1. How much compound can be reduced on one catalyst column?
It depends on the type and the molecular weight of the compound. Also, the lifetime of the catalyst is affected by polarity, molecular weight, purity, solvent and types of functional groups, e.g. sulphur groups which may poison the catalyst. With the shortest column, on average, at least 500 mg is reduced, but we have reduced up to 10 g of certain compounds without any catalyst deactivation.
2. How do you dispose of a used CatCart®?
A deactivating vial containing a solution of sodium hydrogen sulfite comes with a CatCart® purchase. Once the CatCart® is finished with, it is placed in the deactivation vial and this renders the catalyst non-pyrophoric. You can dispose of the deactivated cartridge in the same way as you would heterogeneous catalyst from a batch reactor.
3. Is there any partially poisoned catalyst available?
A selection of poisoned catalysts for selective reduction are available, including Lindlar’s catalyst and Pt sulfided catalysts.
4. Can the catalyst in the CatCart® be used longer than the catalyst in a batch reactor?
In certain reactions, the product formed, e.g. primary amine, will bind strongly to the catalyst leading to deactivation overtime. In the H-Cube®, the deactivation will take place over a longer period of time because the deactivating product is always flowed out of the catalyst, so the product has a very short residence time on the catalyst. In a batch reactor, the product, starting material, and catalyst mixture are always in contact with each other throughout the entire experiment. As the product concentration increases, the deactivation of the catalyst will also increase.
5. How do we know that the catalyst is still active after repeated use?
You can either try one of the validation reactions (e.g. 5-nitroindole reduction) on a 50 mg scale, or you can make your reactions in more fractions, test the result of each, and recycle back the non-reduced fraction on a new column.
6. After a reaction, is there any problems that a catalyst is stored in original tube?
If you wish to store the CatCart® in the original vial, the vial must be filled with deionized water because if you let the catalyst dry, it will catch fire.
7. After a reaction, is it better to remove the catalyst from the H-Cube®?
ThalesNano recommends that the catalyst be removed at the end of the reaction after the system is washed.
8. Do you have a technique to avoid contamination?
Wash the system with pure solvent after each reaction for at least 10 minutes and then test using an LC or GCMS to see if there is any contaminant. If there is, wash for a further 10 minutes.
9. What is preservative solution of Raney Ni?
If you wish to store Raney Ni or any other catalyst after use, ALWAYS use deionized water. Never use acid with Raney Ni because you will dissolve the nickel.
10. Is it possible to use CatCarts® for H-Cube® on an H-Cube Midi™?
The cartridges for H-Cube® and H-Cube Midi™ are different sizes and so H-Cube® cartridges cannot be used on the H-Cube Midi™ system.
11. What kind of solvents cannot be used in the H-Cube®?
With the PEEK H-Cube®:
Marginally Suitable (these solvents do not attack the PEEK tubing but may cause swelling which may weaken the PEEK tubing)
Dimethyl sulfoxide (DMSO)
Not recommended (these chemicals will attack the PEEK tubing)
Hydrobromic acid (100%)
Hydrobromic acid (20%)
Hydrobromic acid (10%)
Hydrofluoric Acid (100%)
Nitric acid (100%)
Sulphuric acid (100%)
Sulphuric acid (70%)
With the SS H-Cube®
Usual solvents to be used are: EtOH, MeOH. Click here to see H-Cube® CatCart® solvent compatibility table. However, if you are still unsure please contact askthechemist/[at/]thalesnano.com.
Please note that AcCN should not be used as solvent since it may get hydrogenated instead or parallel with your starting material.
