Ammonia Soluble Hexachloropalladates (IV)

[kadriver]

I poured the mixture into a 250ml gas bubbler using straight HCl to rinse the black powder out of the beaker and into the bubbler.

 

[kadriver]

And now to assemble the chlorine gas generator.

The small bottle on the right contains a crushed up tablet (they are about 3 inches in diameter) from the large container on the left.

I put the large tablet inside of a large heavy plastic freezer bag by Glad.

Then I put that inside of another Heavy glad freezer bag and gently as possible so as not to put a hole thru the bag, set it on the concrete floor and carefully crushed it into a powder with light blows with a hammer.

It worked perfectly.

 

[kadriver]

Here is a close-up of the label for the chlorine tablets. I got them at Lowes in the swimming pool section.

The label says "trichloroisocyanuric acid".

 

[kadriver]

I fashioned a paper funnel out of a sheet of paper and some masking tape and poured the entire contents, one crushed up 3 inch tablet, into the gas generator reaction flask with side arm output.

Please notice that I am doing this in a fume hood. Don't try this inside an enclosed space or room as deadly chlorine gas is going to be generated and once the reaction starts it really can't be stopped.

 

[kadriver]

I added a little distilled water to make a slurry out of the trichloroisocyanuric acid.

This greatly increases the efficiency of gas production.

Using the powder dry don't work so good because I tried it the first time I did this.

The gas flow was erratic and difficult to control.

With a slurry mixture the flow of gas can be regulated much better.

 

[kadriver]

Next I fitted the flask with a 250ml equalizing funnel and charged it with about 200ml of concentrated hydrochloric acid.

 

[kadriver]

Here is a shot of the entire assembly ready to start chlorine gas production.

 

[kadriver]

This is the chlorine gas generator apparatus completely set up and ready to run.

Again, please notice that this is inside a fume hood. This gas is very dangerous and this can't be done inside a house or other enclosed space.

Once I open the stop cock on the funnel, deadly chlorine gas will be produced and the reaction can't be stopped.

My emergency plan in case of a power failure is to turn off the flow of acid and then carefully tote both stands out the back door and place it in the middle of my back yard.

I have discovered that a regular 3M respirator will provide a little protection to enable me to transported the apparatus outdoors.

A respirator is not recommended because it will not filter the gas, but it is better than no protection at all.

I got a whiff of this gas once by getting too close to a leaching bin and it almost brought me to my knees.

 

[kadriver]

I started the drip at about one drop per second and the gas began to flow immediately.

I must say that this was one of the more pleasurably experiments that I have done in a long time.

I could increase the flow or decrease the flow of gas by adjusting the drop rate from the equalizing funnel.

That is concentrated HCl and the mixed PGM blacks inside the gas bubbler, about 100ml of HCl.

It started to get darker as soon as the gas started to bubble thru it, indicating that the powder was being dissolved by the gas flow

 

[kadriver]

At no tine did I smell even a hint of chlorine gas during this whole experiment.

Notice the color inside the generating flask, it looks menacing!

 

[kadriver]

After about 10 minutes the liquid began to turn red looking, the photo is not the same as if viewed in person.

It looked like red wine.

 

[kadriver]

After about 1/2 hour I could no longer see through the solution inside the bubbler.

I held a bright flashlight behind the bubble and then I could see through the solution.

Notice that most of the powder is gone in this shot.

Only a small amount of the black powder remains in the bottom.

It can be seen in the front and to the left a little inside the bubbler while illuminated with the flashlight.

 

[kadriver]

Finally the solution became thick and looked blood red, no amount of light would pass through the solution.

It took about 1.5 hours to get to this point.

I did add another 200ml charge of HCl part way through this process because the first 200 ml had been used up.

At this point the TCA was expended and the gas slowed down no matter how much HCl I added.

I did swirl the reaction flask and got a little more gas.

I also was able to swirl the bubbler since it was clamped into a stand.

Swirling seemed to help dislodge black powder that was built up inside the bottom of the bubbler.

I could not see any black powder, but my experience tells me that there is probably a little undissolved left in the bottom of the bubbler.

This is as far as I got - this was much fun and I really enjoyed doing this.

Everything is going much smoother this time around.

Tomorrow I'll probably add some HCl to the bubbler and recharge the chlorine generator to get the last of the black powder to dissolve.

kadriver

 

[Lou]

Kevin,

Finish the digestion with some peroxide

 

[kadriver]

Lou,

Great idea. This would be much easier than setting up the chlorine generator again. I'll do it as soon as I get back to the shop.

I spent this whole day cutting down an 80 foot yellow pine tree that kept dropping branches and poking holes in my roof - I didn't even get to work a little today on this experiment.

Thanks again for the AP suggestion!

More to follow.

kadriver

 

[kadriver]

I had some more PGM solutions sitting around so I gathered then together and evaporated them to collect the black PGM powder.

This is 6 liters in these two beakers, it started out as about 15 liters - I evaporated off over 9 liters of liquid.

I think I over evaporated because this horrendous looking salt began to form, even while it was hot.

This photo is after the solutions had cooled to room temp.

 

[kadriver]

I decided to try and filter the salt out and keep evaporating, but the solution was vey syrupy and took a long tine to pass through the filter paper even under vacuum.

 

[kadriver]

Here is what it looked like in the beaker.

 

[kadriver]

I was asked to test a little of the salt so I got a little piece and dissolved it with dilute HCl right in the spot plate cavity.

It dissolved easily and the stannous test revealed what looks to be some platinum.

 

[kadriver]

I dissolved the remaining salt with dilute HCl and added back to the main solution, then added zinc shavings/turnings and cemented out all the PGMs.

After washing and drying there was 2.8 grams of additional black powder that I am planning to add to the original 8 plus grams.

I decided to dissolve with acid/peroxide instead of chlorine and began dissolving the 2.8 grams.

I used 40% H2O2 from Sally's Beauty Supply.

But after a while on the hot plate stirrer I began to see a white to pale yellow precipitate form.

I think I did not get all the zinc out before I started the AP.

Can this be filtered out after all the mixed black powder has been dissolved?

Or should I start over and cement back onto zinc?

kadriver