# first time with cats and PGM



## geologist (Dec 29, 2008)

Hi everyone. At Steve's suggestion, I am posting some tests I started yesterday. I aquired 13 foreign cats and two baggies of crushed honey comb before christmas. Steve suggested using the crushed honey comb as practice to develop technique and skill.

Sample 1 was 112.2 gr and Sample 2 was 118.9 gr. Not a lot to start with but as I noticed throughout the forum, safety is number 1. So a couple of small batches is the wise course (with butyl gloves and safety glasses).

I placed the samples in separate 2-quart containers and added 1 pint of HCl and 1 pint if water. Then approximately half a pint of bleach was added. Both containers were partially covered with lids and placed into separate 5-gal buckets with lids.

This morning I checked on the samples, the liquid in each was greenish yellow prior to stiring and grayish green after stiring. I could smell a slight chlorine odor so I covered them and will check later again today. I will probably stir several times throughout the day for a week or so and adding bleach as needed.

During this time, I will work on opening the 13 remaining cats.

I appreciate any comments and will post pics when I make the stannous and filter. Thanks again Steve.


----------



## lazersteve (Dec 29, 2008)

Sam,

I've never diluted my HCl before adding the bleach. Also, I add the bleach in smaller increments (1/2 cup per addition) since larger additions only serve to produce more chlorine gas than is soluble in the solution. Pumping the bleach in via a tube run to the bottom of the container will insure maximum exposure of the material to the rising chlorine gas bubbles and help agitate the material.

I'm working on a rig that allows me to meter in controlled amounts of chlorine gas with a peristaltic pump. This will keep salts from forming and keep the solution volume minimal.

Temperature will affect the speed of the reaction. Colder temperatures allow for more chlorine to remain dissolved in the solution while warmer solutions speed the overall reaction time. Heat can be applied with adjustable bucket heaters that belt around the bucket.

You should test the solution once per day before making any clorox additions to determine the progress of the reaction. When the solution no longer absorbs PGMs as indicated by the darkening of each successive stannous test, it's time to filter and recovery the mixed black PGM powders with zinc.

Keep us posted.

Steve


----------



## geologist (Dec 29, 2008)

Thanks for the comments Steve. I did not think to test each day and will need to get some tin to make the stannous chloride. I have been having some trouble finding the metals - tin and zinc. The easiest way to get the zinc is just order it from you. I will ease off the clorox for now until I get the tin.


----------



## Oz (Dec 29, 2008)

Steve,

That is a neat pump design but I am curious as to one that pumps a gas instead of liquid. Salt formations when concentrating PGM filtrates from a HCl-bleach solution is problematic, how are you sourcing your chlorine gas?


----------



## lazersteve (Dec 29, 2008)

Oz,

The design is only on paper with about 90% of the parts in hand. The source for the chlorine gas in my prototype will be a simple glassware and teflon pressure equalized addition funnel rig with back flow prevention.

The chlorine gas is formed in a vacuum flask fitted with the addition funnel (HCl into Chlorine solid tabs) and piped into a double layer bucket design. The material stays in the inner bucket and the leach is cycled through the via small electric pumps and values in my grand design. 

The initial prototype will likely just be controlled via pressure differentials in the reaction bucket. All gas input and liquid outputs conducted through gas diffusion tubes and check valves protected from sediment with electrolytic grade polypropylene filter cloth.

In the low tech method complications due to salt formation are easily avoided by using zinc to precipitate the PGMs from the initial leach and redissolving the mixed powders with AR.

My DVD covers this low tech method in depth. The low tech method is a proof of concept reaction that proves the fundamentals for the new prototype device. In an of itself the low tech method is a sound reaction as I have extracted many cats using it.


Steve


----------



## qst42know (Dec 29, 2008)

Have you considered Chlorine gas from a cylinder. I know of a guy that used to make household bleach to sell around the neighborhood from tanks of chlorine like the large argon cylinders welders use. It was a very long time ago but should still be available.


