Recomendation needed

[MrCrusher]

Hi Everyone,

I wanted to thank everyone first and foremost for all the great information here. I have spent many hours here and studying. I needed a new hobby and watched some you tube. ( Streetips not the obvious danger dans ) Thought I would really like this.

Well I started gathering the basics, when I suddenly realized . . . WOW this is getting costly to get set-up right. Anyhow I have a reasonable lab going now and have done some basic processes. While I know from here really small batches are not very profitable, they are great experience.

I have had a few mistakes along the way. And by searching here have found what I needed ( at least as a noob I think so )

I just managed to get my last Item which was some gas tanks for melting. Since it was a long weekend I wanted to take all of my saved up filter papers with my small batches in them and put it all together for a melt.

I now have a situation I am not sure of the best way to resolve and could not find an answer for. Here is the situation.

I was processing a batch of GF material. I have been using Harold's process for that. So when I was doing my 2nd incineration I added all my saved filter papers and incinerated them with the batch I was running. I then did the HCL bath per the process. I then filtered and rinsed the material and put back in the beaker to dissolve the gold. I am getting low on Nitric so I thought I would dissolve with HCL and Bleach.

This is where I am now. The problem is the gold does not want to dissolve completely. The solution test positive for gold but there is still lots of gold in the beaker. Since I have never tried to dissolve this amount of gold at once before ( ~ 35 grams) What would be the best path to go from here?

I am not sure how much HCL + bleach I would need for this. I currently have 400ml in a 2L beaker Which is ~ 350ml of HCL and 50ml of bleach.

I have some thoughts but would be grateful for more experienced advice.

Thanx
Mr_Crusher

 

[Geo]

Did you grind or mill the material to a fine powder? The HCl/bleach method works best on really fine material. It could be that the remaining material is not gold. Decant the pregnant solution into a clean container leaving the solids behind. Either test the material with a little AR or rinse and mill it smaller.

 

[MrCrusher]

Geo,

I did not grind the material. ( lesson learned )

I noticed when I incinerated my previous batches that the gold powder in the filters seamed to "lump together" That is what's in the beaker, the lumps. I don't think I actually melted the gold during the incineration I was only using a small propane torch.

Well If it was you would you: ( not that you would make this mistake in the first place )

Decant into clean beaker and just use AR to dissolve the rest after rinsing. Or grind and stick to the HCL bleach?

Also I would think I will need to drop the gold from both solutions separately if I use AR to finish the job?

I am guessing that the amount of HCL and bleach was enough volume to dissolve that amount of gold ( finely ground )

By your command . . 8)

Thanx Geo
Mr_Crusher

 

[Geo]

Since it takes roughly 1 mL of nitric acid and 3 mL HCl to dissolve 1g of gold, You can dry and weigh the material left for a reasonable estimate of acid needed or you could add an excess of HCl and heat. start adding the nitric by the drop until you do not get a reaction. let it cool and settle and decant the ARsolution into the previous solution as it can all be dropped together. The losses are less, the more you do at one time in one large batch as apposed to several smaller ones.

 

[nickvc]

You could also use poormans AR the recipes for which are all over the forum.
You could also try adding hydrogen peroxide to some HCl this is a stronger oxidiser and may work if you haven't got solid pieces of gold.
Can I say well done for reading and trying to educate yourself it makes our lives so much easier to explain ideas and processes.

 

[MrCrusher]

Update

I followed Geo's advice and went with the excess HCL and slowly added Nitric until all gold was dissolved.
It worked wonderfully. I am now rinsing and am going to dissolve it one more time as I really want as close to .999 as I can get. If everything goes as planned I hope to make my first button on Independence day 8)

I do have one other question. I know it has been addressed in a few places here. I have tried 4Metals "Alconox" recommendation for cleaning my glassware I am now using Bon Ami.

It seams no matter how spotlessly I clean my beakers "some" brown film always sticks to it when I make a drop. I am obviously doing something wrong. I am thinking, should I not dry my beaker with a paper towel,
Is that causing my issue?

