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How can one fully dissolve zirconium oxynitrate in water?
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+ Inorganic chemistry
+ Dissolution
+ Stock solution
+ Sol-gel
+ Zirconium
+ Nitric acid
Posted by
Matthew Dubeau
How can one fully dissolve zirconium oxynitrate in water?
Hi Roman, I actually use aqueous solutions of this salt quite frequently in my work, so hopefully I can be of some help. In the past, I have purchased the Zr oxynitrate salt from Sigma-Aldrich, which comes as a mixture of large clumps and fine powder (I have not purchased the Zr oxynitrate salt from Alfa Aesar, but I am assuming that this is the same/similar). The fine powder dissolves more readily than the large clumps, so I will crush the large clumps using a mortar/pestle or selectively weigh out only the fine powder. Then I will heat a vigorously stirring solution of water to near boiling (probably 80-90 degrees C). I then add small portions of the salt to the water, waiting until the salt is fully dissolved before adding the next portion. After I add the last of the salt, I will let this solution stir for 30-60 minutes. (note: if you heat this solution too long, it will congeal and you will never get your stir bar back!). I will then let the solution cool to R. T. (still stirring) and then dilute appropriately to whatever concentration I am aiming for (using a volumetric flask). The solution will still be slightly cloudy, but filtering with 0.45 um syringe filters will yield a clear, colorless solution. Good luck. Let me know if this works for you! P.S. I have a manuscript in preparation that details this procedure. Hopefully it will be out soon!
Hi Roman, I actually use aqueous solutions of this salt quite frequently in my work, so hopefully I can be of some help. In the past, I have purchased the Zr oxynitrate salt from Sigma-Aldrich, which comes as a mixture of large clumps and fine powder (I have not purchased the Zr oxynitrate salt from Alfa Aesar, but I am assuming that this is the same/similar). The fine powder dissolves more readily than the large clumps, so I will crush the large clumps using a mortar/pestle or selectively weigh out only the fine powder. Then I will heat a vigorously stirring solution of water to near boiling (probably 80-90 degrees C). I then add small portions of the salt to the water, waiting until the salt is fully dissolved before adding the next portion. After I add the last of the salt, I will let this solution stir for 30-60 minutes. (note: if you heat this solution too long, it will congeal and you will never get your stir bar back!). I will then let the solution cool to R. T. (still stirring) and then dilute appropriately to whatever concentration I am aiming for (using a volumetric flask). The solution will still be slightly cloudy, but filtering with 0.45 um syringe filters will yield a clear, colorless solution. Good luck. Let me know if this works for you! P.S. I have a manuscript in preparation that details this procedure. Hopefully it will be out soon!
Hi, I usually dissolve 0.1g ZrO(NO3)2.6H2O (from Sigma aldrich) in 5 ml of distilled water in closed container on stirrer (in room temperature for 10 min). most of the time it dissolve totally, and sometimes almost (!!!!). i dont know what is the different of these days, but increasing the time of stirring doesnt work to have a better dissolving, i increase the temperature up to 40C and still it doesnt dissolve completely. i should tell you that if i add another nitrate to zirconyl nitrate and then want to dissolve them in water together, they wont dissolve at all,even in 10ml of water. i attached a paper about solubility of zirconyl nitrate.I hope that it will help you.
Hi, I usually dissolve 0.1g ZrO(NO3)2.6H2O (from Sigma aldrich) in 5 ml of distilled water in closed container on stirrer (in room temperature for 10 min). most of the time it dissolve totally, and sometimes almost (!!!!). i dont know what is the different of these days, but increasing the time of stirring doesnt work to have a better dissolving, i increase the temperature up to 40C and still it doesnt dissolve completely. i should tell you that if i add another nitrate to zirconyl nitrate and then want to dissolve them in water together, they wont dissolve at all,even in 10ml of water. i attached a paper about solubility of zirconyl nitrate.I hope that it will help you.
