter?

SWIM is so new it hurts.  Trying to dot i's and cross those t's.

SWIM may be making too much out of this but might as well clear it up here.

noj

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #25 on: February 06, 2002, 08:08:00 PM »
The idea is to use as little Hg as possible. It doesn't go away when the reaction is finished, and it doesn't go very far when you flush it down the drain. And acquisition isn't getting any easier either.

there must be an answer for everything, if only you knew how to set forth the questions

SuperStar

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #26 on: February 06, 2002, 08:17:00 PM »
OH yea, SWIM definetly wants to use as little as possible. That is what I am trying to figure out. I need someone with more experience though. I don't have quite enought knowledge yet to figure this out. Those digital thermoms are definetly becoming the standard.

Can someone verify that 500mg Hg added to 30 ml 2% Iodine = 1130mg HgI2?  If not how much do you have?

SWIM is back to the original question. How many grams of HgI2 do you end up with?

PoohBear4Ever

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #27 on: February 06, 2002, 08:22:00 PM »
Best to use empirical evidence in this case, since there are many variables that exsist for the HgI2 formation. 

PB

backburner70

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #28 on: February 07, 2002, 11:57:00 AM »
Its interesting what you find in the trash these days...

"A very small amount of elemental mercury was added to 2 molar equivalents of iodine crystals in a closed container and gently shaken. A clumpy crimson powder formed over the next hour. Visual inspection indicated that a small portion of unreacted mercury and iodine was trapped in the clumps, so a few drops of methanol were added. All clumps disappeared and the components went into solution. This mix was added to a larger volume of methanol, and the experimenter noticed a very small portion of greenish-yellow solids remained undissolved in the bottom of the flask. This was assumed to be mercurous iodide (versus mercuric). Al foil was added to the flask and amalgamation began in earnest in less than 2 minutes time (probably owing to the large volume of Hg salts present). The experimenter concluded that the HgI2 formed was completely viable."

One would assume that I2 tincture should behave in a similar fashion.

BB 7.0

LaBTop

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #29 on: February 07, 2002, 03:14:00 PM »
Hehhe, Backburner70!
Only thing I would like to add to this thread:
Do you realize that when you dump ANY amount of fluids containing fluidal mercury in your wash table's drain pipe, that that fuckin mercury is so damm heavy, it will stick at the bottom of the first S curve it finds, and that is the one which will over time dry out when you don't use your lab frequently, thus giving the mercury all the time in the world to EVAPORATE into your precious little lab, and then, when you enter after a summer of love, your playground again, it will be taken up in your lungs, AND NEVER LEAVE THEM EVER AGAIN!
There used to be a little thread around here telling the story of a full proof professional researcher, a woman btw, who slowly showed all signs of mercury poisoning and didn't understand them, until too late, she DIED.
Look up how much elementary mercury your precious life system, called body, can afford.
Be prepared to get a shock.

Don't play around with elementary mercury, if you are a total newbee.
Lugh somewhere gave some basic rules for handling mercury and mercury spills, a must read for all those who read this thread. There is a simple way of getting rid of elementary mercury, by turning it into a not very toxic salt, so find that thread! Think of iron. LT/

WISDOMwillWIN

PoohBear4Ever

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #30 on: February 07, 2002, 03:14:00 PM »
What ratio of HgI2:Al was used?  How long was the iodine and mercury allowed to react for?

PB

isohuman

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #31 on: February 07, 2002, 03:59:00 PM »
Holy shit!  ISO-SWIM goes on a synthesizing binge, and comes back to see this thread has doubled in size.  Anyways party people, this is not hard.  For one, you will never know how much of the hg actually converts to the salt, and two, this reaction is not THAT sensitive to the amount of Hg salt used.  ISO-SWIM has had consistent success for anywhere from .2 to .5g blobs of mercury, for a standard size MM nitro/al-hg.  As my stoichiometry skills have calculated, 1 30ml 3% I2 tincture can process .5g of  mercury.  It just happens that it only takes one tincture.  Trust me, a range of .3 to .6g of mercury will work, as long as the tincture is allowed AT LEAST a few days to stand.  ISO-SWIM has already done a half dozen more of these, and this procedure is BULLET-PROOF.  ISO-SWIM has had a 100% success rate.  BTW, please report on your successes, this is a good procedure, so I don't want this thread to sit here for two years before somebee trys it.

