36 replies to this topic

[richard2]

Another option if you cannot easily aquire the HCl required in the above post is the acetic acid (ie vinegar) > barium acetate + XXX nitrate > barium nitrate route. It has been disscused here before i believe so if you search for some key words you should come up with details (mabye even with all the calcs done for you).

Regards


Rich

[Bonny]

I suggest you do a Small scale version 1`st, it really takes quite a bit of heat (Boiling) to drive off the Ammonia and Co2 to swing the reaction direction in your favor.

a Gallon of it for instance would need a day to boil (outdoors of course) and regular topping up with water.
it Is Doable, but it`s hard work!

so try a small amount 1`st, and keep the carbonate in excess, it`s the AN traces you don`t want!, the Carbonate is mostly insoluble anyway and so after filtering it`s negligible

Any idea how long this should take? I tried a batch of 40g NH4NO3 with 37g SrCO3 and then added extra SrCO3. With regular topping off of water, this has been boiling for about 6hrs and still smells of ammonia. Have to turn it iff now as I'm out of time...

[wyattp4007]

@ YT2095

I'm trying to find a way to produce both Barium Nitrate and Strontium Nitrate from the carbonates of each as well, without using HNO3.

From what I understand in your previous post, you can convert Barium Carbonate to Barium Chloride via HCl correct? How does the reaction of Barium Chloride and Ammonium Nitrate go, is it just a simple displacement reaction or is there heating involved like with the Strontium Carbonate? How about subbing the Barium Chloride with Strontium Chloride in the same process? I'm not very chemistry literate, so if you could clarify it for me it would be appreciated. Man I wish I'd taken chemistry in high school...

What would be the best nitrate salt to use for the process? I have Ammonium and Potassium nitrates to work with and can make Sodium Nitrate via the reaction of NH4NO3 and NaOH. What is the best route to go?

[YT2095]

Bonny: there is no set time for this reaction, it`s done when no more ammonia can be detected, that`s why I said try a small batch 1`st, it helps you get a feel for the RXN. however tha fact that you`ve been able to smell the ammonia means that you have already made a little Sr(NO3)2.

Wyat: if you have the chlorides of these, you get rid of the solubility issues associated with most of the group 2 metals (Never Use Sulphuric acid with either the Ba or Sr). what happens is called a double decomposition reaction, they swap Ions making Ammonium chloride and your metal nitrate.
then with careful crystalisation (exploiting the fact that they have different solubilities) you can obtain your product.

just a quick look at my book and I can see that the solubility for Ammonium chloride in water at room temp is: 37.2g / 100ml
Barium Nitrate is only: 9.02g/100ml.

just over 4 times as soluble, so when you evaporate your soln, the 1`st crystals you`ll see form will be your Barium Nitrate

the Opposite is true for Strontium nitrate! its solubility is 69.5g/100ml
so the 1`st crystals you will see when using That, will be your Ammonium Chloride, the Sr(NO3)2 will be in the soln still

stay with the Ammonium salt, you`ll never remove the K+ from the NO3- with any combination we`re going to be using, also Sodium satls are a waste of time, they will color contaminate your product making it useless for pyro apps.

hope that`s helped a little

[Bonny]

[quote name='YT2095' date='Oct 1 2007, 08:00 AM' post='38338']
Bonny: there is no set time for this reaction, it`s done when no more ammonia can be detected, that`s why I said try a small batch 1`st, it helps you get a feel for the RXN. however tha fact that you`ve been able to smell the ammonia means that you have already made a little Sr(NO3)2.

Good to know I should be getting some Sr(NO3)2. I guess I'll add water continue and boiling again after work.
I was wondering if I covered the pot, it would allow the gas to escape , but maybe some of the water would condense and drip back in, so I won't have to top it up as much?

[YT2095]

it`s generally best to boil it open so the Am dissipates better, and then top it up with boiling water from the kettle.
I gotta ask though, you ARE boiling this in a Glass vessel yes?

[Bonny]

it`s generally best to boil it open so the Am dissipates better, and then top it up with boiling water from the kettle.
I gotta ask though, you ARE boiling this in a Glass vessel yes?

