The white precipitate is Ag2SO4, which is poorly soluble in water, but very soluble in concentrated H2SO4. As soon as you diluted the acid, the precipitate formed. That precipitate contains most of your silver. You can either try to dissolve it into a huge amount of water, or you can put about 500 ml of distilled water and NaCl and stirr. Because the Kps (solubility product constant, Ksp (AgCl) = 1.7 x10-10) of AgCl is much smaller than that of Ag2SO4 (1.2⋅10−5), an exchange will happen as the equilibrium is displaced to form 99.99% AgCl in the precipitate. You should be able to recover your silver after that...
My favorite part is when he shows his lunch. You should have said, "I add in the 50 ml of dilute acetic acid to the 100 ml of olive oil, give it a good stir, and add it to my lunch". (acetic acid is vinegar) ps. I get the feeling he is subtly flexing on us by showing off his watch.
I had to do a Google Lens search. Omega Constellation in yellow gold? Pfft. I'm not going to wear anything on my wrist that has a higher street price than my hand! Totally feel you about the lunch.
Learning more and more every day! Thank you! You know that silver bar being stamped "reetips" is a mint error. It will be rare and sought after one day. Just subscribed to tomoko's
Interesting method, I had not thought of this approach before, thanks for sharing. . As a chemist, regarding the precipitate: I can think of two possibilities: (1) silver sulphate is actually only moderately soluble in water. (0.83 g/100 mL at 25 deg C, and only 1.33 g/100 mL at 10 deg C), and much more so in concentrated sulphuric acid. So: one possibility is that the white precipitate is silver sulphate that crashed out of solution when you diluted the sulphuric acid. In that case, your yield can be much improved by using (a lot) more water, so that all the silver sulphate stays in solution. I think this is what was meant in your textbook by 'a considerable amount' of water. Note also that without stirring, the dense sulphuric acid solution will tend to settle in a layer on the bottom, and stirring or swirling after adding all the sulphuric acid may cause the solutions to mix and heat up suddenly. I would advice stirring while pouring the sulphuric acid into the water. (2) Another possibility I can think of is that the precipitate is lead sulphate. It is soluble in concentrated sulphuric acid, but very insoluble in water or dilute sulphuric acid so it would crash out when you dilute the concentrated acid. However, I don't think lead is a common component of silver alloys, and the candleholder doesn't seem to contain many (if any) soldered joints, so the amount of precipitate you observed seems to be too much for it to be lead sulphate. So, my money is on hypothesis nr 1. Would be interesting if you could figure out what the precipitate is and let us know.
Yup. This is why the Hoke book said to dilute it in AMPLE quantity of water. Solubility in water 0.57 g/100 mL (0 °C) 0.69 g/100 mL (10 °C) 0.83 g/100 mL (25 °C) 0.96 g/100 mL (40 °C) 1.33 g/100 mL (100 °C)[2]
@@AirForce15A No... instead not enough water. the oversaturated solution when being poured into the water still resulted in a total amount of silver sulfate that was more than his 700-odd (and later 1200-odd) ml of distilled water could hold, so it precipitated out.
I was thinking the same, Silver sulfate is minimally soluble in water but highly soluble in concentrated Sulfuric acid so the solution was highly saturated.. When the acid solution was diluted, the excess Ag2SO4 crashed out of solution.
John, the misdeeds of a few ruin it for the many. I bought the concentrated sulfuric acid drain opener over the counter at Ace Hardware. Same with the lye. Sugar and sea salt at the grocery store.
Typically I make a salad dressing from Acetic Acid, Sodium Chloride, Piperine and Oleic Acid. Use a 3:1 Ratio of Oleic to Acetic Acid, then Sodium Chloride and Piperine to taste. Yummy.
Hey....long time no see. I've been sick lately, so I haven't had the energy to watch many videos that last more than a couple minutes. Your videos are so refreshing and honest. I can take seriously anything you say, because you keep a lot of BS out of your videos and stick to the subject. I love these videos, because you explain so well with being condescending or arrogant. Thank you so much for your hard work
@sreetips No thanks necessary. I think it's important to tell people how they impact you. I'm always trying to learn new things and I find your videos are a very effective tool to cut out the bloat and learn the important stuff. I've had such a difficult time focusing on any one thing because of my ADD and I find it extremely frustrating and depressing. When I need to understand a complicated chemical procedure, I want to cut to the chase, and so I turn to your videos. You are such an excellent teacher. It is a pleasure to learn from you. This is no fan boy crap, I thought it was important to let you know. I could die tomorrow for all I know
Thank you. I’d like to develop this a little more to get a good yield. I think it can get just as good yield as nitric can. Just have to tweak it some.
Great content as always! I thoroughly enjoy gaining hobbies and enjoy it even more when I can learn from others' mistakes! Thank you very much for putting your experience online!
Thanks for showing your lunch (in addition to all the interesting chemistry as usual). One of the great things about the personality you show in these videos is that you exude personal discipline.
I’m a chemistry graduate, and So the stuff that crashed out of solution was likely silver sulfate, silver sulfate is not very soluble in water, unless the water is super acidic. Upon dilution, you raised the pH, and crashed it out of solution
I solved it by not adding water. Instead I slowly added hydrochloric acid a little at a time directly to the silver sulfate solution. The chloride comes down immediately. Silver chloride is then rinsed with plenty of water to remove the acids. Then I convert the silver chloride to pure silver metal with lye and sugar. Welcome to my channel Drew. I almost failed the only chemistry class I ever took back in high school 50 years ago.
@@sreetips that would make sense, as silver chloride has such a low solubility level, even extremely acidic solutions couldn’t solvate it. I love the channel, I actually found your channel through some hobby chemistry research. Anyway, if you ever have a chemistry question, comment, or concern, I’d love to help!
The precipitate you're getting might very well be silver sulfate, which is soluble in sufuric acid, but poorly soluble in water. That's why it came out of solution when you diluted the acid. You can turn the solid silver sulfate into silver oxide just by mixing it thoroughly with sodium hydroxide the same way you did with the silver chloride.
Really? I had no idea. I just did a video on getting the silver chloride from the sulfate. It's uploading right now. If that's the case then a totally new video is in order. I'll do side by side refinings of some sterling flatware. One in nitric and one in sulfuric. Max yield from both is the goal. Oh well.
@@sreetips I am an amateur at best, but I immediately thought of what craoun said. My thinking was, the sulfuric was still 44 degrees c, when it hit the distilled water, the colder temperature combined with the fact it's water forced some silver out of solution.
2Ag + 2H2SO4 ---> Ag2SO4 + SO2 + 2H20 Ag2SO4 is hardly soluble in H20 at room temp. So that precipitate is going to be Ag2SO4. You need to heat to 100degC for a solubility of 1.33g /litre. You could thermally decompose the Silver Sulfate. Ag2SO4 + Heat ---> 2Ag + SO2 +O2
@@johnlintorn6768 i am searching for a source that can teach me the chemistry behind everything. It seems what you said is what I said, just exhibiting a much greater understanding of the material. are there any books on the subject that you've read that you felt helped everything 'click' together? I would like to start a dialogue with you about a few roadblocks I have hit. If you are interested and can provide contact information, it would be greatly appreciated
Solubility of silver sulfate is about 1 gram per 100 ml of water, 1.3 liter could hold about 10 grams which is consistent with the resulting button. Take the white salt that crashed out of the sulfuric acid and boil it in another liter of distilled water, then test it with some chloride salt. I think you will be surprised.
1.33g per 100ml at 100C. Thanks Goran, had to look it up. I figured some of the silver got hung up in that precipitate. Plus, it too is light sensitive.
@@sreetips Yep, and only 0.96 grams at 40 degrees C. That precipitate is almost 100% silver sulfate., with probably a trace of copper sulfate. Copper sulfate has a much higher solubility in water, so very little of it will precipitate during the dilution step. It might be easier to just pour off the mixed metal solution and just dump it into your stock pot. You could then continue the processing with the almost pure silver sulfate precipitate.
Thank you sreetips. In norway its not legal to own nitric acid for privat use. I really wanted to try refining silver at home and you showed me a way. Cheers.
Mrs sreetips bought $1500 worth of gold yesterday - for $485. People are clueless about gold. As long as they can keep gold price from spiking up we should be able to keep doing this. But when it gets away from them, and people begin to understand that the metal is worth more than the paper dollars, then we won’t be able to find it anymore - anywhere. A spike in gold price will put sreetips out of business!
This is a fantastic resource, thanks Sreetips, definately a thumbs up and saved to my refining playlist! Now if only there were a way to do something similar with gold... 🤔
The precipitate is silver sulfate. It's poorly soluble in cold water, about 8 g/100mL, goes way up in solubility to around 80 g/100mL in .10% molar sulfuric acid/water. Adding a small amount of sulfuric acid to the beaker and hearing it would have dissolved most of that white stuff.
