kurtak
Well-known member
Ok I have done my test run on Jerrys process (from here on referred to as the M44 process or just M44) along with comparative testing of 3 other process (all run at the same time)
I was actually done on Wednesday but needed time to compile it into a format to present to the forum (as suggested by Lou) & as well wanted Jerry to run the process for the purpose of doing a full discloser video --- he needed to get some material together & then had some weather delays --- also I wanted run the process one more time in & of its self & I also encountered some weather delay
I was not really able to take notes because of having 4 processes going at once & as well I had Jerry on the phone for the full run so he could walk me though it - with Jerry on the phone I also could not take pictures while running the processes - however I got a pic of the starting set up as well as pics after
Before Jerry decided on the name M44 he had referred to it as "his version of reverse AR" --- though it is not really a version of reverse AR - it does have somethings in common with it - first & foremost of which is that it works with having both chlorides & nitrates in solution at the same time --- the difference being that instead of dissolving the gold but not the base metal - you want to dissolve the base metal but not the gold --- so - like reverse AR it is "important" that a balance be maintained between the nitrates & chlorides - if you flop (up set) the balance you will have a mess - meaning just like reverse AR if the balance is up set you will dissolve both gold & base metal
The Claim
The claim is that the M44 process is near to as fast (meaning with a narrow plus/minus factor) as nitric for dissolving base metals in order to recover the foils from gold plated material for refining - with copper/brass pins being the most discussed - So I was originally going to run the test with just the M44 process & nitric --- however then it was brought up that "hot" ferric Chloride (alone) could be used &/or ferric chloride with an oxidizer to do the job near as fast as nitric --- so I decided to include each of those in my testing
Note; - I have never used anything other then nitric for my foil recovery of copper/brass pins simply because I get my nitric cheap & in bulk - that includes that I have never run the AP/CuCl2 process
Therefore the claim is that if you want to recover your foils with the speed of nitric - but ether can't get nitric &/or have to pay a outrageous high price for nitric - then the M44 process is an alternative to nitric
Objective
So my objective in my testing was to run each (all 4) of these methods "at the same time" as a comparative test of each process to the speed of nitric to see if it (they) actually meet/met the above claim(s)
Setting Up & Equipment
I set up outside as the project was larger then I could run in my lab/fume hood (see pic)
Nitric process; - I used a stainless steel 2 gallon pot (left side of work table in the pic) & single burner hot pate - this got moved over to its own table (before actually starting) so I didn't have Nox fumes at the table I was working the M44 process on
Hot ferric chloride & ferric chloride with oxidizer; - two 4 liter beakers (1 for each process) & a griddle type hot pate (to hold both beakers)
M44 process; - 1 gallon Vision glassware pot & single burner hot plate, 4 liter beaker (used to prep ferric chloride)
Other equipment; - scale, smaller beakers for measuring chem, 3ml pipets, large plastic spoons (like used for cooking) 1/2 teaspoon measuring spoon, 2 liter vacuum flask & filter funnel, 3 plastic colanders & 3 plastic buckets (for filtering)
Chemicals
68% nitric, D-water, ferric chloride, sodium nitrate (this is 16% [or 16-0-0] Hi Yield brand nitrate fertilizer) HCl, 3% H2O2
Material
The only material I had on hand was 4 lbs of a mix of low grade & very low grade pins that had been incinerated (to relieve them from there plastic housing) & leftover from being used as my collector metal for smelting - so weighed out four 1 lb batches
Note; - its to bad the discussion of the M44 process didn't come up a couple weeks earlier because I had just processed about 10 lbs of high grade pins from which I got a nice 31.4 gram bar --- it would have been nice to have had those pins for this project
Running The Test
The first thing Jerry wanted me to do was concentrate/saturate/load the ferric with more iron for the M44 process - so the night before I put 1 liter of ferric in a 4 liter beaker tossed in some iron laminates from a transformer casing turned the heat on & actually boiled it - this took about 1&1/2 hour - turned the heat off & let set over night (this was done in my fume hood)
Next morning the ferric (brown) had turned to ferrous (green) with green ferrous crystals in the bottom & about an inch of heavy kind of gooey foam on top - so I called to tell him what I had - he said not to worry - just turn the heat on to about medium heat & when the crystals start to get soft & mushy turn the heat up on high & let it boil for a while & the crystals & foam will dissolve back into solution & it will go back to brown (this was done in my fume hood)