----------



## lazersteve (Dec 29, 2008)

qst,

If I were to ever scale up beyond the prototype device, cylinders would be the next logical choice. For the scale I process on now it's not in my budget to purchase.

I'm also hoping to get my small scale gas phase rig setup and tested this year if possible.

So many projects, so little time...

Steve


----------



## Oz (Dec 29, 2008)

Thanks for the description Steve. I am aware of the zinc but need to get some without the silica to keep it free flowing.


----------



## lazersteve (Dec 29, 2008)

Oz,

I've managed to acquire several zinc discs that I had planned on having lathed into pure zinc turnings. It turns the lathe I have access to won't accommodate the discs. I checked on having another machinist turning the disc, but they wanted too much for the job.

I'm going to have to bite the bullet and drill them out myself with my power drill so we can all have some good zinc. 

I prepared a few pounds of test turnings with my drill and the resulting PGMs had no foreign material after being dissolved.

Mark has also expressed interest in the zinc turnings I'll try to get some posted on my site for sale soon.

Steve


----------



## qst42know (Dec 29, 2008)

What size are the disks?


----------



## geologist (Dec 29, 2008)

Steve,

I may be interested in zinc turnings also since I can not find any locally.

Sam


----------



## Lou (Dec 29, 2008)

If worst comes to worst on the zinc, I can see about ordering a large amount of reagent grade zinc of known analysis from a proper supplier.

It will not be cheap. By the pound it is $30 or so, in bulk probably less. Of course, if anyone sees a supplier that has reagent grade zinc for cheaper, do let me know so that I can order it for them.


As far as the chlorine goes, I think for most of us here, it would be relatively simple to do what Steve is doing with TCCA and HCl, which is an effective, easy method that has been well documented by so many amateur scientists.

Obtaining liquefied chlorine will not be easy without a business license, legitimate use, and probably a little bit of paper work. On the plus side, it's dirt cheap! The nickel regulator is kind of pricey though :-/

As far as suppliers, I know for a fact that Matheson Trigas will sell it to you, but you must have an account set up and be in good standing. They are my gas supplier. Linde or Praxair may have Cl2; mostly like LSO2 as well.


----------



## LittleJohnnyH2SO4 (Dec 30, 2008)

http://www.rotometals.com/ZINC-INGOT-999-Min_p_1816.html

99.9% pure zinc at $2.29/lb plus shipping. How about melting and pouring the zinc into water?


----------



## Oz (Dec 30, 2008)

Beware of breathing the vapors, they are very nasty. I’ll stick to drillings or the lathe.


----------



## Lou (Dec 30, 2008)

It's possible to shot it. Just remember that it will probably stink like phosphine/silane when it dissolves in acidic medium.

There ought to be some 4N zinc.

I prefer using zinc powder of around 80-120 mesh just because it is quick, gives a dense product, and I think I don't have to pay the hazmat surcharge because it isn't considered flammable, or dangerously so.


----------



## qst42know (Dec 30, 2008)

I was wondering if anyone had tried this form of zinc?

Any thoughts?

I have seen 3N5 but haven't found any posted prices. It would save the trouble of pouring shot.

http://www.plattbros.com/zincshot.htm

http://www.abrasivematerials.com/products/zinc_cut_wire.html


----------



## geologist (Dec 31, 2008)

I saw posts of fishing sinkers made of tin. Bass Pro Shops had tin shot for under $2. The pack has 30 pieces and I got the smaller ones so they would dissolve quicker. I could find no info as to 100% tin or an alloy like the tin solder and antimony.


----------



## synthetiklone (Feb 4, 2009)

I get my pure zinc from a local zinc electroplating service. he was generous enough to give me a cast lump/ingot the size of my fist.
he had bucket loads, i have more than enough, maybe you have a similar service in your area?


----------



## goldsilverpro (Feb 4, 2009)

All my life, I used 325 mesh zinc dust for precipitating gold from cyanide solutions. It is available in 50 and 100# pails and is cheap. However, like Lou inferred, it is much more flammable than 100 mesh, under the right conditions. I kept it dry and sealed and never had any problems. Maybe I was lucky. It tended to lump, so I added it to the solution through a squeeze type flour sifter to break it up.

