Amalgamation taking too long, due to <0c temps?

[Gale]

I learned the al/hg using Reynolds and normally used to starting reactions around 30mins-1hour after adding mercuric chloride, now I stepped up to sheet metal and now some new alternative 99.99% aluminum nails, had some succcess with the sheets but it takes forever to get going in the cold, I wasn't sure if this played a major roll so I just want to ask what you all think.

Methanol + Aluminum + mercuric chloride in excess amounts, took nearly 3 hours to start becoming noticeably dull and methanol not bubbling. Should I warm the methanol to room-temp at-least? is methanol and mercuric chloride alone a good choice to get things started? or would adding another solvent help?
al/hg without nitro

 

[UWe9o12jkied91d]

Solid pieces of aluminium are crap for this.I tried sheets, granules, discs, nothing has ever worked better than some thick ass foil.
1H to amalgamate is crazy even at 0c.Are you working outside btw? In any case heat that sucker up to about room temp.With ground foil amalgamation is done in 5-10 minutes @23C.
Just water always worked great, what is the role of methanol if you are just going to drain and wash it anyways?

 

[Gale]

Is thick foil OK for like >2kg reactions. Work outside yes but moved indoors

 

[Gale]

And thick foil is basically really thin sheet and I have scaled up to .012" thickness and it has done me well for 1kg but now the temps outside have been dropping especially at the lab I've been getting varied results for amalgamation.

found thi,

 

[UWe9o12jkied91d]

Damn, what kind of yield are you getting from1kg scale?

 

[Gale]

It was good yield, I was scaling up quickly and encountered a few problems but I had a really nice reaction 1.1kg got back around 950g... That was dumping everything in wholesale. All the sheet was consumed, barelt any left and the reaction had a nice grey/blue color. I'm learning to tweak things but I think I will switch to borohydride very soon, pumped. Seems more forgiving/easier for larger reactions

 

[Gale]

I like to do smaller reductions like 650g at a time using this method I find it easier to get consistent results. I think its find for 1+kg but I haven't really made the proper adjustments to my methods.

I'm trying the boro reduction now, will let u know what I think of it vs al/hg

 

[UWe9o12jkied91d]

Oh borohydride you can scale up a lot for sure, I've seen 750-1500kg scale, not illicit ofcourse.
But it's interesting to know you managed to scale up this big, i was thinking it can be scaled up over 100g.Were you left with a lot of aluminium?How much salts ?And thickness of sheet?