PoohBear4Ever

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #32 on: February 07, 2002, 05:09:00 PM »
Hey isohuman, turn on those PMs if you'd like me to reply...

PB

Vibrating_Lights

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #33 on: February 08, 2002, 03:35:00 AM »
buy 1 $ heat thermostat from the hardware store and pt iti in a 1oz bottle of 2% tincture. allow to set for a few days till the black color is gone and dump the liquid into the al solution.  then just add another bottle of fresh i2 to the remaining blob.  continue until the blob is gone.
VL_

backburner70

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #34 on: February 08, 2002, 07:39:00 AM »
LT,

I am aware. I guess the emphasis on my post should be on the phrases:

"A VERY SMALLL amount of mercury," and "a CLOSED container".

But yeah, elemental mercury is not to be messed with. A quick scan of Google or any other search engine will yield a number of horror stories. SWIM generally uses prepared HgCl2, but this thread was interesting.

Now that I think about it, something that is missing from the Hive is a mercury safety FAQ. This would be extremely useful for Newbees since this topic seems to come up on a regular basis. I volunteer to compile it.  Suggestions for starting material are wlecome.

BB 7.0

Rhodium

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #35 on: February 08, 2002, 07:55:00 AM »
Backburner: That is a very good initiative. There has been good threads in the past on mercury handling, disposal and toxicity, so a good starting point would be TFSE.

noj

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #36 on: February 08, 2002, 08:18:00 AM »
Here are some things from the EPA:

Chemical Formula:  HgCl2

Molecular Weight:  271.52

Routes of Entry:  Inhalation:  Yes (Weiss 1980, p. 581)
                      Skin:  Yes (*Gosselin 1976)
                      Ingestion:  Yes (*Browning 1969)

    Health Hazards (Acute, Delayed, and Chronic):  It is classified as
    extremely toxic.  All forms of mercury are poisonous if absorbed.  Probable
    oral lethal dose is 5-50 mg/kg; between 7 drops and 1 teaspoonful for a 150
    lb. person.  Mercuric chloride is one of the most toxic salts of mercury
    (*Gosselin 1976).  Material attacks the gastrointestinal tract and renal
    systems (*Friberg 1979).

Extinguishing Methods:  Some of these materials may burn but none of them
    ignite readily.  Extinguish with water spray, fog, foam, dry chemical or
    carbon dioxide (*DOT 1984).

Unusual Fire and Explosion Hazards:  Material may explode on heating, with
    friction, or contact with alkali metals, sulfides, acetylene, ammonia, and
    oxalic acid (*Rumack 1975 to Present).

Stability:  Unstable:
                Stable:  Yes (Weiss 1980, p. 581)

        Conditions to Avoid:  Mercuric chloride may explode with friction or
        application of heat.  Mixtures of mercuric chloride and sodium or
        potassium are shock sensitive and will explode on impact (*NFPA 1978).
        Avoid contact with acids or acid fumes (*Sax 1975).

    Incompatibility (Materials to Avoid):  Formates, sulfites, hypophosphites,
    phosphates, sulfides, albumin, gelatin, alkalies, alkaloid salts, ammonia,
    lime water, antimony, arsenic, bromides, borax, carbonates, reduced iron,
    copper, iron, lead, silver salts, infusions of cinchona, columbo, oak bark
    or senna, and tannic acid (*Merck 1983).

    Hazardous Decomposition or Byproducts:  Upon decomposition highly toxic
    chloride and mercury fumes are emitted (*Sax 1975).



there must be an answer for everything, if only you knew how to set forth the questions

SuperStar

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #37 on: February 08, 2002, 10:28:00 AM »
SWIM like vibrating's method the best so far.  That makes sense. You only have to get the mecury once. Those thermostat switches contain about 5g Hg. So that should last 10 bottles of tincture. Also know that one bottle of tinture can convert .5g Hg so you know how much salt you are adding.  Plus only have to handle the mercury once.  SWIM is very interested in disposal of mercury and what to do with the post AL/Hg sludge?

lugh

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #38 on: February 08, 2002, 10:51:00 AM »

Post 228769

(lugh: "Re: proper waste disposal", Chemistry Discourse)


PoohBear4Ever

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #39 on: February 08, 2002, 11:36:00 AM »
Also, concerning HgI2, see:

Post 266736

(PoohBear4Ever: "Re: First posted 100% OTC dream (told y'all) - Eze", Methods Discourse)


PB

SuperStar

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #40 on: February 08, 2002, 01:13:00 PM »
Thanks for the links.