12. How viscous can a liquid be and still be pumped through a KNAUER analytical pump?
Maximum 1 Poise (CGS unit), i.e. 0.1 Pas (Pascal x sec, SI units), i.e. 100 mPa·s. This would correspond to the viscosity of oils. Liquids such as honey (100 Poise) can be pumped with a gear-type pump. Dynamic Viscosities of Newtonian Liquids at 20°C
|LIQUID||VISCOSITY (Centipoise)||VISCOSITY (Poise)|
|Ether (diethyl ether)||0.23||0.0023|
|Ethanol (ethyl alcohol)||1.19||0.0119|
|Joint sealing compound||>108||>106|
100 Centipoise = 1 Poise
1 Centipoise = 1 mPa s (milliPascal second)
1 Poise = 0.1 Pa s (Pascal second)
13. How pure is the Hydrogen and how much is the water content of it?
99.99% H2. A water separator is responsible for the removal of H2O.
14. Do you have any cross-contamination when using different compounds on the same cartridge?
If enough washing with fresh solvent and hydrogen is allowed between samples, e.g. 10 ml, to wash off any residual product from the column, there will be no cross-contamination. The amount of solvent used depends on how polar the compound is and the type of solvent used.
15. Do you have to de-gas the solvent before the reaction?
No, because the amount of O2 is so small.
16. How can you perform selective hydrogenation reactions?
Vary the pressure of hydrogen (Henry’s Law), temperature or use a more selective catalyst from the list.
17. What happens with the oxygen?
It is separated from the hydrogen by an SPE (Solid Polymer Electrolyte) membrane, and then recycled back out of cell with the water and then vented out the back of the instrument.
18. How many times is it recommended to top up the water level?
When full, the water reservoir has enough water to generate hydrogen for a full working week. However, for the sake of procedure, we recommend you check the water level every day, e.g. every morning before you start working with H-Cube®. The stainless steel model has a water level monitor on the touch screen.
19. Is there a safety shut-off if the water tank is empty?
Only on the the stainless steel version of the H-Cube. A message will appear warning the user that the water tank is empty and the user will not be allowed to operate the H-Cube® until the water tank has been refilled.
20. What happens if the cell runs dry?
The membrane inside the cell will dry out and it eventually causes the cell to malfunction.
21. What is the internal volume of hydrogen in the H-Cube®?
The internal volume of hydrogen at 1 bar is approximately 3 cm3, therefore at 100 bar it is 300 cm3.
22. What is the maximum H2 flow in the H-Cube®?
30 cm3/min (in Full H2 mode).
23. What is the volume of the reaction line in the H-Cube®?
The H-Cube reaction line volume is approximately 2.5 cm3 ,including a 30 mm CatCart®. When connected to the HPLC pump the total volume is 4 mL, therefore the time taken for the compound to pass through the reactor at 1mL/min is 4 minutes.
24. What happens if there is a H2 leak inside the machine?
There is a H2 detector, which automatically shuts down the H-Cube® when hydrogen is detected. The power supply is located in a separate unit outside of the H-Cube® box to remove the risk of sparks.
25. Does the machine stop automatically if the pressure goes higher than 100 bar?
No, but if the pressure exceeds 200 bar, the HPLC pump will stop with a blinking “57”, which results in the quick drop of the pressure.
26. How can I perform deuteration reactions in the H-Cube®?
To perform a deuteration reaction it is very important that as much H2O is removed from the system as possible.
Step 1: A stainless steel system is essential for this because it has the Purge water function on the service screen.
Step 2: Drain the water from the reservoir using a syringe.
Step 3: Remove the back of the water reservoir with the allan key. Clean and dry the insides with a paper towel.
Step 4: Go to the service screen. Press Purge water function and press stop at 10 seconds.
Step 5: Replace water reservoir. Add 30 mL of deuterated water. Press Purge Water for 10 seconds.
Step 6: Undo water reservoir, dry insides, again and press Purge water for 10 seconds again.
Step 7: Replace water reservoir and fill with deuterated water. Press Purge water to refill cell with D2O.
Step 8: Take a blank cartridge(titanium) and pass an aprotic solvent (a solvent which doesn’t have OH or COOH in the structure) and run the system at Full H2 mode for 10 minutes. Remove blank cartridge.
System is now ready for deuteration experiment.