So while I was waiting on that I went around & double checked that I had everything in place for the rest of the testing - when the crystals in the ferrous chloride got to a point of being mushy I went out & put 1&1/2 liter (1500 ml) of ferric chloride in each of the 4 liter beakers on the griddle hot plate for the hot ferric test & the ferric w/oxidizer test & turned the heat on medium/high to pre heat this ferric (the SS nitric pot had its 1 lb metal & 2 liters D-water waiting to add the nitric)
When the ferric/ferrous (for the M44 process) had re-dissolved the crystals & foam & gone back to brown (remember - this was boiling) I turned it off - called Jerry - went out & turned the ferric testing griddle up on high - went back in to the lab & brought the ferric/ferrous (1 liter) out - poured it in the Vision glassware pot & turned on its hot plate
Note; - my phone is now turned on to speaker phone mode & setting on the table so Jerry can walk me through the M44 process
I then went over to the nitric pot & poured in 1 liter 68% nitric - went to the ferric griddle & put 1 lb metal in each beaker & then went to the M44 pot & added its 1 lb metal - then added six 1/2 tea spoons of the 16% sodium nitrate - I then added about 10 ml 3% H2O2 to the ferric w/oxidizer beaker
When the sodium nitrate started to react in the M44 process - about a minute or 2 (the reaction is like the fizzing you get when you "slowly" pour a coke into a glass - so "small" fizzing bubbles) I added 15 ml HCL - this changed the reaction a bit - the bubbles got a bit larger & it started to roll a bit - I added another 15 ml HCl & the reaction started to roll a bit more (Jerry is on the phone asking me what I see & telling me what to do)
Note; - I should add that I have all my metal pulled to one side of the pot & I am making my chem additions to the other side of the pot & the above reactions are taking place on the side of the chem additions
So I added another 15 ml HCl - this started the reaction to start to work more on the edge of the metal near the center of the pot - I added another 15 ml HCl - this started the reaction working even more on the metal side which also started a flow back across the top to the nonmetal side
When this reaction started to die down I added another 30 ml HCl - this really kicked off the reaction working on the metal side with the flow to the nonmetal side
So I went over to the nitric pot & added another 500 ml nitric
Note; - not much going on in the ferric beakers so I add another 15 ml H2O2 to that beaker
The M44 reaction was slowing down so I added another 30 ml HCl - this time the HCl addition did not kick start the reaction again (it did a bit - but not like it should) this is the indicator that you are about to flop (up set) the chem balance (which you don't want to do or it will start to dissolve gold) so "right away" I added another 6 spoons (1/2 tea spoons) of sodium nitrate which got the reaction going again - when that started to die I added another 40 ml HCl - then went & put the last 500 ml nitric in the nitric test (now 2 liters total & this is not on the hot plate yet as its not needed at this point)
The ferric griddle beakers are still not doing much (remember I did start these with the ferric preheated & hot) so I added another 30 ml H2O2 to that beaker
The M44 reaction was slowing again so I added another 40 ml HCl & each time the reaction would start to slow I would add another 40 ml HCl - so like another 2 or 3 HCl addition --- like before when the HCl addition didn't kick the reaction off I "right away" added more sodium nitrate
Checking on the nitric test regularly between chem addition at the M44 pot at about 1 hour into the test the nitric reaction still had a vigorous reaction going but was no longer foaming heavy so I put the pot on the hot plate & turned it on high
Still not much happening at the ferric griddle (some reaction but not much) so I added more H2O2 to that beaker - this time just poured from the bottle - I would say another 50 - 60 ml
About 15 - 20 minutes after turning on nitric test hot plate on - I was working the M44 process (following chem additions as described above) when a HCl addition didn't kick off a dying reaction so added more sodium nitrate thinking I had reached that point of flopping the chem balance again - still no kick start of the reaction - hmmm - what the heck - ohhh dam the hot plate is not working - did it come unplugged - no - hmmm - well dam the griddle & nitric hot plate are not working ether - did I kick & unplug main extension cord - no - did I trip circuit breaker - no none tripped - ahhh that outlet must go to fuss box in lower part of barn not to breaker box in upper barn - ok plug into outlet I know is wired 20 amp circuit breaker circuit --- ok - good to go - wait a bit for all to come back up to temp & reactions to start again