SWIM has read many posts about this disposal. No real consensus on what to do.   Using the nitro Al/Hg What to do with the gray sludge after extraction. 

Would adding more Al be enough to neutralize the Hg and then flush or bottle to the landfill?

A lot of post keep talking about Copper or Zinc fillings.

lugh

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #41 on: February 08, 2002, 01:20:00 PM »
Steel machine shop turnings are readily available  :)

SuperStar

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #42 on: February 08, 2002, 01:26:00 PM »
Must remember SWIM is a little slow. Must have details.

So take this sludge, throw in ??grams of steel turnings, mix well, then what?  Throw in a jar and landfill or flush?

lugh

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #43 on: February 08, 2002, 01:35:00 PM »

Must remember SWIM is a little slow. Must have details.



Then SWISS needs to speed up. :)  Many useful details can be found in the thread starting with

Post 103272 (missing)

(ymir: "Mercury Recovery/Disposal", Chemistry Discourse), which is linked to in the post above. There's no need to keep reposting the same information for the sake of those unwilling or unable to search and read  :)


SuperStar

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #44 on: February 08, 2002, 01:59:00 PM »
SWIM has studied and searched fairly well. Don't think real good answer is out there. SWIM sees about 5 different options. Has no idea which ones are right.

OPTIONS:
1. All the Hg is already converted by the Nitro Al/Hg. Place sludge in milk jug and throw away.

2. Seperate the Al particles and place in jug, flush the liquid

3. Place more Al in the sludge, let stand for 5 - 8 hours, seperate, solid in jug, liquid gets a flush.

4. Mix suflur Powder in the sludge and flush.

5. Mix Iron/Steel turnings in the sludge and bottle and toss.

A lot of methods keep talking about recovery of the Hg but don't think that is goind to happen here.

Also confused that if Al will react all Hg then seems way to easy to just add more Al to make sure and throw away. But if that were true why are there so many posts on these other methods.

SWIM is trying and know that other newbees must be having the same questions.

Still don't know what option above is best and whether to flush or jug it and toss?

Pardon my friend officer, He's a little slow.

lugh

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #45 on: February 08, 2002, 04:28:00 PM »
Disposing of mercury wastes into the water shed is not only bad for the environment, but totally unnecessary. Your basified sludge contains elemental mercury, which will amalgamate to metals such as iron, zinc or copper. You take a 20 L/5 gal bucket with a tight fitting lid, throw some clean metal turnings in the bottom, and then your pH 13-14 sludge. Attach the lid firmly. Over a period of time, the mercury is amalgamated, siphon the sludge for disposal down the drain. Keep the lid on the bucket for future use. If you're determined to dispose of the mercury instead of recycling it using nitric acid, you will need to solidify the turnings within plastic, thus isolating the mercury from the watershed. This would be most easily done by slowly portionwise (so as to avoid melting the bucket) pouring molten plastic into the bucket until the metal turnings are completely encapsulated  :)

SuperStar

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #46 on: February 08, 2002, 05:16:00 PM »
Thanks for the post lugh.  Now that SWIM reads what you posted the other posts make a little more sense. 

Said earlier that SWIM was not interested in recovery of the mecury using Nitric Acid. Now changed mind.  Searched all up and down TFSE and didn't find anything clear enough for someone like SWIM.  If SWIM were to try and recover the Mercury (Hg) from the post Amalgam sludge where would a good step by step bee?  See lots about distilling mercury, SWIM has no idea what distilling elemental mercury would be, sounds like a damn mess.