Hi Roman, I actually use aqueous solutions of this salt quite frequently in my work, so hopefully I can be of some help. In the past, I have purchased the Zr oxynitrate salt from Sigma-Aldrich, which comes as a mixture of large clumps and fine powder (I have not purchased the Zr oxynitrate salt from Alfa Aesar, but I am assuming that this is the same/similar). The fine powder dissolves more readily than the large clumps, so I will crush the large clumps using a mortar/pestle or selectively weigh out only the fine powder. Then I will heat a vigorously stirring solution of water to near boiling (probably 80-90 degrees C). I then add small portions of the salt to the water, waiting until the salt is fully dissolved before adding the next portion. After I add the last of the salt, I will let this solution stir for 30-60 minutes. (note: if you heat this solution too long, it will congeal and you will never get your stir bar back!). I will then let the solution cool to R. T. (still stirring) and then dilute appropriately to whatever concentration I am aiming for (using a volumetric flask). The solution will still be slightly cloudy, but filtering with 0.45 um syringe filters will yield a clear, colorless solution. Good luck. Let me know if this works for you! P.S. I have a manuscript in preparation that details this procedure. Hopefully it will be out soon!
Hi Roman, I actually use aqueous solutions of this salt quite frequently in my work, so hopefully I can be of some help. In the past, I have purchased the Zr oxynitrate salt from Sigma-Aldrich, which comes as a mixture of large clumps and fine powder (I have not purchased the Zr oxynitrate salt from Alfa Aesar, but I am assuming that this is the same/similar). The fine powder dissolves more readily than the large clumps, so I will crush the large clumps using a mortar/pestle or selectively weigh out only the fine powder. Then I will heat a vigorously stirring solution of water to near boiling (probably 80-90 degrees C). I then add small portions of the salt to the water, waiting until the salt is fully dissolved before adding the next portion. After I add the last of the salt, I will let this solution stir for 30-60 minutes. (note: if you heat this solution too long, it will congeal and you will never get your stir bar back!). I will then let the solution cool to R. T. (still stirring) and then dilute appropriately to whatever concentration I am aiming for (using a volumetric flask). The solution will still be slightly cloudy, but filtering with 0.45 um syringe filters will yield a clear, colorless solution. Good luck. Let me know if this works for you! P.S. I have a manuscript in preparation that details this procedure. Hopefully it will be out soon!
You can also dissolve in acidic water (HNO3), filtrate and evaporate. The obtained salt should be fully soluble then. If your Zr salt contains impurites insoluble in water, at least you get rid of them.
You can also dissolve in acidic water (HNO3), filtrate and evaporate. The obtained salt should be fully soluble then. If your Zr salt contains impurites insoluble in water, at least you get rid of them.
@Visot Mao, I have sigma aldrich one, it's written on the box of product (x~~6) you can check it in sigma aldrich website also (Degree of hydration, ~6 ) which i send you the address of this page below. I hope it will be useful for you http://www.sigmaaldrich.com/catalog/product/aldrich/243493?lang=en®ion=IR
@Visot Mao, I have sigma aldrich one, it's written on the box of product (x~~6) you can check it in sigma aldrich website also (Degree of hydration, ~6 ) which i send you the address of this page below. I hope it will be useful for you http://www.sigmaaldrich.com/catalog/product/aldrich/243493?lang=en®ion=IR
@ Visot Mao, that should not be too difficult to find out. Take some not too small amount of your chemical, weigh it with a crucible, and calcinate at a temperature of, say, 1000°C. You'll find the amount of zirconia produced from the initial oxynitrate - the rest is simple maths.
@ Visot Mao, that should not be too difficult to find out. Take some not too small amount of your chemical, weigh it with a crucible, and calcinate at a temperature of, say, 1000°C. You'll find the amount of zirconia produced from the initial oxynitrate - the rest is simple maths.
@Faeza Soroush, I saw you mentioned that your Zirconium(IV) oxynitrate hydrate possesses x = 6. I just want to reconfirm with you how you are able to determine the x because at my lab, I use the same product from the same supplier and my collegue told me that the x = 5. However, I checked in literature and I saw some authors used this product but from different suppliers and they found x to be 2.3 . So, I just want to know what is the right value of x for this product because i don't want to miscalculate the weight of the precusor which will be used in my experiments. Thank you in advance for your reply.
