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Author: Subject: Calcium nitrate + Copper Sulfate double displacement not happening....
RogueRose
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Calcium nitrate + Copper Sulfate double displacement not happening....

I mixed up proper molar ratio's of copper sulfate and calcium nitrate, filtered very well and when I started to mix the two I was expecting the white calcium sulfate to form pretty much instantly but nothing happened. The copper sulfate was at it's maximum solubility level as was the nitrate, so I'm not sure what is going on as I've done this many times before and it works fine, the only difference is the calcium nitrate is from a different supplier it isn't from the Norwegian manufacturer (Yara) that I used before.

I'm sure the copper sulfate is copper sulfate and the calcium nitrate is labeled 15.5-0-0. The nitrate dissolved very similarly to the previous batches I've had as far as being able to dissolve about 2KG/L of water and it had an endothermic effect.

I'm guessing this might be Calcium Ammonium Nitrate, which would really suck as I have no idea how this is going to mess up my mixture.

Is there any test I can do to figure this out? I still have some of the prills to test. I'm guessing adding some Ca(OH)2 to the nitrate solution should off gas some ammonia?

I'm more concerned with the copper sulfate solution that now has a mix of unknown nitrate/ammonia mix in it. I would have thought if this was CAN, the calcium nitrate in the mix should have displaced the copper sulfate to some degree, but I got nothing, it just mixed in as if I didn't pour anything in. I've also added ammonia to copper sulfate and it turns a darker blue and this didn't happen either. So I have no idea WTF is going on and I'm really pissed.

Any suggestions on what might be happening and if you have any ideas what this "calcium nitrate" might be other than some shitty CAN mix, i'd really appreciate your input! Thanks!
B(a)P
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Could it be that you have been sold urea? Take a sample of your liquid and add some NaOH and see if it turns purple. Heat the left over prill in a well ventilated area to see what the melting point is. If you can't measure it just heat it until decomposition to see if it forms ammonia.
RogueRose
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 Quote: Originally posted by B(a)P Could it be that you have been sold urea? Take a sample of your liquid and add some NaOH and see if it turns purple. Heat the left over prill in a well ventilated area to see what the melting point is. If you can't measure it just heat it until decomposition to see if it forms ammonia.

I guess urea would have similar solubilities and also be endothermic.. Good point!

I just did a MP test and it had no ammonia smell, it didn't really have any smell or colored gases. I melted about 6-7 prills and it left behind what looks like calcium oxide/hydroxide and had a slight yellow/brown tint to it.

I'll add some lye and see what happens. if there is any ammonia in it, I should get ammonia gas I would think, and if it is CAN, the reaction shouldn't need much agitation as it's pretty humid as is and the water in the CAN should be enough to catalyze it.

[Edited on 6-30-2020 by RogueRose]
RogueRose
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 Quote: Originally posted by B(a)P Could it be that you have been sold urea? Take a sample of your liquid and add some NaOH and see if it turns purple. Heat the left over prill in a well ventilated area to see what the melting point is. If you can't measure it just heat it until decomposition to see if it forms ammonia.

Well it doesn't seem to be urea, so that is good. I came back to the solution and it seemed to have precipitated out some CaSO4, it just took much longer than my previous trials. When I mixed the two before it would precipitate out almost instantly, I could pour it in and a white cloud would form and fall to the bottom of the container. Here it just settled to the bottom and when I stirred it, nothing happened for about 20-30 mins, then I checked about 2 hours later and the mix was cloudy. I've just never seen this reaction move this slowly.

From what I've found CAN is something like this: 5Ca(NO2)3 + NH4NO3 + 10H2O, so a 5:1 ratio of calcium to ammonium nitrate. So I'm wondering if the ammonium nitrate is slowing the reaction?

I decided to add some NaOH to the Ca(NO3)2 prills and added some drops of water. I could smell A LITTLE bit of ammonia but it was extremely faint. I think I did this test before with my original Ca(NO3)2 and smelled ammonia with that as well, so maybe there is always some in calcium nitrate? IDK.