OK, no lid then. I'll get a kettle handy for topping off, then my solution doesn't need to heat up again each time I add more water...should have thought of that one. I was boiling it in a glass pot, corning visionware or whatever its called on an electric hot plate.

[YT2095]

that`s perfect then and by the book

sometimes metals (depending on the metal(s)) can form unfavorable complexes and bork the whole rxn up
happily though, because the rxn is quite sluggish to "rewind" you don`t end up with piles of Am gas threatening to choke you as you would with Other Bases of a higher PH.

I will point out that as mentioned before you CAN use vinegar to make Strontium Acetate and then the Nitrate, leaving ammonium acetate, however that breaks down quite easily to acetamide that has been shown to cause cancer in Lab animals, however you`re not without experience so I`m more than confident you`ll be quite safe IF you go that route

[richard2]

You can also use potassium nitrate to leave potassium acetate and so avoid the above problem. I have not looked up the respective solubilities in order to see if this is viable for the strontium salt. Pottasium acetate is highly soluble as is strontium nitrate whereas with the barium nitrate reaction you can take advantage of the barium salts relativly low solubility.

Regards


Rich

[YT2095]

Rich: Potassium acetate solubility is: 256g/100ml
Strontium acetate is: 41.1g/100ml

again, hope that`s helpful to you

[richard2]

Thanks

I reckon that this method (via acetate) is probably not worth it for the strontium salt as you will lose so much product during seperation and recrystallisation.

Although i like making some of the materiels I use I have to say I buy strontium nitrate. However if I were to make it from the carbonate it would have to be from HNO3 - are you sure you can't purchase even dilute acid from a hydrophonics store (make sure you don't end up with phosphoric).

Regards


Rich

[YT2095]

in the UK you can buy it, I normally buy about 4L at a time each year or so, and even at 38% conc for many things you have to Dilute it (I like extracting metals from Minerals so I do use quite a bit, and I also tailor make my own plant foods for my Veggies).

Phosphoric has it`s place too, but even for my needs a liter bottle of 81% conc is likely to last me a good 5+ years

[Bonny]

I'd love to buy strontium nitrate, but have no local source.Also, the challenge of making some of my own chems is rewarding when it works, as well as good learning.I'll definately be checking hydroponic shops, as I know it is easier to make nitrates from HNO3. I have one source for HNO3 but it is verrrry expensive. For now I'm trying to make due with what I have...frustrating sometimes though.
I did try to make barium nitrate form acetic acid and KNO3 a year or so ago. At the time I didn't really know what I was doing so it didn't work for me. If I can't source any (cheaper) HNO3 it may be my only option in the future though.

[YT2095]

I think the best thing to do is a simple calc, price up the nitric and the carbonate, then work out the yield from that, then compare that combined price to the Ba(NO3)2 sellers charge + P&P.

and although as you mentioned a few posts ago that you can make Nitric from AN and Sulphuric, you still have to distill this off! and that require ALL Glass distillation apparatus and a great deal of care!
as I said, you cannot present ANY sulphate around a barium salt, you`ll render it entirely Useless!

and even when you distill the nitric off you Then have to dilute it to about 25% (you get roughly 70% after distilling) and then it costs you the heat/fuel to get that 70% etc.. etc...

you`re much better off (and safer) buying it and making your own barium nitrate IF it turns out to be cheaper than the seller of the finished product.

and yes seriously even the 38% nitric I buy from Hydroponics is still to concentrated, you need to add it to some water

Edited by YT2095, 01 October 2007 - 04:03 PM.

[Bonny]

My main concern getting Sr and Ba nitrates is customs seizing them. 1l of 70% HNO3 costs me about $60 CDN including shipping. Seems to be only phosphoric available in local hydro shops.
For now I don't think I'm ready (equipment or knowledge)to try and make HNO3 from H2SO4 and any nitrate.The Sr(NO3)2 I'm trying to make right now seems very time consuming, but an interesting experiment all the same. I'll likely end up buying more HNO3 and going that route, but was looking for another possible way.

Edited by Bonny, 01 October 2007 - 04:43 PM.