Did you ever discover what the first strange precipitate was.thank you for your teachings I have studied hard and have my own lab now and am processing my gold from my lode claim I owe it to you.listen to this man if you want to learn how but you have to put in much effort and study.
When you pulled out the book to show your facts is when you had me sold. Thanks for the video. im about to refine 13.8 pounds of silver plate. ill be refering to your video alot.
I didn’t use silver plated material, I did this experiment with solid sterling silver. If you use silver plated material then the yield will be very low. My guess is not even an ounce of silver from 13.8 pounds of silver plate. Plus, a lot of toxic sulfuric acid waste that must be treated prior to disposal. Hot sulfuric is very dangerous. It will burn a hole in your skin if any gets on you. One guy reported that it makes an open wound, very deep, that doesn’t heal well even after thinking all the acid was rinsed and washed away. The risk is too high to try this on silver plate. Especially if you’re new to this. Not a good place for a beginner to start.
lol, so last year I played around with silver in nitric acid then winter came. I learned what happens when silver gets to cold when dissolved in nitric acid. I figured that sulfuric acid considering how hot it gets would give me a better result than it turning to silver Nitrate crystals,,,, I was wrong, lol, but it was fun and interesting figuring out how to fix it so now I’m done for the year till it’s warmer. Thanks sreetips!
That’s silver sulfate falling out of solution. It’s solubility in cold/room temperature water is fairly low, no where near the solubility of silver nitrate. Bringing it back up to boil should bring all that back into solution, then while it’s hot is the time to do the chloride drop. If I remember correctly the solubility at 100 degrees C is about 1.5 grams per 100ml of water. Whereas in cold water it is about 0.4 or 0.5 grams per 100ml.
Great work!! Your are hands down my favorite channel! I have literally tons of old misc electronics. I wanted to start processing stuff but I don't have a fume hood and I'm super freaked out with dealing with nitric acid. I have a liter if nitric but I have not used it yet due to not having a fume hood. I was thinking of building a tiny shed out in my backyard so I can turn it into a lab. The only thing is it get so cold in the winter months. I'm still a newbi but I'm trying really hard to be good so I want to make sure I have all my ducks in a row before continuing on. The other problem I'm having is because I'm not processing any old electronics so they keep piling up. I was wondering if by chance you could do a video to demonstrate an inexpensive way to get started?
My guess for the white precipitate on crashing with water would be silver sulfate. Sterling is usually just silver and copper and the copper sulfate is probably pushing it out of solution as the temperature drops. Hope you didn't throw it out :)
What really made me happy was doing the experiment before hand without that pesky camera looking over my shoulder. I think this made for a better video because I knew what to expect. Many of my videos are shot in the raw; you're seeing me do it for the first time ever with out any knowledge of what to expect.
This is the most backyard chemist project I've ever seen. It's cool and all and a great learning experience but I really wouldn't trust that's anywhere close to 3 9's fine... and I certainly wouldn't go around telling other people it was after the loosest refinement process I've ever seen...
I have a fun challenge for you. High purity Bismuth! Many places that sell Bismuth seem to claim 4 or even 5 9's but if you try and grow bismuth crystals they may either never form properly or be gray and dull in luster. I tried this myself and so far it seems electrolysis is an option but it is soooo slow.
Too bad you didn't weight the initial amount of metal you started from. If you aim is to recover silver, you should keep the first white precipitate... what is mainly Ag2SO4. It is possible that Ag2SO4 is quite soluble into the concentrated H2SO4 by complexation or due to the lack of water, but crashes out of solution when dilluted. Copper sulfate remains soluble and this is observed all allong your process. To me the use of NaCl to make HCl via in situ reaction with H2SO4 and precipitation of AgCl is useless... You can start immediately from demi-water washed solid Ag2SO4 to the next step. Ag2SO4 (s) + 2 NaOH (aq) --> 2 AgOH (s) + Na2SO4 (aq) 2AgOH (s) --> Ag2O + H2O (via heating) C6H12O6 + Ag2O --> 2 Ag + C6H12O7 (gluconic acid as Na gluconate) (via heat and basic NaOH media). I hope this will help you increase the yield, efficiency and reduce the wastes. PHZ (PHILOU Zrealone)
That is a good reply. I am trying to figure out a process where I can use easily available chemicals for recovering some silver plate. You say the copper sulphate remains soluble and this is observed all along your process. How is that being observed? In your method you say.... 2AgOH (s) --> Ag2O + H2O (via heating). Do you simply melt the solid with heat and the water comes off as water vapour? From reading your reaction I guess that is what the process is. I presume the silver oxide could then be added to the silver oxide he precipitated out from the rest of his solution before the conversion to silver metal so all of the silver is recovered. I am wondering if the sulphuric acid and silver reaction would work if the sulphuric acid was less concentrated? I have about 10 litres of sulphuric acid I recovered from scrap batteries and wondering if I can use it. I realised this morning I have a battery hydrometer so can measure its density and maybe give me a clue of its concentration.
@@parcydwr Hi Robert Smith, thank you. The Cu (copper sulfate - CuSO4.xH2O is blue like Cu(2+) what is dissolved ion (into water)... the dehydrated form is white and recolor blue as soon as it catches moisture from the air or liquid water). That color is observed into Sreetips video process into the collecting "recycling" drum. Copper is often joined to Silver to make harder and cheaper alloys. Silver and copper are two "precious" or "near precious" metals and they display a special property to have a high oxydation (électro-)potential... as such they oxydise their ion against glucose if hot and in presence of a base (oxydoredox potential can express in acidic (H(+)) media or basic (OH(-)) with different processes and results... In the present case copper sets a characteristic precipitate of Cu2O red (or sometimes a copper mirror) and silver a characteristic mirror or grey powder. In general aldehydes (reductible) can react to form the related acid... here gluconic acid. Ag(+) + 1e(-) --> Ag(0) (silver mirror or dust) Cu(2+) + 1e(-) --> Cu(1+) (like into Cu2O see Fehling test for sucrose/aldoses) Cu(1+) + 1e(-) --> Cu(0) HO-CH2-CHOH-CHOH-CHOH-CHOH-CH=O --> HO-CH2-CHOH-CHOH-CHOH-CHOH-C(=O)-OH (here only the aldehyd group is oxydised to a carboxylic one and it passes from +1 oxydation state to +3 oxydation state) The AgOH turns into Ag2O suspension/precipitate from "maturation" (concentration and heat of solution). Paradoxaly Ag2O is specifical as it is not wel linked to its oxygen and it will set it free upon heating to live "native" silver and pure oxygen... this happens also with Gold whose oxide is also unstable and even explosive (set O2 free explosively from heat). 2 Ag2O -heat-> 2 Ag2 + O2(g) I will reply a bit further/deeper later about the process of Sreetips soon. PHZ (PHILOU Zrealone from the Science Madness forum)
White precipitate when you dissolved silver in sulfuric acid is silver sulfate, it is slightly soluble in water. Silver hydrogen sulfate was soluble in sulfuric acid but when you diluted, equilibrium shifts and almost insoluble silver sulfate is formed so you technically discarded most of the silver.
@@jameseves9209 Nothing. Simply do not use sulfuric acid. Use nitric acid and precipitate silver with copper metal. You can recycle both copper metal and nitric acid from Cu(NO3)2 byproduct with sulfuric acid and aluminum metal. Also, this way of getting silver from silver chloride is not very efficient. It's much better to put sodium hydroxide with silver solution to precipitate silver hydroxide which turns to oxide and then pure silver, when heated. But here you cannot do it because raw silver contains base metals like copper so hydroxide will be contaminated so best way is definitely precipitating Ag with Cu from AgNO3/Cu(NO3)2 mixture when you dissolve raw silver in nitric acid
I'm pretty sure that the silver sulfate that is created during the dissolving in sulphuric acid, and when you add heat the sulfate sheds the sulfur molecule, and then when added back to distilled water, it absorbs the oxygen molecule, becoming a silver oxide, which in turn is heavier than water. Then settles out in the water, if you were to have set the solution aside for 48 hours or so, more silver would have made the chemical shift to oxide from sulfide, and slowly develop a sulfur oxide on the surface of the water.
