# Not sure how gold precipitate looks like...



## hfywc (Aug 18, 2010)

hi all. 

i tried a small batch of plated pins with AP, with HCL/Chlorox and precipitation with SMB in that order. being new i was careless and did not follow any measurements/ratios of the chemicals. not all the metals melted totally. but i got a nice yellow liquid that i was hoping to be AuCl. 

anyway on the last part with dropping with SMB(i used stump out), nothing happened. knowing that i made a mistake somewhere, i kept the final liquid solution hoping that later on i would be able to remedy it. weeks passed, i noticed the bottom is turning brownish in color. i read somewhere in the forum that it could be that there is an excess of chlorine which prohibits the smb from reacting with AuCl. so i applied heat...eventually this brownish color turned into brown mud which is very fine in nature and easily disturbed when you rotate the container even lightly.

the problem is that i don't know for sure if this brown mud is gold or not for i have not seen an actual gold precipitate....please help. 

thanks,
alan


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## jimdoc (Aug 18, 2010)

It is probably gold.Do you have stannous to test?

Jim


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## qst42know (Aug 18, 2010)

To late for stannous, unless you redissolve a bit and test.


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## philddreamer (Aug 18, 2010)

Hi Alan!
In the photo I was doing the final rinsing w/water. The color can be lighter or darker, depends on purity.

Like Jim said, did you test with stannous, to find out if any gold is still in solution? Do you know how to make stannous test solution?

Phil


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## glorycloud (Aug 18, 2010)

I imagine that your gold precipitate might look more black than brown.
After a few washings with HCL and then water the color gets nice
and light brown like you see in phil's picture.


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## hfywc (Aug 19, 2010)

maybe i could download a picture or two for you guys to look at hmmmm.....

also i'm not sure about the stannous cholride i made whether it's effective or not...i diluted some solder which says 60/40 in some hcl. i heated the hcl until it started to boil and then stop and let it continue it's course. it left some black powder at the bottom. later on i added some tin sinkers which i ordered online to increase potency...

i made three tests on the hcl/clorox solution--two before adding extra tin sinkers and once after. color i got was light brown...

i just found out that the solder i used contains lead... is that acceptable?

also very important!!!! thank you guys for pitching in...


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## hfywc (Aug 19, 2010)

philddreamer said:


> Hi Alan!
> In the photo I was doing the final rinsing w/water. The color can be lighter or darker, depends on purity.
> 
> Like Jim said, did you test with stannous, to find out if any gold is still in solution? Do you know how to make stannous test solution?
> ...



is it heavy? does it settle quickly upon agitation?


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## philddreamer (Aug 19, 2010)

Some pic's would help. 
60/40 no good. Radio Shack has 96%tin/4%silver, that works. Their will be a bit of sediment, it's the silver that doesn't dissolve in HCI. I use 15ml of HCI & 1.5in of the solder. Every couple of weeks I add a bit more solder to ensure its potency; pure tin sinkers are excellent. Lead is no good. And remember, always test your solution! 

The cleaner the gold, the faster it sinks. Like glorycloud stated, your gold it's probably very dark, it means some metals were "dragged down" with the gold, especially copper. 
Use Steve's washing instructions: 
1.Let the gold powder settle to the bottom of the beaker over night.
2.Siphon or gently pour off the used SMB solution into an old milk jug labelled Used SMB. Save in your stock pot or properly dispose of.
3.The gold powder stays in the same beaker you precipitated it in.
4.Add just enough water to cover the gold powder and boil for 5 minutes.
5.Let settle and pour or siphon off the water into the stock pot.
6.Repeat three times.
7.Add just enough muriatic acid to cover the gold powder.
8.Boil for 5 minutes and pour or siphon off into the stock pot after testing with stannous. If gold is present keep in separate beaker to precipitate later.
9.Repeat until the acid is no longer discoloured by the process.
10.Repeat the water rinse as above.
11.If you suspect silver is present as a contamination, repeat the process with hot 3% household ammonium hydroxide (unscented- clear). Put these rinses in a separate container and add muriatic acid until no more white silver chloride precipitates. You have added enough HCl when there are no more white fumes coming out of the liquid. (Any karat, dental, CPU lid, or gold filled scrap will have silver as a contaminate.) 
12.Finish up the rinses with three more hot water rinses. Put these rinses in with the ammonium hydroxide rinses.
13.Gently heat the beaker containing the gold powder while swirling the beaker. As the gold dries it will begin to clump and move around the beaker freely. Don't allow the gold to stick to the beaker. 
14.When the gold is 100% dry it should be a nice light tan color, if not re-dissolve it and precipitate again with SMB. Repeating the above cleaning process after precipitation. Good clean gold settles very quickly when precipitated and clumps into nice balls when dried. No gold should be stuck to the beaker when you are done.
15.When completed transfer the gold to a properly prepared melting dish and melt into a button. 
Steve

I use fiberglass filters & a funnel, it traps the very fine gold. I save the filters & later, when I have few, I process them with HCI/CI.

