Table 2 Key parameters and variables to report in autoclave reactor synthesis in order to maximise reproducibility
| Â | Key parameter/variable | Importance |
|---|---|---|
General autoclave reactor operation | Make and model of autoclave reactor. | Reproducibility and repeatability by others. |
Make and model of autoclave reactor heating system. | Â | |
Maximum heat and pressure specified by manufacturers. | Understanding limits of reactor equipment. | |
Reactor and sleeve cleaning procedure. | May help identify potential issues with contamination. | |
Safety precautions. | Ensuring safety and sharing good practice. | |
Reaction containment and liner | Autoclave reactor chamber volume when empty. | Pressure of reaction depends on volume available for gas generation and expansion. |
Autoclave chamber volume once liner is inserted. | Â | |
Volume of liner. | Â | |
Total volume of reaction mixture added within liner (i.e., fill factor). | Â | |
Liner material. | Influences heat transfer rate. | |
Does the liner have a lid? | If not fully enclosed, gas may expand into autoclave headspace; possible contamination risk. | |
Was an inert atmosphere introduced? | Inert atmospheres may benefit UCNP luminescence. | |
Stirring | Was the reaction mixture stirred? If so, at what rate? | May alter the size of any micelles present in hydrothermal reactions. |
What size and shape of stir bar was used? | Influences chamber volume. | |
Heating and temperature | Autoclave reactor construction materials. | Construction materials influence heat transfer rate. |
Heat source (e.g., oven, hotplate, heating mantle, etc). | Governs heating uniformity and heating rate. | |
Heating control method and target temperature. | Heat delivery rate is a key variable in synthesis. | |
Is the heating control and target temperature based on internal or external temperature? | External temperature and reactor internal temperature are different due to heat differentials. Reactor internal temperature lags behind external temperature. | |
Was the reactor pre-heated? | Influences the heating rate and total energy in the system. | |
When is the reaction timer deemed to have started? | Determines total energy input into the reaction mixture. | |
Was temperature data logged as the reaction occurred? | Aids repeatability and troubleshooting. | |
Heating rate. | Aids repeatability and troubleshooting. | |
Pressure | Does the autoclave reactor have a pressure gauge? | Pressure generated may be important for synthesis outcomes. |
What was the internal reactor pressure during the reaction? | Pressure generated may be important for synthesis outcomes. |