Pardon my friend officer, He's a little slow.

lugh

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #47 on: February 08, 2002, 06:54:00 PM »
You probably won't want to bother with recovery until you've got more than a couple of grams amalgamated. You will want to keep the lid on tight to prevent the escape of mercury vapor. While SWIL has never done the recovery, obviously because of the volume of turnings compared to the amount of mercury, one would want to use very dilute nitric acid, and then evaporate the solution to obtain the mercuric nitrate.

Vibrating_Lights

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #48 on: February 08, 2002, 09:04:00 PM »
whenever you decide to change carrears.  take all the mercury encapsulated in the plastic and deliver it to a DEA facility.  They will spend a few thousand dollars and much time trying to figure out what it is.  those fuckers spend so  much money tryin to figure out shit,  make more work for em.  Mix some other fun shit in it too so they need suits to discect it.
VL_

Vibrating_Lights

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #49 on: February 08, 2002, 09:36:00 PM »
Since swim has not drempt this yet.  will the HgI be dissolved already in the alcohol. if so could the bottle just be poured into the al/MeOH mix. Question here is soloubility of the HgI in the IPA that the tincture comes with.
VL_

isohuman

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #50 on: February 09, 2002, 11:45:00 AM »
The Hg2I2 dissolves itself in the alcohol present in the tincture.  Then, you can just pour the tincture into the aluminum/methanol mix, and stir on high for one minute to thoroughly mix.  That's how ISO has been doing it, very even and fast amalgamation that way.  ISO rinses the tincture bottle with MeOH, to be sure to get all of the Hg, and to make the bottle safe to throw away.  Has anybee out there tried this yet?  Please post results to this thread, so this method can be validated.  Otherwise, ISO will be forced to nudge this thread back to the top every week with a little B.S. post until someone else trys this too :)
Trust me, the reaction proceeds exactly the same as with HgCl2, you will not be disappointed.

LaBTop

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #51 on: February 09, 2002, 01:14:00 PM »
No need to hurry/worry, it is known and said numerous times, especially by Osmium, that any Hg salt will do a fine amalgamation job on f.e. Alu foil or thicker alu sheets.
So, we TRUST you on this one! LT/ ;)

WISDOMwillWIN

SuperStar

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #52 on: February 09, 2002, 01:48:00 PM »
Hate to keep posting but believe that V_L has the right idea about the tinture. Just add 5g Hg to one bottle. Then pour about all liquid and leave what should be 4.5g Hg blob in the bottle.  Add more tinture, repeat, parsley, serves two.

This to me make sense to SWIM for a couple reasons. 1. Don't have to fuck around measuring how much Hg was put in the bottle, (vapors, scales, and shit).  2. Basically should only have to touch mercury once per 10 bottles.

Pardon my friend officer, He's a little slow.

isohuman

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #53 on: February 09, 2002, 05:38:00 PM »
Superstar:  It might be harder than you think to pour off the tincture without dumping the blob as well.  It's easy just to zero a plastic container on a balance, and have another container with the mercury.  Just tip the container poke the Hg with a glass stir rod until you pull a .3-.5g blob into the container on the balance.  Dump it in the tincture, replace the lid and shake the fuck out of it to break up the blob, which increases the surface area of the Hg. ISO doesn't think mercury vapor is TOO much of a risk, mercury having a high B.P., and probably creates very little
vapor at room temp. and atmospheric pressure, but ISO doesn't know that for a fact, so someone flame the fuck out of me if I'm wrong.

Vibrating_Lights

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Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #54 on: February 09, 2002, 07:11:00 PM »

Seperations can be done in a measuring cup careful decantation is an art.
VL

demorol

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #55 on: February 10, 2002, 06:10:00 AM »
I don't  agree with you LaBTop. You said that any Hg salt works just fine, but when I asked about HgSO4, some bees said it won't work. So use HgCl2, since it's cheap and easy to get.

Life without chemistry would be a mistake.

demorol

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #56 on: February 10, 2002, 06:30:00 AM »
Mercury spills can be easily neutralised with Chemizorb® Hg absorbant. This kit is supplied by Merck and can be used to neutralise the contaminated area up to 1 m2. But probably you won't be able to get it, so here is an OTC version of such an absorbant:

Cleaning up Mercury spills:
First collect the drops with a pipet, put them in a bottle and seal it. Those droplets that can't be collected are covered with a paste, that consists of copper powder and diluted H2SO4. Instead of this paste you can use a suspension of Ca(OH)2 and powdered sulfur in hot water. The paste (suspension) is removed after 24 hours and disposed off properly.

