# Aqua Regia Prize



## justinhcase (Jun 15, 2014)

I had a nice little bit of history come in with a job lot of scrap.
It was an A.R.P. badge from the 1940's very nice London Hallmark and nine grams of silver.
Now I was going to bung it on ebay but thought..A.R.P.
Why not re-purpose it and give fellow refiners a chance to hold some thing I think has a little meaning.
This badge was given to some one of importance with in the Air Raid Warden Service at a time of war.
Some one went out of there way to make an object out of scarce materials in a time of hardship so I hope that who ever wins it will appreciate it, hold it for some time. 
And hold a similar competition so as to hand it on to some one else.
A.R.P. can as easily stand for Aqua Regia Prize as Air Raid Precaution so it seems apt.
Who ever can come closest to estimating the weight in grams of the gold recovered from this one letter flask will be sent this very nice little badge post hast.
Good luck and hope you all do well in your hunting.
Justin


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## FrugalRefiner (Jun 15, 2014)

I'll jump in first. 62 grams.

Dave


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## rewalston (Jun 15, 2014)

nice ruby red you have there. I'm going to say 75g

Probably way off but what the heck :lol:


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## dannlee (Jun 15, 2014)

88.8


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## necromancer (Jun 16, 2014)

51.6g


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## GotTheBug (Jun 16, 2014)

28.9


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## Anonymous (Jun 16, 2014)

16.4g


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## shmandi (Jun 16, 2014)

42 grams


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## justinhcase (Jun 16, 2014)

Well some have come with in 25% of the answer but no cigar yet.
I know how much there should be as this is a second run of material.
It is evaporating off nitric acid at the moment so should be dropping in a day or so.
Work is the bani of the drinking classes and I have a lot on this week.
So every one gets one go and if no one has hit the nail on the head by the time it is melted.
Who ever is closest will win.Remember if you win to pass it on when you do an interesting run for every one to speculate about.
Great post's chap's keep it up.
Just


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## goldenchild (Jun 16, 2014)

124.4136 grams


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## justinhcase (Jun 16, 2014)

:lol:


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## 4metals (Jun 16, 2014)

104.9 grams. 

Have you ever considered using sulfamic acid in lieu of evaporating?


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## justinhcase (Jun 16, 2014)

I do use a little Sulfuric acid to help get rid of lead.
But am not much of a Chemist so have stuck with the fool proof method set out by Mrs Hoke and her farther.
I may try a shorter route once I have gained a little experience.Any way I have one hundred and one things to do when I am home so it is easy to leave it for a day or two and nice to watch the development.
Have silver on the go and have to have this site cleared in two weeks so I can finish my extension. 
I have converted my old tool shed into a small lab and put a lean-to on the out side for reactions.I did buy a fume cupboard from a local school which they said would brake in half.but got it home and found it was made of very good weld so it is now in storage until next year.
I have come up with a wet scrubber from off the shelf bit's and bobs which I hope will fill the gap ok. (100l rain barrel and a plastic aspirator designed to clear mud out of ditches+ 400w sealed pump+conduit+green house sprayers. ).
But if all's well it will be a summer of building work and P.G.M. running in the back ground.
May be if I get a moment I will have time to try some more exotic reactions.
Thanks for the suggestion on Sulfuric instead of evaporation I will look it up and spend my night shift at work learning some thing of interest.


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## slickdogg (Jun 16, 2014)

98.6g


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## joubjonn (Jun 16, 2014)

80gr


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## dorutzu (Jun 16, 2014)

30 g


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## etack (Jun 16, 2014)

200.g bob

Eric


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## maynman1751 (Jun 16, 2014)

101g


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## necromancer (Jun 16, 2014)

goldenchild said:


> 124.4136 grams



4 decimal points :lol: i like this guess


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## pattt (Jun 16, 2014)

hi,
my guess 90 grams :lol: 

also, 4metals said sulfamic acid, not sulfuric :

4metals:


> Have you ever considered using sulfamic acid in lieu of evaporating?



you:


> Thanks for the suggestion on Sulfuric instead of evaporation I will look it up and spend my night shift at work learning some thing of interest.



pattt


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## justinhcase (Jun 16, 2014)

thank you for pointing that out pattt.
I was in a rush to get to work and miss read.
Always trying to cramb to much into a limited time.
Still now I am in work I can take my time, as long as no alarms go off I am free to studdy.


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## shaftsinkerawc (Jun 16, 2014)

96.6 grams


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## Digitaria (Jun 16, 2014)

I'd like to guess 27 grams.