Can you think of any way to determine if there is an appreciable amount of it in this mix, and if so, I'm guessing the only way to deal with it is to reflux the nitrate solution with some Ca(OH)2 which should off-gas the ammonia and convert the ammonium nitrate into calcium nitrate + ammonia gas.?

I really can't see how pure Ca(NO3)2 would produce the smell of ammonia w/o it having been made with ammonium nitrate to begin with or is CAN. I really hate when things are mislabeled.
violet sin
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Did you use the solution grade garden fertilizer by yara brand by chance? 14.4% nitrate , 1.1% ammonium.
https://www.yara.com/crop-nutrition/products-and-solutions/g...

I picked up some a while back, my tomatoes love it. The prils will gather moisture from the air much like Lye if you dick around too long transferring the stuff. I could try your reaction real quick and see if it crashes out gypsum promptly or takes a while. A good comparison might be trying a similar amount of cold pack calcium ammonium nitrate. Pretty sure that stuff is not the same quality, IIRC it had more ammonia and less nitrate.

13.5% ammonium & 27% total nitrogen
http://www.achema.lt/calcium-ammonium-nitrate-n27

†****†***†*********************
Solution grade fertilizer 5Ca(NO3)2•NH4NO3•H2 and copper sulfate pentahydrate were combined at 1:5 respectively in 0.01mol and it froze solid with gypsum in ~30 sec in 60ml total volume water

Sorry pic is sideways, no time

[Edited on 30-6-2020 by violet sin]
B(a)P
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According to wikipedia -
The fertilizer grade (15.5-0-0 + 19% Ca) is popular in the greenhouse and hydroponics trades; it contains ammonium nitrate and water, as the "double salt" 5Ca(NO3)2.NH4NO3.10H2O . This is called calcium ammonium nitrate. Formulations lacking ammonia are also known: Ca(NO3)2·4H2O (11.9-0-0 + 16.9 Ca) and the water-free 17-0-0 + 23.6 Ca. A liquid formulation (9-0-0 + 11 Ca) is also offered. An anhydrous, air-stable derivative is the urea complex Ca(NO3)2·4[OC(NH2)2], which has been sold as Cal-Urea.

So looks like you have the double salt.
violet sin
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I tried to edit this into last night's post, but it would not allow edit... Do we no longer have a 24hr period to edit our posts? First time I've noticed that.
**I'm dumb, I posted well before grabbing flasks to play, so it had been 24 hrs. Shoulda confirmed edit last night, lol**

Solution was filtered on old home made buchner, no fines made it through. There was still a portion of the ammonium nitrate from the double salt so it was left overnight stirring gently @~100°F w/0.55g copper basic carbonate. Only smelled the tiniest bit of ammonia right after heating. Should I have probably dealt with that on the front side with slacked lime.. yeah, but I had the basic carbonate still out staring at me.

I have a little over 200ml of what should be copper nitrate with some copper sulfate left in from double salt hydration (•10 not •1H2O) miscalculation.

What's the preferred method to crystalize it out? I read it's hydrates are soluble in alcohols, so I'm guessing that it can't be crashed out with absolute. What about acetone? It's also been warm here, mid 90's to 113°f the other day, I could leave it to dry covered outside.

****. I see that I'll have a hard time here without nirtic acid 'eh? ****
DraconicAcid: "Copper(II) nitrate trihydrate will crystallize from nitric acid solution, but it's very difficult to crystallize from water. I've had some crystals of it melt on a warm, humid day, and they never resolidified"

WGTR:. "After several days the atmosphere in the desiccator turned brown from NO2 fumes, and brown traces of decomposition were becoming apparent in the salt, as it was drying out too much"

So guess I'm to make a little nitric acid? Don't feel like dessicating 200 ml out. But if I could gently diminish the water sans decomp, to an acceptable level i'd be happy to know it.