Well, I gave this refining processes a go. I also ended up with ALLOT of Silver Sulfate. Also of note, in the bottom of the beaker with boiling Sulfuric Acid and Silver, a black cement formed, that cemented a stir bar fast to the bottom of the beaker. I had to use some heavy duty, needle nose pliers to break it up. My solution is cooled and settling over night. The "Silver Cell", your engineering, is Percolating really well. I just started it this afternoon and I already have a really nice accumulation of Silver Crystal's forming on the Cathode! Completely Awesome. The black, very dense, cement that formed, will fill my burn cup, probably 4 times, altogether. I figured that I'd melt it into metal, and, then test it, to see what in creation it is. I did notice a redish blush, in the Sulfuric Acid I used, that was not present in yours. Maybe an, "Unknown" chemical slipped in. I used pure Sulfuric Acid, so I really am a little stumped. I'll burn it tomorrow and let you know what I've got. Another good purchase, on another flatware set today. Sterling Silver. This time it was a bit more dear, to the tune of 2K. Worth it though. A little over 10 pounds, English Standard weight. My digital scales haven't arrived yet. The only thing that is a pain, with both sets, recently purchased. The blades on the knives, cake server and butter knife, all have Stainless blades and the tang of the blade, running up into the handle! What a pain! Great Grandma's are completely Sterling Silver, even the blades. Lost a bit of weight there; but, still worth it. Your presentation of the face value of a quarter versus it value in the Silver it was made from, really reverberated! That is a very good method for the explanation of the value of Precious Metals against our printed currency. With this current administration.... Woops! Sorry! We don't do "Politics"! You have a pleasant evening. Thank you again for reigning, dormant grey matter, that is now crunching equations again! It feels great and is fun and is, (with the element of possible catastrophic disaster, explosions and other neat stuff), really exciting! Wade
Still don't know what the original black cement is. 3 Map gas torches and the cutting head on my OXYACETALYNE rig. Just won't melt! Incredible! So much heat was being produced, it warped my ¼ inch Steel burn table! Going to add a 2nd OXYACETALYNE torch to what I've already tried. If that doesn't melt it, I'll try the Kiln....... Never had the Kiln as hot as all the gas torchs combined, produced. One way or another, it's going to melt, (Or I'll go out in a BLAZE OF GLORY)!...... Well, hopefully not. Guessing that I'll find out!
You sure come up with some great ideas. What a sweet wee bar.I must have had at least a dozen new subs mentioning you sent them today and a bunch over the last week since your last post. Thank you very much my dear friend.
XRF would give you a definitive answer, but that white precipitate has to be either (1) a contaminant in your sulfuric acid, or (2) a salt of one of the metals from your sterling, so a silver, copper, tin, etc sulfate / oxide/ hydrate. Likely contaminants in drain cleaner sulfuric acid include a corrosion inhibitor like Rhodine 31A, which can crash out when neutralized (you might try pouring a few mL of the acid into 10 mL of water and see if you get a similar precipitate volume). Silver sulfate is a white salt that is barely soluble in neutral water (1.3g/100mL at 100C), but it's light sensitive like silver nitrate, and the missing silver's mass would show up if you can get a yield on one of those runs. Most copper sulfates are vivid blue and highly soluble. Tin, nickel, cadmium, or zinc sulfates all seem too soluble (33g/100mL, 65g/100mL, 76g/100mL, and 57g/100mL respectively). A tin or zinc oxide seems like a possibility too, depending on the sterling.
Start small to get the feel for it. Resist the urge to go all in with a hundred grams of karat gold. Instead start with just five grams to see how it goes.
The precipitate is silver sulphate powder. Silver sulphate is insoluble in water and the dilutuon of silver sulphate and sulfuric acid in water causes the silver sulphate to precipitate out somewhat.
I believe the Silver is on the bottom at when you poured the silver nitrate and copper nitrate into distilled water. Since it's more heavy weight than copper and water. When molecule weight is higher than 100. The molecules as Silver of 107 are heavy weighting. Copper will just float in the water. The ending result gets blue color as only copper. But as copper and silver in nearly same is like the same as green and blue. But silver in bottom make only copper look blueish, when copper is green with Silver. But both can make either what they represent. So green solution has more likely copper and silver. But both can be sometimes either blue or green. But what Silver acts as color is gray. As in the second solution with the mixer. You don't know it before you pour copper and silver which is used as alloy together. There is actual strange difference in the color blue and green. Both don't make yellow color. But they make their dark green and dark black blue which in logic can't make yellow. But as soon it either is blue or green dark. Having only darker colors. You should try as well to find out easiest way for copper refining. Many people would be interested in 100% output refining. You nearly where there. So best solution is really to take out the water of blue into other compartment. As silver lies in the bottom. What you had when you first dissolved with sulfuric acid was platina and in the bottom as very darkish collection. Might as well be titanium or other metals as gold. But palladium is clearly short the same molecule weight. Since nature make palladium first as halving to Silver. If there is no escape of energy palladium stays in the mountain. It is short lived. The molecule weight represents important information. I believe you know much. But you might not know everything yet?
FYI -- Sea salt does contain SOME iodine although less than iodized salt. As for the precipitate, "Sterling silver is prone to tarnishing,[1][2] and elements other than copper can be used in alloys to reduce tarnishing, as well as casting porosity and firescale. Such elements include germanium, zinc, platinum, silicon, and boron." So possibly you are seeing one of these other materials, like silicon, boron or zinc compounds precipitating out, but I am not sure of their solubilities in concentrated versus dilute (~20%v/v) sulfuric acid. One suggestion for saving cash, buy bulk paper coffee filters, great for initial filtering and work really well with buchner funnels.
I had not ever though of using coffee filter in the Büchner funnel - that's a great idea. I believe that the precipitate is merely silver sulfate. To get the silver I'll dissolve it (the silver sulfate) in boiling water then add the salt while its still boiling, before it has a chance to cool down and precipitate as silver sulfate again.
The white sediment could be zinc sulfate. Stirling silver is an alloy about 90 % silver and 10 % of copper, nickel or zinc. Possibly others. The blue/green is probably copper sulfate II I think.
That white precipitate is silver sulfate ;). It tends to only wan't to dissolve in concentrated H2so4, once diluted with water the solubility goes down.
Your solution was over saturated and silver sulfate is practically insoluble in water. It is soluble in hot sulfuric acid but again, over saturated with the cooling and further cooling and diluting helped it crystallize out.
Jimmy, 1.33g per 100ml water at 100C. I had to look it up. It'll dissolve in hot water. Then add the sodium chloride to the hot solution to get the rest of the silver. Brilliant!
Its silver sulfate witch in water is insoluble, but when in a highly concentrated solution of sulfuric acid probably of 98% or higher the silver will react and dissolve since there is almost no water present. then when you poured that solution into the water the silver sulfate crashed out because the ph becomes to high for it to remain dissolved.
I know Sreetips said this here but be very, VERY careful with boiling 98% (any concentration really)Sulfuric Acid. It’ll scold and dissolve skin very, very fast. It’s boiling point is over 600F, which can be very deceiving. It’s like pouring molten lead on your skin with the added effect of dissolving everything it touches very fast. That Rooto brand Sulfuric Acid is the good stuff. Nice and clear, possibly no iron passivates or organic compounds. You could make some very pure nitric acid with nitrate salts using it, like 99% fuming. It’s not really good for refining due to the extreme chance of runaway, but I’ve never tried it. Thanks for showing that brand of drain cleaner, my local hardware store has it in gallons for $26.
It about the same here, used to be about $15 per gallon back in 2010 when I first started. Has it become that much more valuable? Or has the currency lost that much value?
A shortcut I'm experimenting with right now is adding Spectricide stump remover (100% Potassium Nitrate) to the sulfuric acid solution and heating it. The mixture creates nitric acid in-situ and seems to dissolve the metal (copper and silver out of scrap jewelry) exactly like commercial nitric acid. So far, so good. We'll see how the potassium bisulfate follows the silver through the process and if it messes up the silver or gold. Perhaps you'd like to try this experiment with your setup.
I’ve never tried this, but if it works and everything dissolves (have to filter out solids with a micro fiber glass filter due to sulfuric with dissolve a paper filter) then the silver can be precipitated by adding hydrochloric acid (carefully because it reacts violently with sulfuric) to precipitate out the silver chloride. Then the silver chloride can be converted to pure silver with lye and sugar.
The problem with dumping the sea salt in without dissolving in water first is that it will also force precipitation of some of the copper sulfate. Also, once the silver chloride is precipitated, you should test the blue liquid to make sure all the silver has been precipitated.
It would be nice that you put in the video description the chemical formulae for those products. In the EU we don't have the same BRANDS but maybe we have the same chemicals in a different brand. In case you have 2 minutes of free time to teach me, I'll be happy to learn :)
Sugar ; self explanatory Lye ; caustic soda or sodium hydroxide sulphuric acid; also known as battery acid. seasalt is also table salt but without iodine.