As the gold gets cleaner, it will settle faster.

I hope this helps.

Phil


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## joem (Aug 19, 2010)

where do you get the fiberglass filters?
would a bunched up furnace filter work?


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## philddreamer (Aug 19, 2010)

I got some @ Home-depot. Fireplace insulation, left over is what I've been using, it also works good. Just pull a piece, about the size of a cotton ball or so. Depending on how fine the gold is, you would compress the plug. I leave the plug a bit loose the first time around, then on the second I compress it more, that makes the solution run thru quicker each time. Paper will be dissolve, can get a bit messy & some even fall into the already filtered solution.

Check this post out in TECHNIQUES: Whatman glass filters for gold stripping cell?


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## HAuCl4 (Aug 19, 2010)

This deceptively simple filtering technique is amazingly effective, and economical, and I learned it right here from one of your picture posts phildreamer!.


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## Anonymous (Aug 19, 2010)

> 4.Add just enough water to cover the gold powder and boil for 5 minutes.
> 7.Add just enough muriatic acid to cover the gold powder.
> 8.Boil for 5 minutes



I routinely add at least twice the volume in water or acid.Any less and you risk "popping" the gold up on the sides of your container when the solution boils.Years ago my beakers looked like they were lined with gold powder after I finished with them.



> 14.When the gold is 100% dry it should be a nice light tan color, if not re-dissolve it and precipitate again with SMB.



This one could cause you to be redissolving your gold for weeks.The color of precipitated gold varies dramatically.It can look as light as melted gold,or as dark as night.There have been many cases where the gold precipitates with what appears to be "gold flakes" in it.
A couple of good rules of thumb are,
Do it right the first time and there will be no question,
and the moderators' favorite phrase....."Garbage in,garbage out."



> I use fiberglass filters



I have never used fiberglass filters,however it makes very good sense.
The fibers will not "absorb" your solution,and will not break down like tissue paper.I have some here and will be trying it soon.

EDITED


> I got some @ Home-depot. Fireplace insulation


I like this idea better.This would work better as a "plug" than traditional fiberglass.


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## philddreamer (Aug 19, 2010)

Thank you HAuCI4, but I can not take the honor. I learned it from Irons. I just worked on it 'til I had it work good for me & shared some pic's. Some one said: a pic speaks 1000 words, or something like that. :lol:


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## philddreamer (Aug 19, 2010)

Hi Mic!
I had trouble with the poping when I first started, so I tried a couple of things. First I added more water. I think I just miss understood "cover the gold" with just to the top of the gold, when in reality I could fill the beaker. :roll: I also notice that if a swirl the water when it starts to pop, it helps spread the temp all thru the bottom of the beaker & the popping stops. I think parts of the bottom get hotter that others. I get much less popping now.


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## Anonymous (Aug 19, 2010)

Very nice.I use a hot plate with a teflon coated pot on top.This helps distribute the heat and if I have an accidental tip over,I have a couple of minutes to pour it into another container.Also my primary beaker for washes is a 1000ml thick wall.It helps distribute the heat as well as give me enough volume to add plenty of extra liquid if needed.


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## lazersteve (Aug 19, 2010)

Here's some of the previous discussions on filter plugs:

Filter Plug Threads

I feel the fiberglass filter plug is the best choice for filtering dirty gold powder from the sulfuric cell, but the Charmin plug is best for nearly all other applications of the plug filtering method.

Here's some reasons why:

1. The raw material for the Charmin plug is less expensive and more widely available ( not everyone has a Home Depot down the road).