[Edited on 1-7-2020 by violet sin]
RogueRose
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 Quote: Originally posted by violet sin Did you use the solution grade garden fertilizer by yara brand by chance? 14.4% nitrate , 1.1% ammonium. https://www.yara.com/crop-nutrition/products-and-solutions/g... I picked up some a while back, my tomatoes love it. The prils will gather moisture from the air much like Lye if you dick around too long transferring the stuff. I could try your reaction real quick and see if it crashes out gypsum promptly or takes a while. A good comparison might be trying a similar amount of cold pack calcium ammonium nitrate. Pretty sure that stuff is not the same quality, IIRC it had more ammonia and less nitrate. 13.5% ammonium & 27% total nitrogen http://www.achema.lt/calcium-ammonium-nitrate-n27 †****†***†********************* Solution grade fertilizer 5Ca(NO3)2•NH4NO3•H2 and copper sulfate pentahydrate were combined at 1:5 respectively in 0.01mol and it froze solid with gypsum in ~30 sec in 60ml total volume water Sorry pic is sideways, no time [Edited on 30-6-2020 by violet sin]

The first stuff I had lke 5 years ago was Yara "Tropicotie" or something like that. I still filtered it, but it was pretty clean with a slight yellow tint. With a little AC and filtration, it was crystal clear. This new stuff, IDK WTF it is. I refluxed with Ca(OH)2 and had a decent amount of NH3 coming off it, so that really screws things up. But I did fine an old bag of Yara in the back of the warehouse that is a large 50lb brick (absorbed moisture) but I'm going to play with that.

I've had 6 different cold pack brands, some just labeled Amm Nitrate (on box and MSDS/SDS) (none were only amm nitrate), and I've had some "CAN" that was labeled ammonia nitrate & calcium nitrate, I had some Urea. Basically all the stuff I found in the states at grocery stores and pharmacies were SHIT. None were properly labeled. I'm guessing they use whatever they have in stock and maybe even mix and match batches. If it gets cold, that's all they care about. Total Bs. I wasted $50-60 figuring this shit out.. Side note, I found a supplier of NH4NO3, KNO3, NaNO3, KClO3 and NaClO3, all from one supplier. They would never sell to me before but after 8 years of buying and being a good customer (and helping them get their products properly labeled), they finally trust that I'm not some trailer park crazy or something. With this "green revolution" and much of it being hydroponics, there is a good bit of #$$to be made with some proper custom fertilizer blends that no one around here sells. Most of it is like$30-50 for a 5lb bag of "all natural" crap that doesn't even dissolve in the hydroponic systems they are running. Sorry, for the tangent /rant
RogueRose
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 Quote: Originally posted by B(a)P According to wikipedia - The fertilizer grade (15.5-0-0 + 19% Ca) is popular in the greenhouse and hydroponics trades; it contains ammonium nitrate and water, as the "double salt" 5Ca(NO3)2.NH4NO3.10H2O . This is called calcium ammonium nitrate. Formulations lacking ammonia are also known: Ca(NO3)2·4H2O (11.9-0-0 + 16.9 Ca) and the water-free 17-0-0 + 23.6 Ca. A liquid formulation (9-0-0 + 11 Ca) is also offered. An anhydrous, air-stable derivative is the urea complex Ca(NO3)2·4[OC(NH2)2], which has been sold as Cal-Urea. So looks like you have the double salt.

Yeah, I found that as well, but I think it's worse. I think Ihave CAN, which is 27-0-0, which is why it wsa producing so GD much NH3 when I added the Calcium Hydroxide.

I'm working on 7 setups now and testing what the possible ammonia levels are in the mixes - the generic one I'm having problems with, and my new (old stock / swolen brick / Yara product) and I'm going to get a definitive answer on the ammonia content of all of these.

The kicker is when I told the distributor and retailer that there was a ton of ammonia coming out of the product, they had NO idea what I was talking about and even after explainig AMMONIA is NOT NITRATE, I don't thin any of them followed.. HOW TF can you run a fertilizer business (retail to farmers) and a wholesale distribution company and not know the difference! And these are the people ruining our fields for the last 50 years. For fucks sake... No wonder the soil is dying.