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## g_axelsson (Jun 16, 2014)

68.5 g

Really nice color!

Are you doing the evaporation in that flask? If you do then I suggest you try an evaporating dish, the larger surface area and lower sides makes it a lot faster.

Göran


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## justinhcase (Jun 16, 2014)

Thanks Göran.
I thought about using an open evaporating dish,but wanted to make sure I limited any loss if it started to knock.
obviously I am using a graham (distillate through spiral) condenser when I digest to keep everything in my digestion flask ,and wanted to make sure I minimised loss during evaporation.
I try not to let it boil but some time's when you are getting the heat right it will knock a bit.
was I being to paranoid??


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## Geo (Jun 16, 2014)

64g. 

Sulfamic acid works well to remove free nitric acid. Sulfamic acid, when mixed with nitric acid, will evolve nitrous oxide (laughing gas) and is a clear, sweet smelling gas. Add solution of saturated sulfamic acid in water slowly in small increments allowing time for the reaction after each addition. When there's no more reaction, free nitric is gone.


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## justinhcase (Jun 16, 2014)

I have just ordered 1k Sulfamic acid to try out next time as it would save a lot of time.
Thank you.


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## yar (Jun 16, 2014)

44g, nice red color!!


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## justinhcase (Jun 16, 2014)

necromancer said:


> goldenchild said:
> 
> 
> > 124.4136 grams
> ...


The only problem with four points is I only have a scales that detect only three.
http://www.ebay.co.uk/itm/121128444551? :lol:


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## danieldavies (Jun 16, 2014)

36 grams of gold


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## Platdigger (Jun 16, 2014)

19.75g


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## necromancer (Jun 16, 2014)

justinhcase said:


> necromancer said:
> 
> 
> > goldenchild said:
> ...



oh no, i think we are going to have to disqualify goldenchild (joking)


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## etack (Jun 16, 2014)

Geo said:


> 64g.
> 
> Sulfamic acid works well to remove free nitric acid. Sulfamic acid, when mixed with nitric acid, will evolve nitrous oxide (laughing gas) and is a clear, sweet smelling gas. Add solution of saturated sulfamic acid in water slowly in small increments allowing time for the reaction after each addition. When there's no more reaction, free nitric is gone.



Yum...............

DO you have a recipe for this? purely scientific reasons of course. 8) 8) 

Eric


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## justinhcase (Jun 16, 2014)

etack said:


> Geo said:
> 
> 
> > 64g.
> ...


I was going to say it might be worth a laugh but though that may be a bit of a sixty's joke.for this forum :lol:


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## justinhcase (Jun 16, 2014)

Crystallized while I was at an other job.
But dissolved fully again straight away.
Just dilute it a bit more and start to drop.
Should have a bar and left over button end of tomorrow.


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## Geo (Jun 16, 2014)

etack said:


> Yum...............
> 
> DO you have a recipe for this? purely scientific reasons of course. 8) 8)
> 
> Eric



For purely scientific reasons : Nitrous oxide can be made by heating a solution of sulfamic acid and nitric acid. HNO3 + NH2SO3H → N2O + H2SO4 + H2O

After looking at this myself, the byproduct is sulfuric acid. Thats a bit of useful information to me. :lol:

I feel I should add that other gasses are formed that can and will be dangerous to inhale so DON'T DO IT!


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## necromancer (Jun 16, 2014)

justinhcase said:


> Crystallized while I was at an other job.
> But dissolved fully again straight away.
> Just dilute it a bit more and start to drop.
> Should have a bar and left over button end of tomorrow.



are you saying that there is enough free nitric to redissolve the gold precipitate, even after evaporation ?

what are you going to dilute with ? i hope it's HCL ?


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## glondor (Jun 16, 2014)

99.95


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## Digitaria (Jun 16, 2014)

When does the competition end?
Thanks


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## necromancer (Jun 16, 2014)

justinhcase said:


> Well some have come with in 25% of the answer but no cigar yet.



hints like this are not fare to those that guessed before the hint was given.

you tell people within 25% of the number, doing the math after the hint is a good way to win, guessing before the numbers is just an honest guess

(my 2 cents about giving hints to the latter group only)


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## butcher (Jun 16, 2014)

Ahh come on, sure it is fair, I guess 25% more.
:lol:


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## necromancer (Jun 16, 2014)

butcher said:


> Ahh come on, sure it is fair, I guess 25% more.
> :lol:



hit the nail right on the head (winner, winner. free chicken dinner)
or as they say in Quebec (gagnant, gagnant. dîner de poulet libre)


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## justinhcase (Jun 17, 2014)

Well I said some had come with in 25% but not who,I thought it was vague enough but maybe not.
sorry if any one feels they have not had a good opportunity to bat,I have to admit I am a terrible card player.
Viva la Ontario très bien très magnifique!!