That precipitate may be one of the Copper Chlorides. Sterling contains Copper, possibly Lead. There is a 999 Dusan video where he shows that one of the Copper Chlorides is soluble in concentrated acid, but merely diluting the acid, (greatly), with distilled Water, caused the Copper Chloride to precipitate out because that compound is much less soluble in dilute acid. Its solubility probably drops off logarithmicaly with the decrease in concentration. In the video by Dusan, the Copper compound was white, or very white-ish. Any Lead in there might exhibit a similar behavior.
I've already determined that it's silver sulfate. And that it can be converted to silver oxide with lye just like silver chloride. Bummer. I just made a new video showing how to get the chloride from the sulfate. Obsolete before it even gets published.
Hello Sreetips I think if you added some Potassium Nitrate (Stump Remover) to the solution it will work a lot like Nitric acid. I tried it once before sourcing Nitric and it worked pretty well.
@@sreetips i was wondering that myself. The conversion of sulfate to oxide probably goes faster than chloride due to the slightly more soluble sulfate. Maybe not, but it doesnt surprise me at all that the sulfate can also be converted with the lye/sugar method
It's silver that crashed out in the cold water. Silver is less soluble in the colder temp. I'm really just guessing. I'm not a chemist but I watch every video you come out with. I pay attention
@ 11:50 = "if any of you chemists know what's going on here..." - most obliged, Sir... The thing is, silver sulphate, Ag2SO4, is just marginally soluble in water, but quite soluble in H2SO4, even at lower concentrations. A 100 mL of pure water @ 25°C (77°F) can dissolve just 0.83 g of Ag2SO4 (and it doesn't change much with temperature), while 100 mL of 0.1 mol H2SO4 at the same temperature can dissolve as much as 31.56 g of (if my quick calculations are correct, 0.1 m H2SO4 is approx. 10% solution). Specifically, Auntie Wiki says: Solubility in water 0.57 g/100 mL (0 °C) 0.69 g/100 mL (10 °C) 0.83 g/100 mL (25 °C) 0.96 g/100 mL (40 °C) 1.33 g/100 mL (100 °C) Solubility in sulfuric acid of 8.45 g/L strength (0.1 mol H2SO4/L H2O) 25.44 g/100 g (13 °C) 31.56 g/100 g (24.5 °C) 127.01 g/100 g (96 °C) So, the difference is huge - which means that diluting remaining (unreacted) acid (as far as I can tell, the reaction was done with a huge excess of H2SO4) will inevitably result in precipitating of Ag2SO4. About "splattering everywhere" (a minute or so earlier in the video) - as you probably know, mixing concentrated sulphuric acid with water is VERY exothermic, and if you do it too quickly and/or in large quantities it can even lead to boiling of the mixture (which is to be avoided). So if one pours a very hot (around 100°C) and still pretty concentrated H2SO4 into water it will heat the water almost instantly above its boiling point, and splattering will be the result. BTW, that H2SO4/H20 "reaction" is so exothermic that "hyper-concentrated" H2SO4, often referred to as "oleum" (a shortening of oleum vitrioli, not to be confused with oleum dulci vitrioli, which is diethyl ether, while oleum vitrioli is a solution of SO3 in 100% H2SO4) must not, EVER, be mixed directly with water - one has to dilute it first with concentrated H2SO4. And it goes without saying that thick rubber gloves, elbow length, with a second (lighter) pair underneath is a must in handling that devil in a bottle. And so is full face mask AND goggles - and some respiratory protection IN ADDITION to fume hood is highly recommended. And, while I'm here... I'm always... say, "amused" by that mismatch of your nearly quantitative analysis precision in precipitating precious metals and then blowing at them with strong stream of gases from oxyacetylene torch - it's just... it just doesn't make any sense to me. A good small second-hand electric furnace would cost probably much less that all that gold and platinum dust blown off in all those melts to date. Just saying... ;-) Cheers, KB
I cut my teeth with fused silica melt dish and oxy/acet torch. Learned it from the pros on the goldrefiningforum.com you don't have to be a chemist to be a refiner. But it probably helps.
@@sreetips Of course, you don't have to be a chemist to be a refiner, but yes - a good understanding of all those reactions and processes does help a bit. Still, with applied chemistry, hands-on experience and knowledge of all those "tricks of trade" are just as important. Like, quartering gold with silver - AFAIK there's nothing really in "chemistry knowledge base" about why one should stick to a certain proportions of those metals to get just the right size of particles of gold "mud" - i.e. just fine enough, but not too fine. And yes, I agree - old timers and pros of the trade have their own paths, well trodden... Still, innovation and improvement comes from challenging all those "old and established" truths and practices. But hey, who am I to tell you how to refine (and melt) your gold... ;-) Best, KB
The white precipitate is Ag2SO4, which is poorly soluble in water, but very soluble in concentrated H2SO4. As soon as you diluted the acid, the precipitate formed. That precipitate contains most of your silver. You can either try to dissolve it into a huge amount of water, or you can put about 500 ml of distilled water and NaCl and stirr. Because the Kps (solubility product constant, Ksp (AgCl) = 1.7 x10-10) of AgCl is much smaller than that of Ag2SO4 (1.2⋅10−5), an exchange will happen as the equilibrium is displaced to form 99.99% AgCl in the precipitate. You should be able to recover your silver after that...
This looks like a good way of handling it. Just add the salt without decanting and let the alchemy do the work.
What would the happen if there was copper in that solution? How would you handle that?
@@lukebaehr3851 There was copper in solution
What about mixing the AgSO4 directly with NaOH and do the procedure like it was AgCl ?
That might work
My favorite part is when he shows his lunch. You should have said, "I add in the 50 ml of dilute acetic acid to the 100 ml of olive oil, give it a good stir, and add it to my lunch". (acetic acid is vinegar)
ps. I get the feeling he is subtly flexing on us by showing off his watch.
I had to do a Google Lens search. Omega Constellation in yellow gold? Pfft. I'm not going to wear anything on my wrist that has a higher street price than my hand! Totally feel you about the lunch.
Flexing...😂😂😂😂
@@AppliedCryogenics Work in the cryogenic industry?
I been watching you for many years!🙂 You Sir are the Bruce Lee of precious metal recovery💪🏅🏅🏅🏅🏅🏆 Thank you so much for all you do!🙏
Learning more and more every day! Thank you! You know that silver bar being stamped "reetips" is a mint error. It will be rare and sought after one day. Just subscribed to tomoko's
Interesting method, I had not thought of this approach before, thanks for sharing.
. As a chemist, regarding the precipitate: I can think of two possibilities:
(1) silver sulphate is actually only moderately soluble in water. (0.83 g/100 mL at 25 deg C, and only 1.33 g/100 mL at 10 deg C), and much more so in concentrated sulphuric acid. So: one possibility is that the white precipitate is silver sulphate that crashed out of solution when you diluted the sulphuric acid. In that case, your yield can be much improved by using (a lot) more water, so that all the silver sulphate stays in solution. I think this is what was meant in your textbook by 'a considerable amount' of water.
Note also that without stirring, the dense sulphuric acid solution will tend to settle in a layer on the bottom, and stirring or swirling after adding all the sulphuric acid may cause the solutions to mix and heat up suddenly. I would advice stirring while pouring the sulphuric acid into the water.
(2) Another possibility I can think of is that the precipitate is lead sulphate. It is soluble in concentrated sulphuric acid, but very insoluble in water or dilute sulphuric acid so it would crash out when you dilute the concentrated acid. However, I don't think lead is a common component of silver alloys, and the candleholder doesn't seem to contain many (if any) soldered joints, so the amount of precipitate you observed seems to be too much for it to be lead sulphate.
So, my money is on hypothesis nr 1. Would be interesting if you could figure out what the precipitate is and let us know.
Is it Possible to do this same process with old PCB's?
Silver sulfate
I'd need a fume hood if I ate that many raw veggies at one time.
If you just get rid of the cheese you will be eating completely healthy.
@@scottcampbell7944 Uhuh sure!
This is the best comment ever
The white precipitate is silver sulfate, as the concentration of your solution was oversaturated👍🏻
Yup. This is why the Hoke book said to dilute it in AMPLE quantity of water.
Solubility in water
0.57 g/100 mL (0 °C)
0.69 g/100 mL (10 °C)
0.83 g/100 mL (25 °C)
0.96 g/100 mL (40 °C)
1.33 g/100 mL (100 °C)[2]
So your saying there was too much water used?
@@AirForce15A No... instead not enough water. the oversaturated solution when being poured into the water still resulted in a total amount of silver sulfate that was more than his 700-odd (and later 1200-odd) ml of distilled water could hold, so it precipitated out.
@Frank Roberts I thought he checked it for copper with 10% amonia is this an unreliable method to test for copper sulfate?
I was thinking the same, Silver sulfate is minimally soluble in water but highly soluble in concentrated Sulfuric acid so the solution was highly saturated..