[Edited on 7-3-2020 by RogueRose]
RogueRose
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 Quote: Originally posted by violet sin I tried to edit this into last night's post, but it would not allow edit... Do we no longer have a 24hr period to edit our posts? First time I've noticed that. **I'm dumb, I posted well before grabbing flasks to play, so it had been 24 hrs. Shoulda confirmed edit last night, lol** Solution was filtered on old home made buchner, no fines made it through. There was still a portion of the ammonium nitrate from the double salt so it was left overnight stirring gently @~100°F w/0.55g copper basic carbonate. Only smelled the tiniest bit of ammonia right after heating. Should I have probably dealt with that on the front side with slacked lime.. yeah, but I had the basic carbonate still out staring at me. I have a little over 200ml of what should be copper nitrate with some copper sulfate left in from double salt hydration (•10 not •1H2O) miscalculation. What's the preferred method to crystalize it out? I read it's hydrates are soluble in alcohols, so I'm guessing that it can't be crashed out with absolute. What about acetone? It's also been warm here, mid 90's to 113°f the other day, I could leave it to dry covered outside. ****. I see that I'll have a hard time here without nirtic acid 'eh? **** https://www.sciencemadness.org/whisper/viewthread.php?tid=14... DraconicAcid: "Copper(II) nitrate trihydrate will crystallize from nitric acid solution, but it's very difficult to crystallize from water. I've had some crystals of it melt on a warm, humid day, and they never resolidified" WGTR:. "After several days the atmosphere in the desiccator turned brown from NO2 fumes, and brown traces of decomposition were becoming apparent in the salt, as it was drying out too much" So guess I'm to make a little nitric acid? Don't feel like dessicating 200 ml out. But if I could gently diminish the water sans decomp, to an acceptable level i'd be happy to know it. [Edited on 1-7-2020 by violet sin]

I didn't get a chance to read your post here, but I did somethign similar a while back with "pure" cal nitrate (which I now believe had some NH4NO3 - about 15% of the nitrate...) and that is probably why I got a really shitty product. I spent forever purifying the Cal Nit and CuSO4 before mixing the two in perfect combinations, but the end product was just terrible - I expected 4-5lbs and got just over 2, even after 8 washes of he CaSO4. I think something with the ammonia in it allowed it to boil off or something. IT never crystalized correctly, never got nice colored crystals - totally disappointing for he 20+ hours I spent.

On a side note, how do you plan on filtering the CuNO3 from the CuSO4? It's a BITCH. I'm looking for a cheap, new high speed washing machine I can use as a centrifuge (look for the augerless ones & make a big "bag" with super fine mesh. Fill it with the CaSO4 and put on max spin then drain all the liquid from the unit (don't let the pump pump it out you can disconnect this and just drain with gravity). It may work well with an older washing machine but the new "eco friendly" ones spin like 2-4x faster.
B(a)P
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 Quote: Originally posted by RogueRose I think Ihave CAN, which is 27-0-0, which is why it wsa producing so GD much NH3 when I added the Calcium Hydroxide. [Edited on 7-3-2020 by RogueRose]

That is annoying. So you think you have Ca(NO3)2.4NH4NO3.2H20?
At least you get more N for your buck!
What is your end goal, Cu(NO3)2? or something else?

violet sin
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Well, I made a bit of crude nitric acid with the same fertilizer, specifically yara-liva calcinit and liquid fire. cloudy a bit, yellowish, sure. But it eventually ate copper, would not drop more gypsum on CA(NO3)2 addition.

Left a tiny bit in a vial with copper strip, produced crystals. Wether they are left over ingredients forced out by increasing nitrate salt content and decreasing acid content, or just actually copper nitrate I'll wait to see.

I repeated twice more with previous amounts for a theoretical 0.055mol x 3. But I was lazy and only used slacked lime for the first run converting ammonium nitrate. So there will be some ammonium sulphate in there as it's only filtered, not distilled,( there is a limit to my wife's patients).