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## justinhcase (Jun 18, 2014)

Well the total was 111.524g
It seems the winner is 4metals if I have missed one let me know.
So the little badge will be winging it's way to the northeast of the USA.
Thanks to every one for playing it has been great fun.
Now just have to send it off to see how well I did, let's hope I have managed the rid my self of some of that unwanted 0.04%.


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## maynman1751 (Jun 18, 2014)

Thanks for the contest Justin. I'm surprised that I got so close with 101g. :shock:


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## necromancer (Jun 18, 2014)

thank you, guessing game contests are great,


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## butcher (Jun 18, 2014)

Dang, I guessed 25% too much.
Thanks for sharing the great pictures of your gold in various states, very nice examples of gold in more pure solutions and powders, and concentrations, and a very nice gold bar.

In this case I say justinhcase is the winner here.


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## justinhcase (Jun 18, 2014)

Thank you very much butcher that means a great deal coming from you.
still looking at the auction recepts since Christmas but it is looking good.
It takes time hovering up the unwanted lot's but may just pay off in the end.Fingers crossed for a good result from Sheffield so I can cash it in and start all over again.If 4metals wants to P.M. me some postal details it will be my pleasure to send him a little bit of U.K. history.
Thanks to you and all the other's who make his site work. the education it continues to provide is invaluable.


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## 4metals (Jun 18, 2014)

Wow I just did a guestimate at the volume and factored in the maximum concentration aqua regia holds and used that number. I love AR when it is that red!


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## heliman4141 (Jun 18, 2014)

4metals said:


> Wow I just did a guestimate at the volume and factored in the maximum concentration aqua regia holds and used that number. I love AR when it is that red!




You just answered the burning question that I was going to ask you..............I thought, how on Earth did he precisely calculate that by just a picture? :shock: 
That was a fun contest with a cool ending!

Dave


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## g_axelsson (Jun 21, 2014)

Interesting to see that both this and the last contest (tantalum capacitors) were won by using math.

Thanks for the contest. 8) 

Göran


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## justinhcase (Jun 21, 2014)

Well Maths and a very good eye coupled with a lot of experience I would say.
Mr 4metals obviously knows his stuff to a very high level.
Still waiting for postal instructions.
:lol:


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## necromancer (Jun 21, 2014)

heliman4141 said:


> 4metals said:
> 
> 
> > Wow I just did a guestimate at the volume and factored in the maximum concentration aqua regia holds and used that number. I love AR when it is that red!
> ...




i guess he's just that good 8)


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## samuel-a (Jun 22, 2014)

Very nice job Justin !


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## justinhcase (Jun 22, 2014)

Thank you very much Sam.
That is very much appreciated.
Justin


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## justinhcase (Jul 3, 2014)

I was going to leave this until I had the bar back.
But I have to say I am just tooooo excited.
Just spoken to Sheffield Assay office.
And I am actually embarrassed to say I had to look it up.
But apparently the bar was three nines.
I was hoping fingers crossed to be 99.98 and had set my hopes below the 99.99% so as not to be disappointed.
I am quite Chuft to be told I got to 99.999%.
What would be the best way for me to get a good price so I can cash it in and start again.
I was going to try eBay but now I am band for life I have to rethink.
I cant wait to see what it looks like with my hallmark when they have finished.
Thanks again to every one.
Just


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## shmandi (Jul 3, 2014)

If your bare is 99.999% pure, that is actually five nines


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## justinhcase (Jul 3, 2014)

I know I have just look at some other article's and I am a little bit confused.
On the market, 99% purity of gold is called “pure gold”. 99.9% or higher is called “thousand pure gold” which is what I got last time.
Among common gold jewelries, gold bars and gold/silver coins, the highest purity is 99.99%, which is also known as “four 9s”. In the new edition of national standard, “high-purity gold” means 99.999%, which is “five 9s”.
then I saw Nines are an informal, yet common method of grading the purity of very fine precious metals . Based on the system of millesimal fineness, a metal is said to be one nine or one nine fine if it is 900 fine, or 90% pure. A metal that is 990 fine is then described as two nines fine and one that is 999 fine is described as three nines fine. Thus, nines are a logarithmic scale of purity for very fine precious metals. 
so I took it to be a mathematical way of describing a very small percentile.
I may have been a bit to pleased with the result but the way she said it was different to the 99.96% description they told me the last time and she did make a bit of a fan fare so I got a little bit swept up..
When I mused as to what impurity's where left she seemed a bit taken back as if I should have been satisfied with the result.
I will scan and post the results when they arrive so you can help me decipher them.
Would an analytical lab Like the Sheffield Office use an informal description or describe it in decimal point's
Just