When the acid solution was diluted, the excess Ag2SO4 crashed out of solution.
I’m glad you have made this video for us that don’t have a lot of access to nitric acid and all the equipment. Great video Streetips
But most of us who don't have access to nitric acid don't have access to sulphuric acid either.
John, the misdeeds of a few ruin it for the many. I bought the concentrated sulfuric acid drain opener over the counter at Ace Hardware. Same with the lye. Sugar and sea salt at the grocery store.
@@sreetips But I'm in the UK, you cant bye anything stronger then piss without a licence.
@@snipersquad100 Hi John, you can buy 96% Drain cleaner in the UK
@@peterwilliams5631 Where Peter?
Typically I make a salad dressing from Acetic Acid, Sodium Chloride, Piperine and Oleic Acid. Use a 3:1 Ratio of Oleic to Acetic Acid, then Sodium Chloride and Piperine to taste. Yummy.
Hey....long time no see. I've been sick lately, so I haven't had the energy to watch many videos that last more than a couple minutes.
Your videos are so refreshing and honest.
I can take seriously anything you say, because you keep a lot of BS out of your videos and stick to the subject.
I love these videos, because you explain so well with being condescending or arrogant.
Thank you so much for your hard work
Thank you
@sreetips No thanks necessary. I think it's important to tell people how they impact you.
I'm always trying to learn new things and I find your videos are a very effective tool to cut out the bloat and learn the important stuff. I've had such a difficult time focusing on any one thing because of my ADD and I find it extremely frustrating and depressing.
When I need to understand a complicated chemical procedure, I want to cut to the chase, and so I turn to your videos. You are such an excellent teacher. It is a pleasure to learn from you.
This is no fan boy crap, I thought it was important to let you know. I could die tomorrow for all I know
You are my teacher I most respect you, and God bless you. Thanks for this video.
Thank you. I’d like to develop this a little more to get a good yield. I think it can get just as good yield as nitric can. Just have to tweak it some.
Great content as always! I thoroughly enjoy gaining hobbies and enjoy it even more when I can learn from others' mistakes! Thank you very much for putting your experience online!
Thanks for showing your lunch (in addition to all the interesting chemistry as usual). One of the great things about the personality you show in these videos is that you exude personal discipline.
And discipline is key to achieving success.
A man that owns a hard copy of Refining precious metal wastes by C.M Hoke is a hero IMHO.
calm morrison hoke? want a copy?
The only problem with the hard cover of that book is by the time you refine enough gold to afford it you won’t need it anymore
@@bencapobianco2045 a digital copy
Love the skull and crossbones on the sugar🤣🤣👍. As Mary Poppins says" a spoonful of sugar makes the silver fall down, the sugar fall down"
Works with Karo syrup too.
Probably has it on there so it is no longer considered "food grade" as it has been used in an environment where it can get contaminated.
I’m a chemistry graduate, and So the stuff that crashed out of solution was likely silver sulfate, silver sulfate is not very soluble in water, unless the water is super acidic. Upon dilution, you raised the pH, and crashed it out of solution
I solved it by not adding water. Instead I slowly added hydrochloric acid a little at a time directly to the silver sulfate solution. The chloride comes down immediately. Silver chloride is then rinsed with plenty of water to remove the acids. Then I convert the silver chloride to pure silver metal with lye and sugar. Welcome to my channel Drew. I almost failed the only chemistry class I ever took back in high school 50 years ago.
@@sreetips that would make sense, as silver chloride has such a low solubility level, even extremely acidic solutions couldn’t solvate it. I love the channel, I actually found your channel through some hobby chemistry research. Anyway, if you ever have a chemistry question, comment, or concern, I’d love to help!
Excellent Drew, thank you
The precipitate you're getting might very well be silver sulfate, which is soluble in sufuric acid, but poorly soluble in water. That's why it came out of solution when you diluted the acid. You can turn the solid silver sulfate into silver oxide just by mixing it thoroughly with sodium hydroxide the same way you did with the silver chloride.
Really? I had no idea. I just did a video on getting the silver chloride from the sulfate. It's uploading right now. If that's the case then a totally new video is in order. I'll do side by side refinings of some sterling flatware. One in nitric and one in sulfuric. Max yield from both is the goal. Oh well.
@@sreetips Very nice! I'm looking forward to seeing how it turned out!
@@sreetips I am an amateur at best, but I immediately thought of what craoun said. My thinking was, the sulfuric was still 44 degrees c, when it hit the distilled water, the colder temperature combined with the fact it's water forced some silver out of solution.
2Ag + 2H2SO4 ---> Ag2SO4 + SO2 + 2H20
Ag2SO4 is hardly soluble in H20 at room temp. So that precipitate is going to be Ag2SO4. You need to heat to 100degC for a solubility of 1.33g /litre.
You could thermally decompose the Silver Sulfate. Ag2SO4 + Heat ---> 2Ag + SO2 +O2
@@johnlintorn6768 i am searching for a source that can teach me the chemistry behind everything. It seems what you said is what I said, just exhibiting a much greater understanding of the material. are there any books on the subject that you've read that you felt helped everything 'click' together? I would like to start a dialogue with you about a few roadblocks I have hit. If you are interested and can provide contact information, it would be greatly appreciated
I keep watching your videos and I sure appreciate this. I'm so glad you put these out there. I'm learning a lot. I'll be doing it real soon.
Solubility of silver sulfate is about 1 gram per 100 ml of water, 1.3 liter could hold about 10 grams which is consistent with the resulting button.
Take the white salt that crashed out of the sulfuric acid and boil it in another liter of distilled water, then test it with some chloride salt. I think you will be surprised.
1.33g per 100ml at 100C. Thanks Goran, had to look it up. I figured some of the silver got hung up in that precipitate. Plus, it too is light sensitive.
I was wondering if it it was super saturated silver basically lol
@@sreetips Yep, and only 0.96 grams at 40 degrees C. That precipitate is almost 100% silver sulfate., with probably a trace of copper sulfate. Copper sulfate has a much higher solubility in water, so very little of it will precipitate during the dilution step.
It might be easier to just pour off the mixed metal solution and just dump it into your stock pot. You could then continue the processing with the almost pure silver sulfate precipitate.
Oh man the lunch looks AWESOME! MAKING ME hungry!
I really like the little things you do in your videos to show a personal side to all of the things you do. Keep it up, Sreetips!
Thank you sreetips. In norway its not legal to own nitric acid for privat use. I really wanted to try refining silver at home and you showed me a way. Cheers.
You have to wonder WHO was THE 1st one to figure out this process.Metal into a liquid with common items.Kinda makes you want to hit the yard sales.
Mrs sreetips bought $1500 worth of gold yesterday - for $485. People are clueless about gold. As long as they can keep gold price from spiking up we should be able to keep doing this. But when it gets away from them, and people begin to understand that the metal is worth more than the paper dollars, then we won’t be able to find it anymore - anywhere. A spike in gold price will put sreetips out of business!
Cool video REETIPS! Thanks for sharing that process with us. Aloha😉
the white precipitate is silver sulfate, which does not well disolve in water.
Got it, I'll redissolve it in sulfuric acid, then pour it into more water to get more of the silver. Thank you!
This is a fantastic resource, thanks Sreetips, definately a thumbs up and saved to my refining playlist! Now if only there were a way to do something similar with gold... 🤔
The precipitate is silver sulfate. It's poorly soluble in cold water, about 8 g/100mL, goes way up in solubility to around 80 g/100mL in .10% molar sulfuric acid/water. Adding a small amount of sulfuric acid to the beaker and hearing it would have dissolved most of that white stuff.
Add a little sulfuric, I'll have to make a note of that thank you.
Did you ever discover what the first strange precipitate was.thank you for your teachings I have studied hard and have my own lab now and am processing my gold from my lode claim I owe it to you.listen to this man if you want to learn how but you have to put in much effort and study.
Yes, it was silver sulfate. Just add hydrochloric to silver sulfate and it turns to silver chloride - like magic!
You obviously live healthy may you have a long life I learn a lot from you this is a great Channel
Thank you!
This looks like one to try. Thank you! 👍🏻🍺
I agree! Need to go to the grocery store for some lunch supplies. Good video👍
Won’t sea salt have trace iodine in it? I would think kosher salt would be closer to being just NaCl.
When you pulled out the book to show your facts is when you had me sold. Thanks for the video. im about to refine 13.8 pounds of silver plate. ill be refering to your video alot.