Ammonia wasn't much, but definitely noticed it on mixing dry powders fertilizer/slacked lime. So I think 5:1 CA(NO3)2/NH4NO3. Is quite reasonable. It was heated and stirred for a bit with very little ammonia smell. You weren't driven back immediately.

Anyhow it's stirring on low heat with acid to keep from loss of NO2 and decomp. Here's some pictures,
1) litmus test before sulfuric acid test against Ca2+, and then separate fertilizer test against SO42-. It was slight on dissolved Ca and not sulfate rich.
2) sulfuric acid, nitric acid, yesterday's copper nitrate and one used small vial in foreground dissolving copper strip.

3) closeup of copper strip and crystals

RogueRose
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Quote: Originally posted by B(a)P
 Quote: Originally posted by RogueRose I think Ihave CAN, which is 27-0-0, which is why it wsa producing so GD much NH3 when I added the Calcium Hydroxide. [Edited on 7-3-2020 by RogueRose]

That is annoying. So you think you have Ca(NO3)2.4NH4NO3.2H20?
At least you get more N for your buck!
What is your end goal, Cu(NO3)2? or something else?

The end goal was Cu(NO3)2 and CuSO4 as I needed both (I needed about 100lbs of CaSO4) and I have a number of buyers for good quality Cu(NO3)2, so it was a win, win for me ( high purity sells for $34-42/lb here from hydrate to anhydrous - many of the "economic products" have a fair amount of CuSO4 pentahydrate mixed into the powder I've been told) . Now I'm stuck with either making my own Cal Nitrate from ammonium nitrate (finally found a source VERY VERY good price!!!!) + Cal Hydroxide - mix, reflux, & either capture NH3 as concentrated solution (which I will probably do) and maybe as some NH4Cl, which I need as well. I could just add some claclium hydroxide to my Cal nitrate /CAN (whatever it is), reflux with Ca(OH)2 and filter (capturing the NH3 that is produced), and will proabalby do that just to see what the real composition is of this mix. It's just a SHIT TON more work than I expected. I figured 2 steps - find molar equivelants of Cal Nitrate Tetra hydrate & Copper Sulfate, dissolve each seperatetly, filter (with AC) - which I did and got it VERY Pure. Then I find the Cal Nit is a shit mix, so now my 60 moles of CuSO4 has a bunch of the CAN/CalNit shit mix stirred into the solution - but only about 25-50ml of very concentrted CalNit mix - so it shouldn't be so bad. But wasting 60 moles (about 25 lbs) of copper sulfate would be painful... The worst part is the company that sold it didn't care at all, their distributor didn't care, and they all blew me off telling me "it was impossible for ammonia to be in it" and maybe it was something I did, or maybe it was my "storage" or it was old. I bought it the night I started processing.$260 for all the stuff I bought (got other stuff), but still, These people are the ones who tell you what to put on your fields to grow crops. You should hear what I've heard them tell people. It's no wonder the soil and micro organisms are DEAD in the States & other countries. They put so much chemicals on, kill any beneficial bacteria, and overload it with nitrates and phosphates and potassium to make up for any "mistakes" that happens from good care of the soil. Oh, and don't even THINK about allowing your field to be fallow once every 3-7 years - that is SACRILEGIOUS!!!

This older class of farmers should be stripped of their ability to farm.

[Edited on 7-3-2020 by RogueRose]

[Edited on 7-3-2020 by RogueRose]
OldNubbins
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My hardware store carries the Hi-Yield brand which I believe is relabeled Yara. I used to go the same sulfate route but got tired of dealing with the calcium sulfate so now I buy a bag of the calcium-ammonium nitrate mix (15.5-0-0) and a bag of potassium chloride. I just dissolve and mix the two and crystallize out the potassium nitrate and leave the calcium chloride in solution. It's easier to purify the potassium nitrate and it makes a great starting point for the other salts.
RogueRose
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 Quote: Originally posted by OldNubbins My hardware store carries the Hi-Yield brand which I believe is relabeled Yara. I used to go the same sulfate route but got tired of dealing with the calcium sulfate so now I buy a bag of the calcium-ammonium nitrate mix (15.5-0-0) and a bag of potassium chloride. I just dissolve and mix the two and crystallize out the potassium nitrate and leave the calcium chloride in solution. It's easier to purify the potassium nitrate and it makes a great starting point for the other salts.