I was actually done on Wednesday but needed time to compile it into a format to present to the forum (as suggested by Lou) & as well wanted Jerry to run the process for the purpose of doing a full discloser video --- he needed to get some material together & then had some weather delays --- also I wanted run the process one more time in & of its self & I also encountered some weather delay
I was not really able to take notes because of having 4 processes going at once & as well I had Jerry on the phone for the full run so he could walk me though it - with Jerry on the phone I also could not take pictures while running the processes - however I got a pic of the starting set up as well as pics after
Before Jerry decided on the name M44 he had referred to it as "his version of reverse AR" --- though it is not really a version of reverse AR - it does have somethings in common with it - first & foremost of which is that it works with having both chlorides & nitrates in solution at the same time --- the difference being that instead of dissolving the gold but not the base metal - you want to dissolve the base metal but not the gold --- so - like reverse AR it is "important" that a balance be maintained between the nitrates & chlorides - if you flop (up set) the balance you will have a mess - meaning just like reverse AR if the balance is up set you will dissolve both gold & base metal
The Claim
The claim is that the M44 process is near to as fast (meaning with a narrow plus/minus factor) as nitric for dissolving base metals in order to recover the foils from gold plated material for refining - with copper/brass pins being the most discussed - So I was originally going to run the test with just the M44 process & nitric --- however then it was brought up that "hot" ferric Chloride (alone) could be used &/or ferric chloride with an oxidizer to do the job near as fast as nitric --- so I decided to include each of those in my testing
Note; - I have never used anything other then nitric for my foil recovery of copper/brass pins simply because I get my nitric cheap & in bulk - that includes that I have never run the AP/CuCl2 process
Therefore the claim is that if you want to recover your foils with the speed of nitric - but ether can't get nitric &/or have to pay a outrageous high price for nitric - then the M44 process is an alternative to nitric
Objective
So my objective in my testing was to run each (all 4) of these methods "at the same time" as a comparative test of each process to the speed of nitric to see if it (they) actually meet/met the above claim(s)
Setting Up & Equipment
I set up outside as the project was larger then I could run in my lab/fume hood (see pic)
Nitric process; - I used a stainless steel 2 gallon pot (left side of work table in the pic) & single burner hot pate - this got moved over to its own table (before actually starting) so I didn't have Nox fumes at the table I was working the M44 process on
Hot ferric chloride & ferric chloride with oxidizer; - two 4 liter beakers (1 for each process) & a griddle type hot pate (to hold both beakers)
M44 process; - 1 gallon Vision glassware pot & single burner hot plate, 4 liter beaker (used to prep ferric chloride)
Other equipment; - scale, smaller beakers for measuring chem, 3ml pipets, large plastic spoons (like used for cooking) 1/2 teaspoon measuring spoon, 2 liter vacuum flask & filter funnel, 3 plastic colanders & 3 plastic buckets (for filtering)
Chemicals
68% nitric, D-water, ferric chloride, sodium nitrate (this is 16% [or 16-0-0] Hi Yield brand nitrate fertilizer) HCl, 3% H2O2
Material
The only material I had on hand was 4 lbs of a mix of low grade & very low grade pins that had been incinerated (to relieve them from there plastic housing) & leftover from being used as my collector metal for smelting - so weighed out four 1 lb batches
Note; - its to bad the discussion of the M44 process didn't come up a couple weeks earlier because I had just processed about 10 lbs of high grade pins from which I got a nice 31.4 gram bar --- it would have been nice to have had those pins for this project
Running The Test
The first thing Jerry wanted me to do was concentrate/saturate/load the ferric with more iron for the M44 process - so the night before I put 1 liter of ferric in a 4 liter beaker tossed in some iron laminates from a transformer casing turned the heat on & actually boiled it - this took about 1&1/2 hour - turned the heat off & let set over night (this was done in my fume hood)
Next morning the ferric (brown) had turned to ferrous (green) with green ferrous crystals in the bottom & about an inch of heavy kind of gooey foam on top - so I called to tell him what I had - he said not to worry - just turn the heat on to about medium heat & when the crystals start to get soft & mushy turn the heat up on high & let it boil for a while & the crystals & foam will dissolve back into solution & it will go back to brown (this was done in my fume hood)