Also as of this posting I notice there have been almost 100 reads on my post. Suddenly I feel so popular.
However I also know I am sure many of the experienced refiners here look over the new help wanted to see what "laughable" new thing some noob did. Heck I am a noob and I admit I rofl at many of the noob post :lol:

While I am sure I would have resolved my issue on my own in time, Since it was all my work so far I was in a little panic when the process did not go exactly as I had planned.

If I can figure out how to post a pic here I will post a pic of my first button. I want to thank everyone here for the fine job helping others and being so logical.

Thanx
Mr_Crusher

 

[nickvc]

For your beaker problem keep one dedicated new beaker just to precipitate in and clean well after use.
If you are going to refine your gold again use HCl and Chlorox as now it's all finely divided it should dissolve very easily. It's always a good idea to swop methods of dissolution and those of precipitant when aiming for high purity as it helps remove some of the problematic elements such as copper and silver.

 

[jason_recliner]

Mr_Crusher,

Harold has always advocated Bon Ami, while I have tended to use dishwashing detergent, a soft cloth and elbow grease. Either way, they must be sparkling if you want purity. But no matter how you scrub your beakers, and no matter how perfect the glass surface may look, it will always have microscopic crevices and imperfections, to which gold powder may adhere. Some puritans will have a new beaker dedicated to the purpose: for nothing other than precipitation. {Edit: Nick just beat me to it on that one}

Personally I do see the slightest of gold sticking, but if you swirl it around just before it's completely dry, it seems to collect rather well. And my next solution goes into the same beaker, so it's never a loss.

As for the number of views, many of us watch every single post that comes through. Each reply causes a new view by multiple interested readers. Rather than 'laugh at the noob', I would say there are few here who could come close to matching your skill to post ratio; certainly not me. And for this I both congratulate and commend you.

For attempting .999, the only suggestion I would make is that you add your precipitant (presumably SMB) on the second refine in small increments as one would with nitric. For SMB has the tendency to 'co-drag down' copper if applied excessively.
{Edit 2: Starting with 80% of as much SMB as you expect to need, then adding more until it tests negative for gold.}

I look forward to seeing your independence button in the gallery. Welcome to the forum.

 

[Topher_osAUrus]

I use Bon Ami or barkeepers friend, both work well and do not scratch.

When it comes to pre precipitation, i was my glassware (and dry) 3 separate times, and wear gloves the entire time, i also wear gloves when drying them. And i use a roll of expensive shop towels (the blue ones) to dry them, since ive started washing 3x and rinsing 3x and drying 3x with my gloves on, i haven't had any problems with floating gold.

It could also be oils from the material too. But, since you said you incinerated, I am going to guess the material wasn't the cause.

 

[Geo]

Gold will adhere to any surface that has been exposed to tin chloride whether by accident (in a digestion of mixed metals) or by purpose (adding stannous chloride directly to the solution). I did an experiment where I dipped a plastic spoon in stannous chloride. I rinsed the spoon in clean water and wiped the spoon dry. I used the spoon to stir a gold chloride solution after adding SMB and the spoon came out with a beautiful, shiny gold plating. I found that if I stirred to hard, the gold would peel off into shiny flakes. I've seen members comment about having solid gold flakes in their gold drop and not understanding where the (gold foils) came from. Any metal film on the glass will cause the gold to precipitate on the glass. You can wash the glass in some warm AR solution to remove the film.
Tin chloride will create fumes that will collect on any cool surface it touches. It looks like a white glaze on any exposed glassware in the vicinity. It can't be washed off, not even with AR solution because it is converted to tin oxide by the air. It has to be abraded off. Use the green Scotch-brite scrub pads along with the bon ami to really get it clean. The plastic will not scratch the glass.

 

[MrCrusher]

Please enjoy Laughing at this one. :lol:

I deserve it

Well my total impatience to make my first button has well most likely cost me a lot of time and wasted effort.

Now for the funny part ( note I am not laughing yet, myself, but in years to come I am sure I will )

The 2 crucibles I got both cracked trying to season them. I was desperate and have heard you could melt gold in a potato. I went and got a potato. BIG MISTAKE. I did manage to get a nugget done. However I now have a potato with well lets say beautiful gold specks all through it.