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## goldsilverpro (Jul 3, 2014)

justinhcase said:


> I know I have just look at some other article's and I am a little bit confused.
> On the market, 99% purity of gold is called “pure gold”. 99.9% or higher is called “thousand pure gold” which is what I got last time.
> Among common gold jewelries, gold bars and gold/silver coins, the highest purity is 99.99%, which is also known as “four 9s”. In the new edition of national standard, “high-purity gold” means 99.999%, which is “five 9s”.
> then I saw Nines are an informal, yet common method of grading the purity of very fine precious metals . Based on the system of millesimal fineness, a metal is said to be one nine or one nine fine if it is 900 fine, or 90% pure. A metal that is 990 fine is then described as two nines fine and one that is 999 fine is described as three nines fine. Thus, nines are a logarithmic scale of purity for very fine precious metals.
> ...



In the US, things are a bit different. As I understand it, the terms, "Fine Gold", "24K gold", or commercially pure gold indicate a minimum purity of 99.95%. "Fine silver" is 99.9% pure, or better.


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## samuel-a (Jul 3, 2014)

Chris,

As far as i know, it is the standard worldwide. 

justinhcase
You did good. 
For commercial purposes, there's really no reason for you to produce 99.999% (five nines / 5N). Even if you had COA for the gold, no one will pay higher premium than they would for 99.95% gold.

Even the largest firms (JM, Heraeus, Metalor etc'... ) do not charge over 6-8% premium for high purity PVD grade PM's.


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## justinhcase (Jul 3, 2014)

Well I just was disappointed with the 99.96% so put it back into A.R. and did it again which I have to say was very satisfying.
I was surprised how much solid's I actually was able to filter from what I had thought was a good sample of Au.
I do owe it all to you fine chap's.your constant coaching and encouragement make's the hole process so much more achievable.
thank you and I hope every one realize just how rare and special this space is and pay's it the respect it deserves.
J.


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## justinhcase (Jul 9, 2014)

Had my bar back and it go's to show you should not try to take information over the phone.
They where using the informal system of rating and not as I had thought one based on decimals.
It was only99.98%  
Still the good new's I have my eye 0n that last 0.01% and I will have great fun trying to find and extricate it from my next batch.
I will have to leave this little bar unfinished,close but no cigar yet..
Just


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## butcher (Jul 9, 2014)

I say that bar is worth a cigar or two. 
You should be proud of it.
That gold is 999 nice  and pretty.

It would be difficult to get that last bit of impurity without using an electrolytic process, or a very exhaustive aqua regia process, with ultra pure chemicals, where even the water used can become a source contaminants. The closer to pure the gold gets the harder it is to remove the small traces of other metals, by chemical processes.


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## justinhcase (Jul 9, 2014)

Thank you.
I am not to unhappy as it was only my second real run so it is good to have to work for the last bit.
Most of my chemicals has been form A.C.P. Pure so I may try some higher grade consumables in the future, and invested in a little £80 still so I no longer run out of distilled water which has been a real boon.
So will just have to be even more obsessive with each of my processes.
It is very nice to see my own hallmark, now I have to see how meany more bar's I can produce.
Been trying my wet scrubber had some teething problems with standard fittings giving way but should be worked out soon.
Much thanks for every one's help and encouragement,I am having a ball in the dim dark back waters of Devon.Extremely chuffed to have almost completed the circle.

Hope you all are having a similar.
Just


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## Anonymous (Jul 9, 2014)

Justin unless you want to throw money away for the fun of it then that 0.001 really isn't a problem.

Also if you are buying your chemicals from APCPure then you're paying well over the odds for everything.


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## butcher (Jul 10, 2014)

Thanks for the picture of your setup.

I enjoy working outdoors, I built a shed, thinking I might try indoors, then decided I like it outside more, and do not care to work indoors, so I have not installed the fume hood in it, and have just used the shed for storage so far, and probably will not use the shed to recover or refine indoors, I like the way you have the outdoor setup, the best of both worlds.