After precipitating the gold, we hung a couple of zinc bars in the cyanide solution and let it settle overnight. The bars prevented the gold from re-dissolving. I usually bought the zinc bars from almost any marine supply. They are used as sacrificial anodes to prevent electrolysis damage to boats. They run about 3 or 4 dollars per pound and can be obtained in many shapes and sizes.


----------



## iis (Feb 4, 2009)

Hi
I bought 99% zinc powder from this guy 5Kg £29 x $40 + postage.

http://cgi.ebay.co.uk/250g-Pure-Zinc-Powder_W0QQitemZ110341969169QQcmdZViewItemQQptZUK_BOI_Medical_Lab_Equipment_Lab_Supplies_ET?hash=item110341969169


----------



## geologist (Apr 3, 2009)

After coarse filtering the fist two batches, I combined them into one batch and placed in HCl and chlorox for several weeks (due to working in Missouri for two weeks and off for one week). I coarse filtered the second run and added it to the first run for about 1.5 gallons of solution. I would like to fine filter with the toilet paper and funnel but was wondering if it might be better to either allow this solution to evaporate or heat it to reduce the over all amount of solution either prior to or after fine filtering. Any comments/recommendations?


----------



## lazersteve (Apr 3, 2009)

Sam,

I would tough it out and filter the diluted solution. 

A few reasons why are:

1) No salts will form in the solution. Evaporation will likely form chloride salts which will hold your values.

2) Dilute solutions tend to flow easier through the Charmin plug. If you concentrate the solution down, it will become thick and viscous. Filtering with a Charmin plug is already slow enough without slowing it down any more by thickening the liquid.

If you can evaporate off just enough so as not to form a salt or thicken the solution, then I would say go for it. Otherwise, don't cause yourself the extra headaches.

Steve


----------



## geologist (Apr 3, 2009)

Thanks Steve,

I did not realize the solution would thicken and since I have no idea how much is enough to NOT form salts or thicken, I will just go ahead and filter through the Charmin plug as is.


----------



## geologist (Apr 7, 2009)

The stannous test was negative - no color change but here is a photo of the cat leachate after fine filtering.

[img:1600:1200]http://img168.imageshack.us/img168/6285/filteredwstannous.jpg[/img]


----------



## geologist (Apr 7, 2009)

this photo is of my class ring which was labelled palladim plus when I bought it in 1979. The stannous test was greenish black.

[img:1600:1200]http://img168.imageshack.us/img168/7679/classring1.jpg[/img]


----------



## geologist (Apr 10, 2009)

Any suggestions on the yellow cat leachate? I was thinking that maybe the container I used should have had a larger diameter. That way the crushed honey comb would be a thinner layer and would have more surface area for the HCl and chlorox to react with.


----------



## lazersteve (Apr 11, 2009)

Sam,

For crushed honeycomb I use an emptied clean high density plastic one gallon juice jug (Hawaiian Punch). I use enough acid to just cover the honeycomb and add clorox in 1/8 cup increments added periodically.

I process about a 1.5- 2" layer of material in the jug with HCl-Cl over the course of several weeks. I give the jug a very vigorous shaking every time I see it. During that same time I'll add in another 1/8 cup of bleach if I notice the yellow-green chlorine cloud inside dissipates. Open the lid with caution as the chlorine gas will take your breath away and choke you.

I also keep an eye on the pressure inside the jug so it doesn't burst.

This method gets the PGMs albeit very slowly.


Your test swab of the yellow solution appears to have a hint of orange (Platinum). The color looks very light compared to what I'm used to seeing even when working at or below room temperature. Perhaps you need to agitate the honeycomb acid mixture more frequently during the leach process. 

Depending on the source of the material your material may be barren. If it were me I would test a very small sample of honeycomb in a test tube with hot AR to see if you get a good extraction, if not, you may have gotten a hold of some bad material. If you decanned the cat yourself this is not very likely the case. 