I sort of hate to ask but has anyone else ever been this stupid? Err let me rephrase. Has anyone else made this mistake and how did you recover the gold from the potato? Considering how hard these things are to burn I think incineration is out of the question. The only thing I can think of is to let it sit out and dehydrate, then I may be able to burn it.

Since I have no idea what would happen if I tried to put this in any acids I would not think of trying that one. Unless some one here more experienced then me has a known way to process this gold out of the potato.

I would post a pic of the nugget I did manage to make but my phone just wont get a picture worth looking at. It did weigh in at 24.4 grams but has some residue on it I still need to remove. I am sure once I get a "Good" crucible I will re-melt this.

Also for torch melting does anyone have a recommended crucible I should use. One that is durable and worth having?

Thanx
Mr_Crusher

 

[Topher_osAUrus]

Sulfuric will eat up the potato quite well i think.

Or maybe cut out the gold layden portion of your sparkly spud letting it dehydrate as much as possible, then maybe separate with water, as potato is mainly starch it should be fairly easy to get it into water with the gold of course staying on bottom.

I have heard of people using drywall, and a log or piece of coal, i myself have used corningware pyroceram... But i have never heard of the potato until now.

Hope you get your gold!

 

[Geo]

Cut it up in small pieces and burn it to ashes. Collect all the ashes and incinerate.

 

[Topher_osAUrus]

Forgot to add in the end of my last post. =

Can we get a picture of said potato?

I would very much like to see its golden "buttery" goodness.

 

[MrCrusher]

I'll try for a pic I am sort of over it now . . its funny

But I don't know how well the gold will show up

Thanx for the advice guys

Mr_Crusher

 

[MrCrusher]

Ok One Sparkling Spud
sorry about the picture quality
I also included the little nugget that came out of the spud it is much lighter after cleaning it up.

It was 21.8 Grams

 

[Barren Realms 007]

Please enjoy Laughing at this one. :lol:

I deserve it

Well my total impatience to make my first button has well most likely cost me a lot of time and wasted effort.

Now for the funny part ( note I am not laughing yet, myself, but in years to come I am sure I will )

The 2 crucibles I got both cracked trying to season them. I was desperate and have heard you could melt gold in a potato. I went and got a potato. BIG MISTAKE. I did manage to get a nugget done. However I now have a potato with well lets say beautiful gold specks all through it.

I sort of hate to ask but has anyone else ever been this stupid? Err let me rephrase. Has anyone else made this mistake and how did you recover the gold from the potato? Considering how hard these things are to burn I think incineration is out of the question. The only thing I can think of is to let it sit out and dehydrate, then I may be able to burn it.

Since I have no idea what would happen if I tried to put this in any acids I would not think of trying that one. Unless some one here more experienced then me has a known way to process this gold out of the potato.

I would post a pic of the nugget I did manage to make but my phone just wont get a picture worth looking at. It did weigh in at 24.4 grams but has some residue on it I still need to remove. I am sure once I get a "Good" crucible I will re-melt this.

Also for torch melting does anyone have a recommended crucible I should use. One that is durable and worth having?

Thanx
Mr_Crusher

Melting dishes.

How do you crack one seasoning it?

To season one put it in your oven at 100 F, Raise the temp 100 every 30 minutes to an hour till you reach the high temp of your oven. Simple and easy.

LazerSteve has dishes.
http://www.goldrecovery.us/pricing.asp

 

[jason_recliner]

I think the problem is you didn't season your potato. A light sprinkle of sodium chloride is most effective.

Sorry to see you've made such a mash of it, but I yam glad you can see the funny side of your root problem. Something something 24 carrots.
Good luck.

 

[upcyclist]

I think the problem is you didn't season your potato. A light sprinkle of sodium chloride is most effective.

Sorry to see you've made such a mash of it, but I yam glad you can see the funny side of your root problem. Something something 24 carrots.
Good luck.

You're gonna fry for that!

 

[Geo]

If you have ever poured hot metal into a wet mold, well, you will only do it once. I know from experience what happens when melted metal and water come into contact with other. The metal explodes. The water flash boils and the steam created expands much like a real chemical reaction explosion. When the gold melted, it scattered from the water escaping the potato. Your lucky it stayed in the potato. It could have flew every where.