Basically i have question about the capacity of the autoclave. Like there are many sizes i.e., 25 ml, 50 ml and 1000 ml etc. How can we chose among these autoclaves? On what things does this capacity is depended? Is it the amount or precursor or what?
Dear Mohammed,
with different capacity autoclaves you can scale up or scale down you precursor amount depending on the yield you needed.
Typically when you do hydrothermal synthesis, you may have to follow certain safety operation procedures (SOP). You can refer SOP for Autoclaves when used hydrothermal synthesis.
important things you should take care is
1: the volume of the total solvent should not exceed 80% (70 to 75% better)
2: never put the autoclave in high temperature furnace. always use oven
3: always check with the vendor for the maximum pressure, the autoclave can sustain
4: optimize your condition when using volatile solvent (can generate more gases and exert more pressure )
wish you the best
Dear Waqar,
In simple terms, choosing the size of autoclave depends on what scale of process you want to study and what is your system. There are no hard and fast rules.
In my experience, 500-1000 ml is a safe and good representative size for lab scale processes.
All the best!
It depends on your study. We use Acid-Parr digestion bomb which has volume as 23 mL and including teflon cup for metal-organic compounds. The important point is fill rate!
Good luck!
You can see some details about the bomb at below website:
"http://www.parrinst.com/wp-content/uploads/downloads/2011/06/4700MB_Parr_Sample-Preparation-Vessels-Literature.pdf"
As it has been pointed the total volume of your autoclave determines the scale of your process. But, more important than that is, as Emel said, the percentage of volume filled. If you are working with autogenous pressure (the pressure generated when heating the autoclave), the pressure will depend on the percentage of free volume of the system (among other factors as temperature, and solvent). So you need to consider that as well when choosing the total volume of your autoclave.
Best wishes!
Typically filling rate is 70 to 75 percent of the total volume of the autoclave or Teflon beaker. If I chose lets suppose 100 ml autoclave than I must use proportional molarity of my precursor which is used for 25 ml (say). Am I right?
it is mainly depend upon how much amount of catalyst you want to synthesis and you have keep in mind that you autoclave should not be completely filled you can use maximum 80% volume of your autoclave.
Dear Muhammad
For the wet chemical Hydrothermal synthesis, the volume of autoclave mainly depends on:1) The starting materials type and initial amounts 2) The Solvent type and its pressure at final pressure 4) The maximum pressure of the reaction 5) The amount of target product.
Dear Mohammed,
with different capacity autoclaves you can scale up or scale down you precursor amount depending on the yield you needed.
Typically when you do hydrothermal synthesis, you may have to follow certain safety operation procedures (SOP). You can refer SOP for Autoclaves when used hydrothermal synthesis.
important things you should take care is
1: the volume of the total solvent should not exceed 80% (70 to 75% better)
2: never put the autoclave in high temperature furnace. always use oven
3: always check with the vendor for the maximum pressure, the autoclave can sustain
4: optimize your condition when using volatile solvent (can generate more gases and exert more pressure )
wish you the best
tous dépend de ce que vous voulez faire car pour une caractérisation il faut des petit volumes le cas contraire pour des applications.
I am using 50 ml autoclave.. But i am getting only 400 mg of yield.. But my precursors are 1.5 grams.. Can any one tell mw how can i get high yield?
If my paper mention 50mL autoclave and there is nothing mentioned about pressure then can I use 100mL autoclave in place of 50mL?
During hydrothermal synthesis, the volume of the total solvent should not exceed 80%
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