It does look like you could add a little roofing over the area you stand and work.

Nice distilling rig, I bought one, and have had it in the box for several years now, I cannot seem to get myself to use it, my ole homade distilling rigs have worked just fine so far, I cannot bring myself to using the fancy lab glass distilling rig, which may get broken (that lab glass is just too pretty to break).


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## justinhcase (Jul 10, 2014)

Spaceship, I did try to get some of the larger firms to supply me but they will not deliver to a domestic address, Will be getting some proper suppliers when I have moved away from home.(Unless you know of any you could recommend).
Butcher I only use the glass for alloy digestion and have a little stainless steel rig under the fume cupboard/Squirrel defense's for H2O.
I wanted to scrub my fumes but also stop the critters getting to my kit when it is unattended.
I have extended the shed roof to cover the work space but I do have a habit of leaving cover out of the equation for the human components. :lol: 
I am surprised to hear you are an out door refiner,I thought you would be in a large lab from the level of knowledge you have on the subject..
All the best 
Just


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## butcher (Jul 10, 2014)

Nope, just a regular guy, with an interest in this field of work, this has been a hobby for me, I am just a member, and back yard refiner like many of our members here, getting a great education, doing something I love, and as someone who has always loved the outdoors, I prefer outdoors. Although freezing nights, and hot days, and rainy weather, working inside may be a bit more comfortable, I just do not wish to be closed up in a box. 

I have had no formal chemistry training, or schooling, I have learned the chemistry from the forum and studying what interested me.
This is one reason I try to stress study to our new members, it is amazing what you will learn when you have an interest, and put a little effort in pursuing educating yourself in that interest.
Having the forum as a reference, you can learn easily (even without asking questions, basically of which I have not needed to do, there is plenty of information provided here on the forum by our generous members, enough for me to study my lifetime. 

I would love to try and go to a school and learn some of this, but also I have never really liked schools, they tend to be restrictive, in my mind, wanting you to learn certain things in certain ways, learn things you have no interest in, or memorize things just a to pass some test, and where you can easily just forget what you have studied, where if you learn from following your interest, at your own pace you understand better what you are trying to learn, you can see it in a different light, and you may not just memorize it and forget it after the test is over, but apply what your learning to gain a better understanding, you can actually get to where you know it (not just memorized it).

I have never had a memory anyway, I think elephants can memorize more than I can.

In this way I think of the forum as a university, with a great library, with helpful teachers, and fellow members with the same interests, who help guide you in the beginning, to help you learn to find the reference material, needed to pursue your interest and education. With friends who share what they are learning with us others on the forum, and helping to promote this interest. 

A great university indeed.
The best in the world in the science of precious metal recovery and refining, and its chemistry.


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## necromancer (Jul 10, 2014)

nice set up, much better then my table in the woods when its to hot in my shop.

i wonder if you will get the same response as i did working outdoors with no fume suppression ??

keep up the good work, your trees look very happy & healthy !!


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## justinhcase (Jul 11, 2014)

Trees are our friends.
My little shed is always cool as it is given shade by four lovely large sycamore's growing just off my boundary line..
Most trees are actually protected over here , which can be a bit of a pain as you have to apply for permission to even coppice.
Some you have to go to court and explain your self to a local judge before you can even harm the bark.
My friend who is a chemist for South West water(and who kindly donated half my beakers)informs me that they are a vital part of any large facility that produces fume's.
On top of scrubbers and catalytic converters tree's are used to surround the facility as they draw toxins out of the air naturally in a very cost effective way.
They would be of little use by them self's but when facility's are being constantly monitored and there performance rated over years or decade the accumulative effect is more than detectable and brings the over all level of pollutants down in the aria.
Plants amaze me , if only we could convince them to draw up selective elements on demand in high enough concentrations to make phytomining productive we would be a step ahead.
I bet you get some nice trout or steelhead close to your camp Necro.very nice, all I have is Watrose(which is a large supermarket firm over here)..
P.S. I hope you like my little fume scrubber.400w harsh environment sealed unit submersible pump(second hand £20)with a four way flow controller feeding. one large home made aspirator for the cabinet, one lab aspirator for glass ware.and a return circuit for feeding spray heads all the way up the chimney made from an old gutter.
Only a 100l reservoir but with the small level of work I am doing more than enough,I just check the P.H. every day or so and equalize it.


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## Geo (Jul 11, 2014)

We have a couple million tree huggers over here, want to make a trade? :lol: 

I'm just kidding guys. I love my trees as much as any could.


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