2. The Charmin plug gets all of the fine particulate the first time through.

3. You can use a fresh plug each time and are not required to 'clean' your filter medium before it can be used again.

I never plug filter gold that has been precipitated from pregnant solutions, I always let the powder settle, then decant off the liquid. The only method of filtration that I would use for clean precipitated refined gold is vacuum filtration. Solution absorption is not a problem with Charmin plugs if you filter a few mL of water through the plug before and after use.

I have used Charmin filter plugs with a variety of acidic solutions and have never had one fail or dissolve. I currently use the decanting method of separating the gold powder from my sulfuric cell runs, but when I get my hands on the right fiberglass material I'll definitely give it a try. 

I tested some pillow stuffing material I had left over from a Halloween costume with sulfuric acid and it failed with 10 seconds, so be certain you get the right stuff as all of the pillow fillings mentioned by Irons are not created equal. Lou also points out a few synthetic fibers to avoid somewhere in the old thread if I'm not mistaken.

All in all, use the material that works best your particular application. Don't get locked into a tunnel vision mindset that there is only one way. This is exactly how new methods like the fiberglass filter plug come to be. The two variations of the filter plug both have there place in the small scale refiners tool box.

Steve


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## lazersteve (Aug 19, 2010)

mic said:


> Lazersteve said:
> 
> 
> > 14.When the gold is 100% dry it should be a nice light tan color, if not re-dissolve it and precipitate again with SMB.
> ...



Sorry for the confusing terminology, I certainly hope no one got stuck in an endless refining loop due to my poor choice of words. I feel that the statement is accurate as it stands, but I also feel that the color of the precipitated gold depends on many more factors than purity alone.

I'll revise the post so that it does not leave the refiner stuck in limbo trying to obtain light tan gold powder.

Steve


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## Anonymous (Aug 22, 2010)

hi everyone! i am new to the whole refining process. has anyone tried the "sub zero" process? i am feeling very ignorant to this method. the mud and rinsing is a mystery to me. i have never seen "mud" in any form except that of dirt. i have been very excited about learning as i go but it will help to have a better clue on what i am doing-looking for.
i want to thank all of you for asking the same questions that i was having run through my head! you have given me a lot to think about!
thank you!


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## Barren Realms 007 (Aug 22, 2010)

strmchsr said:


> hi everyone! i am new to the whole refining process. has anyone tried the "sub zero" process? i am feeling very ignorant to this method. the mud and rinsing is a mystery to me. i have never seen "mud" in any form except that of dirt. i have been very excited about learning as i go but it will help to have a better clue on what i am doing-looking for.
> i want to thank all of you for asking the same questions that i was having run through my head! you have given me a lot to think about!
> thank you!



Hold off on using it and do some reading on the forum and get a copy of Hokes and start reading.


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## Barren Realms 007 (Aug 22, 2010)

It can take on many colors. 8)
















[youtube]http://www.youtube.com/watch?v=5f0boLmoSGE[/youtube]


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## hfywc (Aug 25, 2010)

Barren Realms 007 said:


> It can take on many colors. 8)
> 
> 
> 
> [youtube]http://www.youtube.com/watch?v=5f0boLmoSGE[/youtube]



the precipitate i see is similar to the second photo. now on the video, mine doesn't behave like that...when you swirl the container the precipitate easily mixed with the liquid to form dark cloud. too light to be gold dust...

also, is it normal for the smb to turn back to crystal form if the solution is undisturbed for some time or is it something else like gold salt? 

thank you for all your troubles...


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## jimdoc (Aug 25, 2010)

Don't think that it is not gold because it is too light,or looks like chocolate milk or coffee.When you melt that light brown or tan powder it melts into gold.You will have to be careful with the torch so you don't blow your gold powder out of the melting dish.Yours may appear a little different because of how much you have processed, it may be "watered down"more than the other pictures,and also how clean it is.

You can always re-refine it if it isn't pure enough first time around.So if you melt what you have now you will see what to expect.Then you will have a little button instead of the powder,and should see how pure it is from how the button looks.
Have you watched Steve's video where he melts the powder?Or any on Youtube?