So while I was waiting on that I went around & double checked that I had everything in place for the rest of the testing - when the crystals in the ferrous chloride got to a point of being mushy I went out & put 1&1/2 liter (1500 ml) of ferric chloride in each of the 4 liter beakers on the griddle hot plate for the hot ferric test & the ferric w/oxidizer test & turned the heat on medium/high to pre heat this ferric (the SS nitric pot had its 1 lb metal & 2 liters D-water waiting to add the nitric)
When the ferric/ferrous (for the M44 process) had re-dissolved the crystals & foam & gone back to brown (remember - this was boiling) I turned it off - called Jerry - went out & turned the ferric testing griddle up on high - went back in to the lab & brought the ferric/ferrous (1 liter) out - poured it in the Vision glassware pot & turned on its hot plate
Note; - my phone is now turned on to speaker phone mode & setting on the table so Jerry can walk me through the M44 process
I then went over to the nitric pot & poured in 1 liter 68% nitric - went to the ferric griddle & put 1 lb metal in each beaker & then went to the M44 pot & added its 1 lb metal - then added six 1/2 tea spoons of the 16% sodium nitrate - I then added about 10 ml 3% H2O2 to the ferric w/oxidizer beaker
When the sodium nitrate started to react in the M44 process - about a minute or 2 (the reaction is like the fizzing you get when you "slowly" pour a coke into a glass - so "small" fizzing bubbles) I added 15 ml HCL - this changed the reaction a bit - the bubbles got a bit larger & it started to roll a bit - I added another 15 ml HCl & the reaction started to roll a bit more (Jerry is on the phone asking me what I see & telling me what to do)
Note; - I should add that I have all my metal pulled to one side of the pot & I am making my chem additions to the other side of the pot & the above reactions are taking place on the side of the chem additions
So I added another 15 ml HCl - this started the reaction to start to work more on the edge of the metal near the center of the pot - I added another 15 ml HCl - this started the reaction working even more on the metal side which also started a flow back across the top to the nonmetal side
When this reaction started to die down I added another 30 ml HCl - this really kicked off the reaction working on the metal side with the flow to the nonmetal side
So I went over to the nitric pot & added another 500 ml nitric
Note; - not much going on in the ferric beakers so I add another 15 ml H2O2 to that beaker
The M44 reaction was slowing down so I added another 30 ml HCl - this time the HCl addition did not kick start the reaction again (it did a bit - but not like it should) this is the indicator that you are about to flop (up set) the chem balance (which you don't want to do or it will start to dissolve gold) so "right away" I added another 6 spoons (1/2 tea spoons) of sodium nitrate which got the reaction going again - when that started to die I added another 40 ml HCl - then went & put the last 500 ml nitric in the nitric test (now 2 liters total & this is not on the hot plate yet as its not needed at this point)
The ferric griddle beakers are still not doing much (remember I did start these with the ferric preheated & hot) so I added another 30 ml H2O2 to that beaker
The M44 reaction was slowing again so I added another 40 ml HCl & each time the reaction would start to slow I would add another 40 ml HCl - so like another 2 or 3 HCl addition --- like before when the HCl addition didn't kick the reaction off I "right away" added more sodium nitrate
Checking on the nitric test regularly between chem addition at the M44 pot at about 1 hour into the test the nitric reaction still had a vigorous reaction going but was no longer foaming heavy so I put the pot on the hot plate & turned it on high
Still not much happening at the ferric griddle (some reaction but not much) so I added more H2O2 to that beaker - this time just poured from the bottle - I would say another 50 - 60 ml
About 15 - 20 minutes after turning on nitric test hot plate on - I was working the M44 process (following chem additions as described above) when a HCl addition didn't kick off a dying reaction so added more sodium nitrate thinking I had reached that point of flopping the chem balance again - still no kick start of the reaction - hmmm - what the heck - ohhh dam the hot plate is not working - did it come unplugged - no - hmmm - well dam the griddle & nitric hot plate are not working ether - did I kick & unplug main extension cord - no - did I trip circuit breaker - no none tripped - ahhh that outlet must go to fuss box in lower part of barn not to breaker box in upper barn - ok plug into outlet I know is wired 20 amp circuit breaker circuit --- ok - good to go - wait a bit for all to come back up to temp & reactions to start again