Life without chemistry would be a mistake.

lugh

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #57 on: February 10, 2002, 12:14:00 PM »

Those droplets that can't be collected




Amounts too small for a pipet can also be recycled by using transparent cellulose acetate tape to pick it up, and then acetone to remove the mercury from the tape  :)


Vibrating_Lights

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #58 on: February 10, 2002, 01:37:00 PM »
After you clean the spill with the chemizorb.  Used the amalgamated chemizorb to reduce a nitrostyrene.
VL_

greeter

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #59 on: February 11, 2002, 09:58:00 PM »
> This mix was added to a larger volume of methanol, and the experimenter noticed a very small portion of greenish-yellow solids remained undissolved in the bottom of the flask.

Please clarify for me here:  Does Hg (or I2 for that matter) dissolve in MeOH?  Swim has some I2 crystals he would like to react with some elemental Hg to form HgI2.  Is MeOH a good medium to perform the reaction in?

SuperStar

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #60 on: February 12, 2002, 11:55:00 AM »
The tincture bottles come in alcohol. Don't know about MeOH though.

Pardon my friend officer, He's a little slow.

PoohBear4Ever

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Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #61 on: February 12, 2002, 12:22:00 PM »
Tincture = "dissolved in alcohol"

PB

Cept

  • Guest
MM/Nitro HgI2. Foil/HgI2 Calculations
« Reply #62 on: February 17, 2002, 06:16:00 PM »
How much aluminum foil and HgI2 is required to run a hundred gram batch of p2p? I'm assuming the reaction requires 83.3g foil (1200ml MeOH). Will it then require 1g HgI2? So in theory, a single 2% 30ml tincture bottle(.6g+.474g=1.074) should suffice.
   How off would one have to be on the salt/foil/p2p to fuck it up? maybe leaving unreduced shit? if there wasn't enough HgI2 wouldn't it just take longer? or would it never reach completion?
    It seems like there isn't a formula or math involved, people just try different amounts and use them? I'd like the calcs. If anyone can hit me off with the math required for the calculation of the foil/salt amalgamation i'd be in your debt.

Cluster_Fucked

  • Guest
Re: MM/Nitro HgI2. Foil/HgI2 Calculations
« Reply #63 on: February 17, 2002, 11:26:00 PM »
Just guessing, SWIC would say that at least 3 bottles of tincture would be needed, each with 0.5g Hg added prior.

Striving for normality!

SuperStar

  • Guest
Re: MM/Nitro HgI2. Foil/HgI2 Calculations
« Reply #64 on: February 21, 2002, 04:48:00 PM »
This is also my opinion. But I am under the understanding that each 30ml 2% bottle tincture with .5 Hg in should create about 1100mg of HgI2.  Using that rational seems as if 1/2 bottle or about 15ml for a MM size reaction would be fine. I have not tried yet so keep that in mind.

Pardon my friend officer, He's a little slow.

riobard

  • Guest
Re: MM Nitro/Al-Hg variation: No HgCl2
« Reply #65 on: February 22, 2002, 08:00:00 AM »
-demorol,

Any SOLUBLE mercury salt will do, quoting osmium and possibly labtop. Sulfate salts are insoluble. Nitrate, Halide, and others will definitely work. COnsult a general chemistry textbook, merck, etc. for sulubility guidelines of salts in aqueous solutions.

Soluble dosen't mean very soluble, either. As long as some dissolves, amalgamation goes, equilibrium shifts, amalgamation goes, yada yada yada. Transition metal salts are not very soluble. You're supposed to have at least a minimal amount of water in the al/hg depending on what variation you use. I know alcohol is present, factoring in, along with all of the other shit. Plainly, water is there. so is the water soluble mercury salt. It works.

Hope my tone isn't dry or antagonistic. I wasn't trying to be an asshole about it, just plain and simple. Good luck with any work that swid might be out to do