@Faeza Soroush, I saw you mentioned that your Zirconium(IV) oxynitrate hydrate possesses x = 6. I just want to reconfirm with you how you are able to determine the x because at my lab, I use the same product from the same supplier and my collegue told me that the x = 5. However, I checked in literature and I saw some authors used this product but from different suppliers and they found x to be 2.3 . So, I just want to know what is the right value of x for this product because i don't want to miscalculate the weight of the precusor which will be used in my experiments. Thank you in advance for your reply.
Zirconium oxynitrate has a rather low solubility. I would suggest to convert it to zirconium tetranitrate pentahydrate, by mixing the oxynitrate with concentrated HNO3 and stirring for several hours until the solution becomes clear. Then, evaporate the liquid at temperatures under 100°C to get the well soluble tetranitrate pentahydrate.
Zirconium oxynitrate has a rather low solubility. I would suggest to convert it to zirconium tetranitrate pentahydrate, by mixing the oxynitrate with concentrated HNO3 and stirring for several hours until the solution becomes clear. Then, evaporate the liquid at temperatures under 100°C to get the well soluble tetranitrate pentahydrate.
Thanks for sharing! I've recently salvaged milkywhite and partly congeled solutions of fairly old ZrO-nitrate by adding 1 mole citric acid per mole Zr and adjusting pH to ~5.5 by adding ammonia.
Thanks for sharing! I've recently salvaged milkywhite and partly congeled solutions of fairly old ZrO-nitrate by adding 1 mole citric acid per mole Zr and adjusting pH to ~5.5 by adding ammonia.
Hi Roman,
I actually use aqueous solutions of this salt quite frequently in my work, so hopefully I can be of some help.
In the past, I have purchased the Zr oxynitrate salt from Sigma-Aldrich, which comes as a mixture of large clumps and fine powder (I have not purchased the Zr oxynitrate salt from Alfa Aesar, but I am assuming that this is the same/similar). The fine powder dissolves more readily than the large clumps, so I will crush the large clumps using a mortar/pestle or selectively weigh out only the fine powder. Then I will heat a vigorously stirring solution of water to near boiling (probably 80-90 degrees C). I then add small portions of the salt to the water, waiting until the salt is fully dissolved before adding the next portion. After I add the last of the salt, I will let this solution stir for 30-60 minutes. (note: if you heat this solution too long, it will congeal and you will never get your stir bar back!). I will then let the solution cool to R. T. (still stirring) and then dilute appropriately to whatever concentration I am aiming for (using a volumetric flask). The solution will still be slightly cloudy, but filtering with 0.45 um syringe filters will yield a clear, colorless solution.
Good luck. Let me know if this works for you!
P.S. I have a manuscript in preparation that details this procedure. Hopefully it will be out soon!
Hi Roman,
I actually use aqueous solutions of this salt quite frequently in my work, so hopefully I can be of some help.
In the past, I have purchased the Zr oxynitrate salt from Sigma-Aldrich, which comes as a mixture of large clumps and fine powder (I have not purchased the Zr oxynitrate salt from Alfa Aesar, but I am assuming that this is the same/similar). The fine powder dissolves more readily than the large clumps, so I will crush the large clumps using a mortar/pestle or selectively weigh out only the fine powder. Then I will heat a vigorously stirring solution of water to near boiling (probably 80-90 degrees C). I then add small portions of the salt to the water, waiting until the salt is fully dissolved before adding the next portion. After I add the last of the salt, I will let this solution stir for 30-60 minutes. (note: if you heat this solution too long, it will congeal and you will never get your stir bar back!). I will then let the solution cool to R. T. (still stirring) and then dilute appropriately to whatever concentration I am aiming for (using a volumetric flask). The solution will still be slightly cloudy, but filtering with 0.45 um syringe filters will yield a clear, colorless solution.