Jim


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## hfywc (Aug 25, 2010)

hi jim,

thanks for a quick reply...and yes, i have watched most of the videos on steve's website. i am taking this slow because i don't want to loose anymore brown mud. i did two batches previously using a different approach in which both cases i was able to precipitate mud-like substance. because of ignorance and lack of knowledge i threw them away. thinking that it will not dissolved in nitric which it did, i mistaken it as something else. it was a considerable amount....tsk, tsk!

right now i am on a hunt for a good torch...i found a good candidate at home depot. only thing that's stopping me from buying is i don't know where i can get a refill on the fuel once the tank gets empty...

thanks again,
alan


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## jimdoc (Aug 25, 2010)

They sell mapp gas at Home Depot,that will do the job.
That is what I use,with a regular old propane torch with
the trigger igniter switch.With Steve's mini furnace it will
melt much easier.But I manage with just the melting dish
on a firebrick.

Jim


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## hfywc (Aug 25, 2010)

great! thanks jim.


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## jimdoc (Aug 25, 2010)

What did you plan on buying?The little welding setup?


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## hfywc (Aug 25, 2010)

i think it's called Port-a-torch or something and it has two metal tanks--one oxygen and the other acetylene?


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## glorycloud (Aug 25, 2010)

The oxygen will get you a hotter flame but the draw back is that
you seem go through a lot of it. That's why most folks here seem
to use the MAPP gas.

Not that I am an expert on melting gold! :lol:


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## Harold_V (Aug 26, 2010)

The melting of values by torch is best accomplished using natural gas and oxygen. Cost isn't an issue, assuming one chooses the larger cylinder sizes of oxygen. Mapp gas, by comparison, is quite expensive. 

The benefits of moving beyond the small cylinder torches is worth the effort, regardless of your fuel type. They simply do not produce the btu's that are required to make melting easy. 

Harold


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## Anonymous (Aug 26, 2010)

I use a full size oxy/acet setup.My acet. tank is about 4 feet tall,and my oxy tank is about 5 feet.I got both of them for free about 3 years ago,I filled them both for less than $50 and I have not had to refill them since.The oxy tanks are easier to come by than the acet. tanks,so if you can find one of those free or cheap get it,and if you can't find an acet. tank free or cheap,then use propane,however you will need to buy a different torch tip for about $10.
Take harolds comment to the bank.If you can find any way to use the larger bottles.....do it.


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## Rickthenewb (Sep 7, 2010)

I recently used the sulfur cell and I am not sure of my results. I combined all of my gold powder (the black stuff from rinses and cell) added equal amounts of water and HCl with tsp of sodium nitrate and add heat. The solution turned green, I then cooled and filtered. I started adding SMB and solution turned first black but now looks muddy brown. How much SMB should I add and is this the color it should be ?

Thanks in advance
rick


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## dtectr (Sep 7, 2010)

Rickthenewb said:


> I recently used the sulfur cell and I am not sure of my results. I combined all of my gold powder (the black stuff from rinses and cell) added equal amounts of water and HCl with tsp of sodium nitrate and add heat. The solution turned green, I then cooled and filtered. I started adding SMB and solution turned first black but now looks muddy brown. How much SMB should I add and is this the color it should be ?
> 
> Thanks in advance
> rick


Rick
I'm asking to learn as much as to advise so bear with me, please.
Color sounds about right. how much powder did you start with & how much SMB did you add? Were you sure all the nitric was 
gone by adding a little more HCl until no more red fumes arose before moving on to SMB?
I'm sure you already did this, but it'll keep me awake tonight if I don't ask - did you roast your cell powder before treating it?


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## Rickthenewb (Sep 8, 2010)

Hi dtechr, I started by adding the equal amounts of water and HCl to my powder (not sure how much powder there was), I added about 1.5 tsp of sodium nitrate and heated. Everything dissolved except for some mossy green looking trash floating. I filtered the solution after it cooled. At this point is was a bright green solution. I added dry SMB (at first some red fumes from the nitric did appear but then ceased. I added quite a bit of SMB because I was waiting for the solution to turn clear then black like with the auric chloride but this did not happen. The solution is muddy brown with a tint of green and tests positive for gold with stannous chloride.

thanks again.


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## dtectr (Sep 8, 2010)

Rickthenewb said:


> Hi dtechr, I started by adding the equal amounts of water and HCl to my powder (not sure how much powder there was), I added about 1.5 tsp of sodium nitrate and heated. Everything dissolved except for some mossy green looking trash floating. I filtered the solution after it cooled. At this point is was a bright green solution. I added dry SMB (at first some red fumes from the nitric did appear but then ceased. I added quite a bit of SMB because I was waiting for the solution to turn clear then black like with the auric chloride but this did not happen. The solution is muddy brown with a tint of green and tests positive for gold with stannous chloride.
> 
> thanks again.


 hey rick
been following something similar on a different thread, same topic, though. I think it was "not precipitating" or something.
Has anything begun to drop out yet?
either way - 2 different but related approaches:
Hoke says problem likely too high acid content & reccomended adding more tap water to lower ph. OR to sprinkle sodium carbonate (Arm & Hammer Super Washing Soda) a pinch at a time to lower ph.