I didn’t use silver plated material, I did this experiment with solid sterling silver. If you use silver plated material then the yield will be very low. My guess is not even an ounce of silver from 13.8 pounds of silver plate. Plus, a lot of toxic sulfuric acid waste that must be treated prior to disposal. Hot sulfuric is very dangerous. It will burn a hole in your skin if any gets on you. One guy reported that it makes an open wound, very deep, that doesn’t heal well even after thinking all the acid was rinsed and washed away. The risk is too high to try this on silver plate. Especially if you’re new to this. Not a good place for a beginner to start.
lol, so last year I played around with silver in nitric acid then winter came. I learned what happens when silver gets to cold when dissolved in nitric acid. I figured that sulfuric acid considering how hot it gets would give me a better result than it turning to silver Nitrate crystals,,,, I was wrong, lol, but it was fun and interesting figuring out how to fix it so now I’m done for the year till it’s warmer. Thanks sreetips!
You need to do a chess set that one side is pure silver and the other is pure gold.
One side pure silver. The other side is 25% pure gold alloyed with 75% streling silver. Then encrusted with gem stones.
@@sreetips The silver king weighs 10 troy oz. plus gems, etc. Gothic-style.
That’s silver sulfate falling out of solution. It’s solubility in cold/room temperature water is fairly low, no where near the solubility of silver nitrate. Bringing it back up to boil should bring all that back into solution, then while it’s hot is the time to do the chloride drop. If I remember correctly the solubility at 100 degrees C is about 1.5 grams per 100ml of water. Whereas in cold water it is about 0.4 or 0.5 grams per 100ml.
Video of this exact process uploading as I write.
Great work!! Your are hands down my favorite channel! I have literally tons of old misc electronics.
I wanted to start processing stuff but I don't have a fume hood and I'm super freaked out with dealing with nitric acid.
I have a liter if nitric but I have not used it yet due to not having a fume hood.
I was thinking of building a tiny shed out in my backyard so I can turn it into a lab.
The only thing is it get so cold in the winter months. I'm still a newbi but I'm trying really hard to be good so I want to make sure I have all my ducks in a row before continuing on. The other problem I'm having is because I'm not processing any old electronics so they keep piling up.
I was wondering if by chance you could do a video to demonstrate an inexpensive way to get started?
I don’t process much electronics for precious metals. The yields are too low.
Those loafers are hella nice Mr. Tips
Those are my initials! A.K.
Thank you sir! That was a very nice video, maybe one of your best in my book. All the filming and editing you do for us, thanks once more.
I literately go tp sleep watching your videos
Thank you sir
My guess for the white precipitate on crashing with water would be silver sulfate. Sterling is usually just silver and copper and the copper sulfate is probably pushing it out of solution as the temperature drops. Hope you didn't throw it out :)
Video on it uploading right now.
Sreetips.. This video really perked you up!
Glad to see you enjoying your hobby at a joyful level again!
Don’t make me worry 😉
✌️PT
What really made me happy was doing the experiment before hand without that pesky camera looking over my shoulder. I think this made for a better video because I knew what to expect. Many of my videos are shot in the raw; you're seeing me do it for the first time ever with out any knowledge of what to expect.
This is the most backyard chemist project I've ever seen. It's cool and all and a great learning experience but I really wouldn't trust that's anywhere close to 3 9's fine... and I certainly wouldn't go around telling other people it was after the loosest refinement process I've ever seen...
Three nines - I guarantee it because I refined it
I have a fun challenge for you. High purity Bismuth!
Many places that sell Bismuth seem to claim 4 or even 5 9's but if you try and grow bismuth crystals they may either never form properly or be gray and dull in luster.
I tried this myself and so far it seems electrolysis is an option but it is soooo slow.
Sorry, I don’t know anything about bismuth.
Too bad you didn't weight the initial amount of metal you started from.
If you aim is to recover silver, you should keep the first white precipitate... what is mainly Ag2SO4.
It is possible that Ag2SO4 is quite soluble into the concentrated H2SO4 by complexation or due to the lack of water, but crashes out of solution when dilluted. Copper sulfate remains soluble and this is observed all allong your process.
To me the use of NaCl to make HCl via in situ reaction with H2SO4 and precipitation of AgCl is useless...
You can start immediately from demi-water washed solid Ag2SO4 to the next step.
Ag2SO4 (s) + 2 NaOH (aq) --> 2 AgOH (s) + Na2SO4 (aq)
2AgOH (s) --> Ag2O + H2O (via heating)
C6H12O6 + Ag2O --> 2 Ag + C6H12O7 (gluconic acid as Na gluconate) (via heat and basic NaOH media).
I hope this will help you increase the yield, efficiency and reduce the wastes.
PHZ (PHILOU Zrealone)
That is a good reply.
I am trying to figure out a process where I can use easily available chemicals for recovering some silver plate. You say the copper sulphate remains soluble and this is observed all along your process. How is that being observed?
In your method you say.... 2AgOH (s) --> Ag2O + H2O (via heating). Do you simply melt the solid with heat and the water comes off as water vapour? From reading your reaction I guess that is what the process is. I presume the silver oxide could then be added to the silver oxide he precipitated out from the rest of his solution before the conversion to silver metal so all of the silver is recovered.
I am wondering if the sulphuric acid and silver reaction would work if the sulphuric acid was less concentrated? I have about 10 litres of sulphuric acid I recovered from scrap batteries and wondering if I can use it. I realised this morning I have a battery hydrometer so can measure its density and maybe give me a clue of its concentration.
@@parcydwr
Hi Robert Smith, thank you.
The Cu (copper sulfate - CuSO4.xH2O is blue like Cu(2+) what is dissolved ion (into water)... the dehydrated form is white and recolor blue as soon as it catches moisture from the air or liquid water).
That color is observed into Sreetips video process into the collecting "recycling" drum.
Copper is often joined to Silver to make harder and cheaper alloys.
Silver and copper are two "precious" or "near precious" metals and they display a special property to have a high oxydation (électro-)potential... as such they oxydise their ion against glucose if hot and in presence of a base (oxydoredox potential can express in acidic (H(+)) media or basic (OH(-)) with different processes and results...
In the present case copper sets a characteristic precipitate of Cu2O red (or sometimes a copper mirror) and silver a characteristic mirror or grey powder.
In general aldehydes (reductible) can react to form the related acid... here gluconic acid.
Ag(+) + 1e(-) --> Ag(0) (silver mirror or dust)
Cu(2+) + 1e(-) --> Cu(1+) (like into Cu2O see Fehling test for sucrose/aldoses)
Cu(1+) + 1e(-) --> Cu(0)
HO-CH2-CHOH-CHOH-CHOH-CHOH-CH=O --> HO-CH2-CHOH-CHOH-CHOH-CHOH-C(=O)-OH (here only the aldehyd group is oxydised to a carboxylic one and it passes from +1 oxydation state to +3 oxydation state)
The AgOH turns into Ag2O suspension/precipitate from "maturation" (concentration and heat of solution).
Paradoxaly Ag2O is specifical as it is not wel linked to its oxygen and it will set it free upon heating to live "native" silver and pure oxygen... this happens also with Gold whose oxide is also unstable and even explosive (set O2 free explosively from heat).
2 Ag2O -heat-> 2 Ag2 + O2(g)
I will reply a bit further/deeper later about the process of Sreetips soon.
PHZ
(PHILOU Zrealone from the Science Madness forum)
White precipitate when you dissolved silver in sulfuric acid is silver sulfate, it is slightly soluble in water. Silver hydrogen sulfate was soluble in sulfuric acid but when you diluted, equilibrium shifts and almost insoluble silver sulfate is formed so you technically discarded most of the silver.
So what would or could you do to prevent the silver sulfate
@@jameseves9209 Nothing. Simply do not use sulfuric acid. Use nitric acid and precipitate silver with copper metal. You can recycle both copper metal and nitric acid from Cu(NO3)2 byproduct with sulfuric acid and aluminum metal. Also, this way of getting silver from silver chloride is not very efficient. It's much better to put sodium hydroxide with silver solution to precipitate silver hydroxide which turns to oxide and then pure silver, when heated. But here you cannot do it because raw silver contains base metals like copper so hydroxide will be contaminated so best way is definitely precipitating Ag with Cu from AgNO3/Cu(NO3)2 mixture when you dissolve raw silver in nitric acid
I'm pretty sure that the silver sulfate that is created during the dissolving in sulphuric acid, and when you add heat the sulfate sheds the sulfur molecule, and then when added back to distilled water, it absorbs the oxygen molecule, becoming a silver oxide, which in turn is heavier than water. Then settles out in the water, if you were to have set the solution aside for 48 hours or so, more silver would have made the chemical shift to oxide from sulfide, and slowly develop a sulfur oxide on the surface of the water.
You can see the viscosity of the concentrated H2SO4.