Steve


----------



## geologist (Apr 11, 2009)

Thanks Steve. Shaking a bottle is better than stirring periodically. I may break the material into two or three batchest for better contact after it settles.

Do you thnk I should process what I have at this time rather than mix it with future solutions?


----------



## lazersteve (Apr 11, 2009)

Sam,

The mix should still contain active muriatic acid so I would say use it on the next batch. Of course you will need some fresh Clorox. This assumes you have not added any precipitants to the liquid (eg. ammonium chloride and/or sodium chlorate).

Steve


----------



## geologist (Apr 11, 2009)

Steve,

All I did to the leachate was filter it through coffee filters and and the charmin plug. With my job being away for two weeks at a time and the weather in PA, I have not gotten past filtering of the leachate. Now that the weather is warming and with your mentoring, I will try to get past the filtering to at least dropping out the PGMs with zinc.

Sam


----------



## geologist (Apr 21, 2009)

I placed the class ring into a bootle as Steve suggested for the crushed honey comb Last week. The solution is still orange red and the stannous test is greenish black. The ring has turned black and I wonder if it may not be better to us some nitric to try to dissolve the ring completely. there is a fine white particulate in the bottom of the bottle. The bottle was a Cl, and chlorox in the bottle.

Any suggestions on total dissolution of the ring and what the white particulate might be?


----------



## Oz (Apr 21, 2009)

geologist said:


> The bottle was a Cl, and chlorox in the bottle



Are you saying you used HCl and bleach (sodium hypochlorite) to put you palladium ring into solution? If so heat can help but is a 2 edged sword, it speeds the reaction but the warmer it gets the less free Cl2 gas your solution can hold (use small additions). If you need too many additions of bleach you will also have trouble with sodium chloride crystallizing out when you concentrate the solution for precipitation.

There is a good chance your white powder is silver chloride. It will also interfere with your HCl-Cl2 getting to your palladium as the silver will form a pacification layer of silver chloride.
If you go to AR at this point the sodium chloride can become a problem when triple boiling to remove the nitric before precipitation and you will still have a chloride that will coat the surface if silver is there in any quantity.

So far it doesn’t sound like I’m helping does it?

If you have nitric I would rinse the ring well and clip out a section and try a small piece in nitric (save your palladic chloride solution of course). Incinerating first to remove HCl in this case is not critical unless you suspect gold. The small amount of AR should not hurt. If the nitric works (heat will help) dissolve the remainder of the ring in nitric, after all is dissolved combine your first and second solutions, this will precipitate most if not all of your silver since you are adding a chloride to your nitric solution. Filter, then proceed to triple boiling to remove all nitric. Check to be sure you have not formed more solids (if so filter or decant), and proceed as usual with your ammonium chloride and sodium chlorate to precipitate your palladium.

This is based on the loose assumption that you have a palladium/silver alloy, that you were using HCl and bleach, and have nitric available.

Note; if you have too much sodium chloride from your bleach to be able to triple boil and remove your nitric you will need to cement your values out to remove it from the sodium chloride in solution.


----------



## geologist (Apr 21, 2009)

thanks for the comments Oz. I am not totally sure what the alloy of the ring is, there might be silver in it. I never gave it much thought.

I would think that rinsing the ring off and dissolving in nitric and/or AR may be the way to go at this point. Determining the metals in the alloy would be the next step. I should have given this more thought and possibly questions in here before attempting refining.


----------



## Oz (Apr 21, 2009)

The harder lessons are the ones we learn the most from. I am only in the position to help because I have made similar mistakes.

I would stay away from the AR for now since there is a good chance the white powder you are seeing is silver. The AR will give you pacification problems similar to your HCl-bleach. Try a small piece in nitric.


----------



## geologist (Apr 21, 2009)

A small piece in nitric may be a problem. The ring is quite thick clipping a piece off it may be difficult. This may take some thought, a cold chisel may work if I can find one.