BR 007 adds ice to his solution until container begins to sweat
Oz puts his in the freezer.
BR 007's way would change BOTH temp & ph; Oz's would change temp only - both swear by it & both should know.

if you have enough solution & want to experiment & report back - maybe divide your solution & try more than one method. don't worry - you won't lose your gold, its always there. you can always combine your individual precipitates for the melt.

THIS IS JUST AN IDEA - but since were discussing this only yesterday & today, I haven't had a chance to try these. check the other thread for more specifics, as well as be able to contact these 2 guys directly.

Just my dos centavos.


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## lazersteve (Sep 8, 2010)

Carbonate will raise the pH, not lower it, since it is a base. 

Acids lower the pH, while bases raise it.

Steve


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## qst42know (Sep 8, 2010)

> I filtered the solution after it cooled. At this point is was a bright green solution. I added dry SMB (at first some red fumes from the nitric did appear but then ceased.



Three questions.

1. Did you dilute your solution before you filtered?



> The solution is muddy brown with a tint of green and tests positive for gold with stannous chloride.



2. Your positive test is purple not some other color?

3. As I understand SMB reacts with HCL to form SO2. The red fumes were from remaining nitric but are you sure you still have some HCL in your solution?

It is possible your HCL was depleted and not available form the SO2 necessary to precipitate.


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## goldenchild (Sep 8, 2010)

lazersteve said:


> Carbonate will raise the pH, not lower it, since it is a base.
> 
> Acids lower the pH, while bases raise it.
> 
> Steve



Yes. He probably meant the normal baking soda which is bicarbonate. The one pictured can be used to clean your crucibles though


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## lazersteve (Sep 8, 2010)

goldenchild said:


> lazersteve said:
> 
> 
> > Carbonate will raise the pH, not lower it, since it is a base.
> ...



Bicarbonate is also a base.

Steve


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## dtectr (Sep 8, 2010)

lazersteve said:


> goldenchild said:
> 
> 
> > lazersteve said:
> ...


steve is right - thanks for catching that terminology snafu. that's the kind of thing that could really confuse someone who follows directions exactly.
the "ph direction" (up vs. down) terminology has been my nemesis since 7th grade chemistry. i still tell my wife to turn up the air conditioner when i want it cooler.

That being said, Hoke did suggest sodium carbonate, washing soda, to "change the ph the other direction from acidity" :lol: 8) of the solution to help drop your gold. Don't know if it works, never tried it, which i believe i stated in the post. but i could be wrong.

Washing soda has no detergents or soaps, in fact, if you switch to soap from regular laundry detergent, you must wash garments first in washing soda (sodium carbonate) only to REMOVE excess detergent to prevent permanent yellowing of your clothes.

don't know why you'd EVER need to know that, but there you are.


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## Rickthenewb (Sep 9, 2010)

ok sorry for the delay, after several days of settling the beaker has about a quarter inch of light blue on top (assuming sulfuric), then the rest of the solution is clear amber with tan mud on bottom (assuming gold) the solution still tests positive for gold. Thanx again in advance.


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## mlgdave (Feb 23, 2011)

ahh, I know where my missing 3 grams went!! I thought the really light and easily agitated mud was just that, mud, it got decanted off into my spent AR bucket. I will now decant that bucket and reprocess the sludge, will let you know if it in fact was where I now think it is! 

Im a goofnewb

mlgdave


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## jmwimw (Jun 15, 2015)

Should my gold dry and look like little pieces of chocolate?


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## 4metals (Jun 15, 2015)

You joined today, waited 8 minutes and posted a question without enough information to get a proper answer. This isn't a magician's forum! 

This thread was started for recovery of plated pins with acid peroxide, is this the process you used? We need to know what you started with and what process you used for recovery to give you a decent answer. 

If you plan on sticking around please include enough information to answer your questions properly if you expect an answer, otherwise you will not be received well. Right now you appear to be someone who does not know what he is doing, please prove me wrong with some details.


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