Good luck. Let me know if this works for you!
P.S. I have a manuscript in preparation that details this procedure. Hopefully it will be out soon!
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I also contacted Alfa's staff and they told me there is a little Cl- residual. Can anybody tell me the content of residual Cl-?
I also contacted Alfa's staff and they told me there is a little Cl- residual. Can anybody tell me the content of residual Cl-?
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Hi,
I usually dissolve 0.1g ZrO(NO3)2.6H2O (from Sigma aldrich) in 5 ml of distilled water in closed container on stirrer (in room temperature for 10 min).
most of the time it dissolve totally, and sometimes almost (!!!!).
i dont know what is the different of these days, but increasing the time of stirring doesnt work to have a better dissolving, i increase the temperature up to 40C and still it doesnt dissolve completely.
i should tell you that if i add another nitrate to zirconyl nitrate and then want to dissolve them in water together, they wont dissolve at all,even in 10ml of water.
i attached a paper about solubility of zirconyl nitrate.I hope that it will help you.
Hi,
I usually dissolve 0.1g ZrO(NO3)2.6H2O (from Sigma aldrich) in 5 ml of distilled water in closed container on stirrer (in room temperature for 10 min).
most of the time it dissolve totally, and sometimes almost (!!!!).
i dont know what is the different of these days, but increasing the time of stirring doesnt work to have a better dissolving, i increase the temperature up to 40C and still it doesnt dissolve completely.
i should tell you that if i add another nitrate to zirconyl nitrate and then want to dissolve them in water together, they wont dissolve at all,even in 10ml of water.
i attached a paper about solubility of zirconyl nitrate.I hope that it will help you.
More
VOTE
Hi Roman,
I actually use aqueous solutions of this salt quite frequently in my work, so hopefully I can be of some help.
In the past, I have purchased the Zr oxynitrate salt from Sigma-Aldrich, which comes as a mixture of large clumps and fine powder (I have not purchased the Zr oxynitrate salt from Alfa Aesar, but I am assuming that this is the same/similar). The fine powder dissolves more readily than the large clumps, so I will crush the large clumps using a mortar/pestle or selectively weigh out only the fine powder. Then I will heat a vigorously stirring solution of water to near boiling (probably 80-90 degrees C). I then add small portions of the salt to the water, waiting until the salt is fully dissolved before adding the next portion. After I add the last of the salt, I will let this solution stir for 30-60 minutes. (note: if you heat this solution too long, it will congeal and you will never get your stir bar back!). I will then let the solution cool to R. T. (still stirring) and then dilute appropriately to whatever concentration I am aiming for (using a volumetric flask). The solution will still be slightly cloudy, but filtering with 0.45 um syringe filters will yield a clear, colorless solution.
Good luck. Let me know if this works for you!
P.S. I have a manuscript in preparation that details this procedure. Hopefully it will be out soon!
Hi Roman,
I actually use aqueous solutions of this salt quite frequently in my work, so hopefully I can be of some help.
In the past, I have purchased the Zr oxynitrate salt from Sigma-Aldrich, which comes as a mixture of large clumps and fine powder (I have not purchased the Zr oxynitrate salt from Alfa Aesar, but I am assuming that this is the same/similar). The fine powder dissolves more readily than the large clumps, so I will crush the large clumps using a mortar/pestle or selectively weigh out only the fine powder. Then I will heat a vigorously stirring solution of water to near boiling (probably 80-90 degrees C). I then add small portions of the salt to the water, waiting until the salt is fully dissolved before adding the next portion. After I add the last of the salt, I will let this solution stir for 30-60 minutes. (note: if you heat this solution too long, it will congeal and you will never get your stir bar back!). I will then let the solution cool to R. T. (still stirring) and then dilute appropriately to whatever concentration I am aiming for (using a volumetric flask). The solution will still be slightly cloudy, but filtering with 0.45 um syringe filters will yield a clear, colorless solution.
Good luck. Let me know if this works for you!