Well if you have any interest I can point you to a few places online that sell sodium and potassium nitrate online anywhere form 1lb to 50lb bags and it's $24 for UPS delivers for 50lbs. KNO3 is$54/50lbs + $24 for shipping and NaNO3 is$208/100lbs and I think $34 for shipping. KNO3 starts at$1.7/lb and NaNO3 starts at $2.8/lb, and it gets cheaper if you buy 5, 10, 15, 20, 25 or 50lbs. I'll be getting prices from my local supplier and if they are good, I'll be offering them to members along with some other things I've found of interest. I found a good supplier for NaOH, KOH, Mg & Al & Ti powder/turnings/sweepings as well as mixes of MagAl, FerroAluminum, Ferromagnesium, Ferrotitanium, iron powder and many more. Also irun turnings and a bunch of other metals like Zn powder, brass powder, turnings, chips, etc. I've filled out an BATF license and am getting ready to send it in along with another licence for another LARGE local group I'm going to be working with. violet sin International Hazard Posts: 1357 Registered: 2-9-2012 Location: Back yard staring at stars Member Is Offline Mood: Good RogueRose: Good grief, that's quite the scale ye be working at there. I was just bored. Almost feels silly even commenting with my experiences working on several ml batches and 10.8g calcinit per test. I got to play, but your post clearly underscores the absolute difference in work and play. Having that much solution/product misbehave... in a monetary manner, no thanks. Good you have a use for that much gypsum RogueRose International Hazard Posts: 1574 Registered: 16-6-2014 Member Is Offline  Quote: Originally posted by violet sin RogueRose: Good grief, that's quite the scale ye be working at there. I was just bored. Almost feels silly even commenting with my experiences working on several ml batches and 10.8g calcinit per test. I got to play, but your post clearly underscores the absolute difference in work and play. Having that much solution/product misbehave... in a monetary manner, no thanks. Good you have a use for that much gypsum Well I think I can salvage what I have. I'm going to reflux everything and then filter out any remainingng cal hydroxide/carbonate and then mix all the solution together and then take 100, evaporate it to anhydrous and see what 100g of solution produces. From there, I should be able to see what I have in my 3-4 gallons of Can Nit solution (god it heavy - probably like 12-14lbs/gallon). That seems like the only reasonable step I've been working with both MgCO3 and CaSO4, both are a major PITA to filter b/c it is so fluffy, but I found an awesome way to do it. Basically I use the same material "wife beaters" are made from (I gett it in 60" wide rolls for like$.50 per yard), put it over a 20 gal bucket with a bunch of spring clips on it and I can dump about 10 gallons on top of the fabric, let it sit for 2 hours, wring it out and 90-95% of the water is gone. Then I do a final rinse with a fiair amount of water, and just dispose of that as it's mostly pure water.

I was looking into the new ultra high speed washing machines and was told that they only do about 1200g's or RPM (forget which) when a real centrifuge will do 5000-6000g's or RPM. But most of the centrifuges I've seen are about 14-18" diameter where the washing machine is pushing 30, so I think you can forgoe the speed if you have a much wider diameter centrifuge - does that make sense?

I'm thinking that once the sulfate and carbonate are 90-95% dry, that is the time to put the in the spin cycle as I can evenly distribute the loading around the bottom of the machine, then as it spins, it will spread it out and flatten it nicely.

I ws surprised when I found that there was demand for MgCO3 in some niche area and if packaged correctly a person is looking at \$80-100/lb for HIGH QUALITY product, and in most ases it sells in the rance of 10-20g a piece. I'm still workingon the formulation but I never thought something so cheap could have such high demand!

Now my question is whether I can mix in the CaSO4 in with it. Is the sulfae more drying (the mix will have a slight bit of water to make a paste? The buyer said they don't care, as long as it's a great product.

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