It’s much thicker
Well, I gave this refining processes a go. I also ended up with ALLOT of Silver Sulfate. Also of note, in the bottom of the beaker with boiling Sulfuric Acid and Silver, a black cement formed, that cemented a stir bar fast to the bottom of the beaker. I had to use some heavy duty, needle nose pliers to break it up. My solution is cooled and settling over night. The "Silver Cell", your engineering, is Percolating really well. I just started it this afternoon and I already have a really nice accumulation of Silver Crystal's forming on the Cathode! Completely Awesome.
The black, very dense, cement that formed, will fill my burn cup, probably 4 times, altogether. I figured that I'd melt it into metal, and, then test it, to see what in creation it is. I did notice a redish blush, in the Sulfuric Acid I used, that was not present in yours. Maybe an, "Unknown" chemical slipped in. I used pure Sulfuric Acid, so I really am a little stumped. I'll burn it tomorrow and let you know what I've got.
Another good purchase, on another flatware set today. Sterling Silver. This time it was a bit more dear, to the tune of 2K. Worth it though. A little over 10 pounds, English Standard weight. My digital scales haven't arrived yet.
The only thing that is a pain, with both sets, recently purchased. The blades on the knives, cake server and butter knife, all have Stainless blades and the tang of the blade, running up into the handle! What a pain! Great Grandma's are completely Sterling Silver, even the blades. Lost a bit of weight there; but, still worth it.
Your presentation of the face value of a quarter versus it value in the Silver it was made from, really reverberated! That is a very good method for the explanation of the value of Precious Metals against our printed currency. With this current administration.... Woops! Sorry! We don't do "Politics"!
You have a pleasant evening. Thank you again for reigning, dormant grey matter, that is now crunching equations again! It feels great and is fun and is, (with the element of possible catastrophic disaster, explosions and other neat stuff), really exciting!
Wade
Can’t go wrong converting your paper to silver, my opinion.
@@sreetips Your opinion counts in my family!
Still don't know what the original black cement is. 3 Map gas torches and the cutting head on my OXYACETALYNE rig. Just won't melt! Incredible! So much heat was being produced, it warped my ¼ inch Steel burn table! Going to add a 2nd OXYACETALYNE torch to what I've already tried. If that doesn't melt it, I'll try the Kiln.......
Never had the Kiln as hot as all the gas torchs combined, produced. One way or another, it's going to melt, (Or I'll go out in a BLAZE OF GLORY)!...... Well, hopefully not. Guessing that I'll find out!
You sure come up with some great ideas. What a sweet wee bar.I must have had at least a dozen new subs mentioning you sent them today and a bunch over the last week since your last post. Thank you very much my dear friend.
Nice!
Very educational , thank you for sharing
Great video with close-ups and details. I love watching you produce 999 fine silver.
XRF would give you a definitive answer, but that white precipitate has to be either (1) a contaminant in your sulfuric acid, or (2) a salt of one of the metals from your sterling, so a silver, copper, tin, etc sulfate / oxide/ hydrate. Likely contaminants in drain cleaner sulfuric acid include a corrosion inhibitor like Rhodine 31A, which can crash out when neutralized (you might try pouring a few mL of the acid into 10 mL of water and see if you get a similar precipitate volume). Silver sulfate is a white salt that is barely soluble in neutral water (1.3g/100mL at 100C), but it's light sensitive like silver nitrate, and the missing silver's mass would show up if you can get a yield on one of those runs. Most copper sulfates are vivid blue and highly soluble. Tin, nickel, cadmium, or zinc sulfates all seem too soluble (33g/100mL, 65g/100mL, 76g/100mL, and 57g/100mL respectively). A tin or zinc oxide seems like a possibility too, depending on the sterling.
It was silver sulfate.
After months of researching I did my first silver recovers with the no nitric acid.
Starting my metal refining journey with help from this video, wish me luck in my eBay endeavours!
Start small to get the feel for it. Resist the urge to go all in with a hundred grams of karat gold. Instead start with just five grams to see how it goes.
@@sreetips Will do, thanks for the advice.
The precipitate is silver sulphate powder. Silver sulphate is insoluble in water and the dilutuon of silver sulphate and sulfuric acid in water causes the silver sulphate to precipitate out somewhat.
Nothing like sweet pure silver com'on...
If the sulfuric wasn't purified that powder layer is the buffers drain cleaner has in it to protect pipes.
Brilliant. You just always amaze me and are entertaining at the same time as being a teacher of sorts.
very nice!!! shiny..... you got a lot really right if it was just that candle holder.
That's my kind of meal right there!
Love your videos Sreetips! Thank you brother
Thanks for the new book purchase
think your using the natures way that takes place deep inthe earths crust
I believe the Silver is on the bottom at when you poured the silver nitrate and copper nitrate into distilled water. Since it's more heavy weight than copper and water.
When molecule weight is higher than 100. The molecules as Silver of 107 are heavy weighting. Copper will just float in the water.
The ending result gets blue color as only copper. But as copper and silver in nearly same is like the same as green and blue. But silver in bottom make only copper look blueish, when copper is green with Silver. But both can make either what they represent. So green solution has more likely copper and silver. But both can be sometimes either blue or green. But what Silver acts as color is gray. As in the second solution with the mixer.
You don't know it before you pour copper and silver which is used as alloy together.
There is actual strange difference in the color blue and green. Both don't make yellow color. But they make their dark green and dark black blue which in logic can't make yellow. But as soon it either is blue or green dark. Having only darker colors.
You should try as well to find out easiest way for copper refining. Many people would be interested in 100% output refining.
You nearly where there.
So best solution is really to take out the water of blue into other compartment. As silver lies in the bottom.
What you had when you first dissolved with sulfuric acid was platina and in the bottom as very darkish collection. Might as well be titanium or other metals as gold.
But palladium is clearly short the same molecule weight. Since nature make palladium first as halving to Silver. If there is no escape of energy palladium stays in the mountain. It is short lived.
The molecule weight represents important information.
I believe you know much. But you might not know everything yet?
FYI -- Sea salt does contain SOME iodine although less than iodized salt.
As for the precipitate, "Sterling silver is prone to tarnishing,[1][2] and elements other than copper can be used in alloys to reduce tarnishing, as well as casting porosity and firescale. Such elements include germanium, zinc, platinum, silicon, and boron." So possibly you are seeing one of these other materials, like silicon, boron or zinc compounds precipitating out, but I am not sure of their solubilities in concentrated versus dilute (~20%v/v) sulfuric acid.
One suggestion for saving cash, buy bulk paper coffee filters, great for initial filtering and work really well with buchner funnels.
I had not ever though of using coffee filter in the Büchner funnel - that's a great idea. I believe that the precipitate is merely silver sulfate. To get the silver I'll dissolve it (the silver sulfate) in boiling water then add the salt while its still boiling, before it has a chance to cool down and precipitate as silver sulfate again.
Your precip is likely Silver Sulfate. The temperature change can trigger the reaction.
I'll dissolve it in boiling water then add salt while its still hot to get the remaining silver chloride.
Precipitate is PbSO4 which is insoluble, or water had Cl ions so AgCl maybe..., Or if Sn is present is SnO2...
Judging from the color there might be more other metals in the bar then you may suspect. An xrf test would be a nice way to find out for sure.
Beautiful silver bar
That salad looked amazing. But I think I can smell your breath from here :p
The white sediment could be zinc sulfate. Stirling silver is an alloy about 90 % silver and 10 % of copper, nickel or zinc. Possibly others. The blue/green is probably copper sulfate II I think.
Silver sulfate
Refiners Bible, thank you sir!!
That white precipitate is silver sulfate ;). It tends to only wan't to dissolve in concentrated H2so4, once diluted with water the solubility goes down.
Sreetips keepin healthy! Lunch looks good! Lots of fiber. 😉👍
Your solution was over saturated and silver sulfate is practically insoluble in water. It is soluble in hot sulfuric acid but again, over saturated with the cooling and further cooling and diluting helped it crystallize out.
Jimmy, 1.33g per 100ml water at 100C. I had to look it up. It'll dissolve in hot water. Then add the sodium chloride to the hot solution to get the rest of the silver. Brilliant!
Its silver sulfate witch in water is insoluble, but when in a highly concentrated solution of sulfuric acid probably of 98% or higher the silver will react and dissolve since there is almost no water present. then when you poured that solution into the water the silver sulfate crashed out because the ph becomes to high for it to remain dissolved.
I solved it by pouring in hydrochloric acid instead of water. It immediately forms silver chloride and I avoid the silver sulfate formation
When I was doing this, after I put the acid into the water I left it for a few days and I built up a thick layer of that precipitate
I know Sreetips said this here but be very, VERY careful with boiling 98% (any concentration really)Sulfuric Acid. It’ll scold and dissolve skin very, very fast. It’s boiling point is over 600F, which can be very deceiving. It’s like pouring molten lead on your skin with the added effect of dissolving everything it touches very fast.