----------



## Oz (Apr 21, 2009)

I would preferably use wire cutters but if you do not have a good pair use a hacksaw over paper and save the filings. You know what tools you have but I can see pieces flying with a cold chisel. I just didn’t want to see you commit the entire piece to a process until you saw if nitric would work well.


----------



## geologist (Apr 21, 2009)

The wire cutters worked and I was able to get a small portion from the narrow section of the ring. Upon closer inspection with my 20x hand lens, the underside of the ring looks like galvanized metal leading me to wonder if the ring was not plated with palladium alloy. It "feels" too heavy to be aluminum but it could be something heavier then plated.

The top of the ring shows more dissolution in some areas as well as a white powder in most of the open areas such as around designs and letters. I would post a photo but doubt if I could get the zoom and focus good enough for a post.

The ends where I cut it look silvery on one side and cast on the other end.


----------



## Oz (Apr 21, 2009)

Short of someone here knowing the alloy content of "palladium plus" (I am unable to find it) you gave I would try your small piece in nitric.

Let us know.


----------



## geologist (Apr 21, 2009)

Thanks Oz. I am looking for nitric and will try when I find it. I also welcome comments from others.


----------



## geologist (Apr 21, 2009)

Oz, attempted to reply, but it will not send. Thanks for the offer, it is much appreciated.


----------



## Oz (Apr 22, 2009)

I got both PMs but I just got in from a job and it is 3am. I will reply tomorrow.


----------



## geologist (Jun 2, 2009)

Hi Steve,

I tried the first batch of filtered HCl-cl solution. All of my solutions are yellow, kind of like a lite beer. When I do test with stannous, I get a slow color change to grayish green (Steve once said he saw a hint of yellow).

Anyway, I added the sodium carbon ate slowly and made sue it was all consumed before adding more. The solution did get darker, a kind of greenish color and when the sodium carbonate foamed it would always decrease with stirring until at one point the foam was a dirty gray and would not decrease. At this point a white precipitate did form and I added zinc which did not foam. Is it possible that I pushed the solution too far basic, above 3.5-5, and that the zinc will not react?

The material that I am using is the crushed honey comb that I got from the man I purchased the cats from. Because of the slow color change with stannous, I keep wondering if this material was not already processed. I do have three honey combs in HCl-clorox in a 5-gal bucket. All the small pieces that broke off the 5 or 6 cats when I harvested the honey combs are in a bottle.

Maybe I should just set all the previous work aside and see what others think and concentrate on the harvested honey comb. At least that way I am working with raw materiel.

Any thoughts anyone, LazerSteve


----------



## lazersteve (Jun 2, 2009)

Sam,

You may be correct about the material being previously processed.

How long did you allow the leach to work on the honeycomb and at what average temperature?

Did you regularly agitate the sediment to expose the crushed material to the acid?

Typically my stannous tests react strongly and quickly.

It may be best to obtain a whole cat and start from scratch harvesting the honeycombs yourself.


Steve


----------



## geologist (Jun 2, 2009)

Steve,

I left the leach work for about 2-3 weeks sitting outside in a plastic bucket at an average temperature of 65-70 degrees (warmer during the day) sitting in the sunlight. I would stir or tap the bucket every few days.

The honey comb pieces I had in a bottle changed color (orange) quickly when I tested it. Another reason I think the crushed mat'l may have been processed.

Thanks

Sam


----------



## geologist (Jun 3, 2009)

Removed two honey combs from HCl-cl to find fine needle-like yellow green crystals around the mid point of the top honey comb (they were stacked in the bucket). They were water soluble, I used a spray bottle to wash them off the honey comb. 

I did a search in the forum to find most crystals associated with gold processing.

Are the crystals a problem? Did I do the right thing in washing them off and then filtering the solution?


----------



## lazersteve (Jun 3, 2009)

Sam,

They are perfectly normal. I think they are either sodium chloride or chlorine hydrate crystals. 

Here's some reading:

Gas Hydrates

Steve


----------



## Lou (Jun 4, 2009)

Most likely both.


----------