P.S. I have a manuscript in preparation that details this procedure. Hopefully it will be out soon!
More
VOTE
You can also dissolve in acidic water (HNO3), filtrate and evaporate. The obtained salt should be fully soluble then. If your Zr salt contains impurites insoluble in water, at least you get rid of them.
You can also dissolve in acidic water (HNO3), filtrate and evaporate. The obtained salt should be fully soluble then. If your Zr salt contains impurites insoluble in water, at least you get rid of them.
More
VOTE
@Visot Mao,
I have sigma aldrich one, it's written on the box of product (x~~6)
you can check it in sigma aldrich website also (Degree of hydration, ~6 ) which i send you the address of this page below.
I hope it will be useful for you
http://www.sigmaaldrich.com/catalog/product/aldrich/243493?lang=en®ion=IR
@Visot Mao,
I have sigma aldrich one, it's written on the box of product (x~~6)
you can check it in sigma aldrich website also (Degree of hydration, ~6 ) which i send you the address of this page below.
I hope it will be useful for you
http://www.sigmaaldrich.com/catalog/product/aldrich/243493?lang=en®ion=IR
More
VOTE
@ Visot Mao, that should not be too difficult to find out. Take some not too small amount of your chemical, weigh it with a crucible, and calcinate at a temperature of, say, 1000°C. You'll find the amount of zirconia produced from the initial oxynitrate - the rest is simple maths.
@ Visot Mao, that should not be too difficult to find out. Take some not too small amount of your chemical, weigh it with a crucible, and calcinate at a temperature of, say, 1000°C. You'll find the amount of zirconia produced from the initial oxynitrate - the rest is simple maths.
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@ Junming Sun, this was one of the first things we tried and did not at all help
@ Junming Sun, this was one of the first things we tried and did not at all help
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@Faeza Soroush, I saw you mentioned that your Zirconium(IV) oxynitrate hydrate possesses x = 6. I just want to reconfirm with you how you are able to determine the x because at my lab, I use the same product from the same supplier and my collegue told me that the x = 5. However, I checked in literature and I saw some authors used this product but from different suppliers and they found x to be 2.3 .
So, I just want to know what is the right value of x for this product because i don't want to miscalculate the weight of the precusor which will be used in my experiments.
Thank you in advance for your reply.
@Faeza Soroush, I saw you mentioned that your Zirconium(IV) oxynitrate hydrate possesses x = 6. I just want to reconfirm with you how you are able to determine the x because at my lab, I use the same product from the same supplier and my collegue told me that the x = 5. However, I checked in literature and I saw some authors used this product but from different suppliers and they found x to be 2.3 .
So, I just want to know what is the right value of x for this product because i don't want to miscalculate the weight of the precusor which will be used in my experiments.
Thank you in advance for your reply.
More
VOTE
Use ultrasonic, you should be able to get a clear solution within 30min
Use ultrasonic, you should be able to get a clear solution within 30min
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Zirconium oxynitrate has a rather low solubility. I would suggest to convert it to zirconium tetranitrate pentahydrate, by mixing the oxynitrate with concentrated HNO3 and stirring for several hours until the solution becomes clear. Then, evaporate the liquid at temperatures under 100°C to get the well soluble tetranitrate pentahydrate.
Zirconium oxynitrate has a rather low solubility. I would suggest to convert it to zirconium tetranitrate pentahydrate, by mixing the oxynitrate with concentrated HNO3 and stirring for several hours until the solution becomes clear. Then, evaporate the liquid at temperatures under 100°C to get the well soluble tetranitrate pentahydrate.
More
VOTE
Thanks for sharing! I've recently salvaged milkywhite and partly congeled solutions of fairly old ZrO-nitrate by adding 1 mole citric acid per mole Zr and adjusting pH to ~5.5 by adding ammonia.
Thanks for sharing! I've recently salvaged milkywhite and partly congeled solutions of fairly old ZrO-nitrate by adding 1 mole citric acid per mole Zr and adjusting pH to ~5.5 by adding ammonia.
More
VOTE