That Rooto brand Sulfuric Acid is the good stuff. Nice and clear, possibly no iron passivates or organic compounds. You could make some very pure nitric acid with nitrate salts using it, like 99% fuming. It’s not really good for refining due to the extreme chance of runaway, but I’ve never tried it.
Thanks for showing that brand of drain cleaner, my local hardware store has it in gallons for $26.
It about the same here, used to be about $15 per gallon back in 2010 when I first started. Has it become that much more valuable? Or has the currency lost that much value?
@@sreetips it’s a Do it Best, price has been that high for a few years now. According to the bar code tag anyways. I know we’re hosed anyways.
A shortcut I'm experimenting with right now is adding Spectricide stump remover (100% Potassium Nitrate) to the sulfuric acid solution and heating it. The mixture creates nitric acid in-situ and seems to dissolve the metal (copper and silver out of scrap jewelry) exactly like commercial nitric acid. So far, so good. We'll see how the potassium bisulfate follows the silver through the process and if it messes up the silver or gold. Perhaps you'd like to try this experiment with your setup.
How did your mixture work out?
Did the silver come out clean or contaminated?
how do you separate the silver from the rest after the "poorman's nitric" solution dissolve everything (copper, silver)
I’ve never tried this, but if it works and everything dissolves (have to filter out solids with a micro fiber glass filter due to sulfuric with dissolve a paper filter) then the silver can be precipitated by adding hydrochloric acid (carefully because it reacts violently with sulfuric) to precipitate out the silver chloride. Then the silver chloride can be converted to pure silver with lye and sugar.
@@sreetips it should work with sulfuric and potassium nitrate for the dissolving phase? By the way amazing salad.
I don’t know because I’ve never tried it.
Love your hat mate. I was on Patrol Boats for 8 years.
I served on two destroyers and a fast frigate. The Navy was good to me. And I to it.
I giggle every time he says lye and sugar. I can’t help but think he’s saying *Lion Sugar* and the thought of that makes me laugh. 🦁🍭
The problem with dumping the sea salt in without dissolving in water first is that it will also force precipitation of some of the copper sulfate.
Also, once the silver chloride is precipitated, you should test the blue liquid to make sure all the silver has been precipitated.
I changed the process. I got a way better yield.
Thanks for your videos, did my first CPU’s in sulfuric acid and peroxide and I got gold!!!
Me: melts down candle holder with propane torch.
He's also refining the silver. Purifying it.
Ag2SO4 is silver sulphate just so you know that’s the white precipitate. I would not discard it because it contains pure silver.
Thank you very much sir, for your efforts and knowledge. Take care
It would be nice that you put in the video description the chemical formulae for those products.
In the EU we don't have the same BRANDS but maybe we have the same chemicals in a different brand.
In case you have 2 minutes of free time to teach me, I'll be happy to learn :)
Sugar ; self explanatory
Lye ; caustic soda or sodium hydroxide
sulphuric acid; also known as battery acid.
seasalt is also table salt but without iodine.
Great video.
I've had the same mystery precipitate in a different scenario
I really appreciate all of the information that you share
This was another great video
*Sneaks in and takes Sreetips lunch.....* it looks fantastic!
That precipitate may be one of the Copper Chlorides. Sterling contains Copper, possibly Lead. There is a 999 Dusan video where he shows that one of the Copper Chlorides is soluble in concentrated acid, but merely diluting the acid, (greatly), with distilled Water, caused the Copper Chloride to precipitate out because that compound is much less soluble in dilute acid. Its solubility probably drops off logarithmicaly with the decrease in concentration. In the video by Dusan, the Copper compound was white, or very white-ish. Any Lead in there might exhibit a similar behavior.
I've already determined that it's silver sulfate. And that it can be converted to silver oxide with lye just like silver chloride. Bummer. I just made a new video showing how to get the chloride from the sulfate. Obsolete before it even gets published.
Hello Sreetips I think if you added some Potassium Nitrate (Stump Remover) to the solution it will work a lot like Nitric acid. I tried it once before sourcing Nitric and it worked pretty well.
Poor man’s aqua regia - I’ve never tried it.
@@sreetips time for a video perhaps 😇
You could try pouring the warm conc. Sulfuric acid/silver sulfate solution into warm distilled water to keep more of the silver in solution.
I was thinking collect the silver sulfate, dissolve in boiling water, then add salt to the boiling solution to precipitate the silver chloride
@@sreetips yeah good idea
I did it, video uploading right now. You won't believe how much silver was tied up in the sulfate.
But then someone has told me that the silver sulfate can be converted to silver oxide with lye just like silver chloride. Then to metal with sugar.
@@sreetips i was wondering that myself. The conversion of sulfate to oxide probably goes faster than chloride due to the slightly more soluble sulfate. Maybe not, but it doesnt surprise me at all that the sulfate can also be converted with the lye/sugar method
I likw your vids really good i have watched an re watch some of them knowlage is an amazeing good at explaining a natural teacher
It's silver that crashed out in the cold water. Silver is less soluble in the colder temp. I'm really just guessing. I'm not a chemist but I watch every video you come out with. I pay attention
❤nice work....
@ 11:50 = "if any of you chemists know what's going on here..." - most obliged, Sir...
The thing is, silver sulphate, Ag2SO4, is just marginally soluble in water, but quite soluble in H2SO4, even at lower concentrations. A 100 mL of pure water @ 25°C (77°F) can dissolve just 0.83 g of Ag2SO4 (and it doesn't change much with temperature), while 100 mL of 0.1 mol H2SO4 at the same temperature can dissolve as much as 31.56 g of (if my quick calculations are correct, 0.1 m H2SO4 is approx. 10% solution).
Specifically, Auntie Wiki says:
Solubility in water
0.57 g/100 mL (0 °C)
0.69 g/100 mL (10 °C)
0.83 g/100 mL (25 °C)
0.96 g/100 mL (40 °C)
1.33 g/100 mL (100 °C)
Solubility in sulfuric acid of 8.45 g/L strength (0.1 mol H2SO4/L H2O)
25.44 g/100 g (13 °C)
31.56 g/100 g (24.5 °C)
127.01 g/100 g (96 °C)
So, the difference is huge - which means that diluting remaining (unreacted) acid (as far as I can tell, the reaction was done with a huge excess of H2SO4) will inevitably result in precipitating of Ag2SO4.
About "splattering everywhere" (a minute or so earlier in the video) - as you probably know, mixing concentrated sulphuric acid with water is VERY exothermic, and if you do it too quickly and/or in large quantities it can even lead to boiling of the mixture (which is to be avoided). So if one pours a very hot (around 100°C) and still pretty concentrated H2SO4 into water it will heat the water almost instantly above its boiling point, and splattering will be the result.
BTW, that H2SO4/H20 "reaction" is so exothermic that "hyper-concentrated" H2SO4, often referred to as "oleum" (a shortening of oleum vitrioli, not to be confused with oleum dulci vitrioli, which is diethyl ether, while oleum vitrioli is a solution of SO3 in 100% H2SO4) must not, EVER, be mixed directly with water - one has to dilute it first with concentrated H2SO4.
And it goes without saying that thick rubber gloves, elbow length, with a second (lighter) pair underneath is a must in handling that devil in a bottle. And so is full face mask AND goggles - and some respiratory protection IN ADDITION to fume hood is highly recommended.
And, while I'm here... I'm always... say, "amused" by that mismatch of your nearly quantitative analysis precision in precipitating precious metals and then blowing at them with strong stream of gases from oxyacetylene torch - it's just... it just doesn't make any sense to me. A good small second-hand electric furnace would cost probably much less that all that gold and platinum dust blown off in all those melts to date.
Just saying... ;-)
Cheers, KB
I cut my teeth with fused silica melt dish and oxy/acet torch. Learned it from the pros on the goldrefiningforum.com you don't have to be a chemist to be a refiner. But it probably helps.
@@sreetips Of course, you don't have to be a chemist to be a refiner, but yes - a good understanding of all those reactions and processes does help a bit. Still, with applied chemistry, hands-on experience and knowledge of all those "tricks of trade" are just as important.
Like, quartering gold with silver - AFAIK there's nothing really in "chemistry knowledge base" about why one should stick to a certain proportions of those metals to get just the right size of particles of gold "mud" - i.e. just fine enough, but not too fine.
And yes, I agree - old timers and pros of the trade have their own paths, well trodden... Still, innovation and improvement comes from challenging all those "old and established" truths and practices. But hey, who am I to tell you how to refine (and melt) your gold... ;-)
Best, KB
MrKotBonifacy agree, I’m constantly refining my refining processes
@@sreetips Good. All the best on your road to five "nines" ;-)
Cool to watch .Cheers mate from Australia 🇦🇺 👌