Deuterated water absorbs water from the air rapidly, so the water reservoir hole must be sealed when not in use. It may be best to have the hole sealed and have a nitrogen stream going into the hole through a needle. Make sure there is another needle allowing the N2 and O2 out again.
The water separator will handle D2O as well as H2O.
The solvent and catalyst used is very important. As mentioned above the solvent should have no OH’s or COOH’s or any group that can donate a hydrogen. Deuterium and Hydrogen undergo exchange readily. Solvents like toluene are readily used for reactions such as this.
The catalyst is also important. Avoid Raney catalysts because they come presaturated with hydrogen. A fresh Pd or Pt should do the trick.
27. What is the minimum size of the reaction when H-Cube Midi™ is used?
Due to the large amount of catalyst in the cartridge going below 500 mg in scalein not advised. Microgram quantities are not suitable for the H-Cube Midi™, the compound would stick to the catalyst and it would not come off.
28. What can I do if ThalesNano doesn’t supply the catalyst that I want?
If you describe what you want, ThalesNano can prepare it for you. Ask firstname.lastname@example.org for details.
29. What can I do if I encounter a system problem (e.g. hydrogen leaking, no solvent is coming out from the reactor)?
Please read the user manual for directions. It tells you what do to with the different problems you may encounter. If you can not solve your problem or the user manual recommends, please contact us at email@example.com.
30. What instruments can be used with the Gas Module?
You can connect the Gas Module to the H-Cube Pro and H-Cube so far.
31. What is the difference when it is connected to H-Cube and H-Cube Pro?
The software of H-Cube Pro can monitor and control the Gas Module, as an External module. When the Gas Module is connected to the H-Cube the unit must be utilized as a stand alone system. There are several safety features implemented into both software.
32. Can the hydrogen generated by the H-Cube or H-Cube Pro be used when utilizing the Gas Module?
For safety reasons, the H-Cube must be used in No Gas mode so there will not be any hydrogen generated by the cell in the reaction line. When the Gas Module is connected to the H-Cube Pro, its software automatically blocks the introduction and generation of hydrogen.
33. Does the Gas Module generate the 12 gases itself?
No. The Gas Module actually does not generate any gases, it only regulates the amount of gas coming from the cylinder.
34. How many gases can be introduced into the system at one time?
Only one cylinder can be used at a time, so the amount of gases depends on the gas type in the cylinder. E.g. gas mixtures such as SynGas can be introduced.
35. At what pressures can I use each gas?
Only gas can be introduced into the Gas Module, you have to make sure the gas pressure is under the vapor pressure. Reaction pressure has to be approximately 15 bar lower than the pressure of the tank.
Vapor pressure of each gas is given in the below table.
|Gas Name||Gas Type||Vapor Pressure|
|Ethane||C2H6||543 psi (37 bar)|
|Nitrous Oxide||N2O||736 psi (50 bar) at 20°C|
|Nitric Oxide||NO||508 psi (35 bar) at 20°C|
|Gas Name||Gas Type||Max flow rate(ml/min)||Max flow rate(mmol/min)||Max flow rate(mg/min)|
37. How is the gas pressure generated?
The reaction pressure is set on the H-Cube or H-Cube Pro, between atmospheric pressure and 100 bar. The gas cylinder pressure must be above the inlet pressure of the H-Cube. No compressor is used. Please ensure the gas source is able to maintain a pressure above the H-Cube inlet pressure above the entire duration of the reaction.
38. Can I use cylinder with dip tube installed?
No. Only dry gases can be introduced into the Gas Module. The use of wet gases is also not allowed.
39. How does the Gas Module connect to the standard H-Cube?
The Gas Module is connected to the H-Cube through a check valve supplied by ThalesNano. This check valve
is connected to the front panel of the H-Cube, as shown on the picture below.
The H-Cube and Gas Module are each controlled separately by their own built in software.
40. Do I need any upgrade on the H-Cube system to be able to use the H-Cube or H-Cube Pro with the Gas Module?
None of the standard H-Cubes needs any upgrade, but any H-Cube Pros with a serial number below 41 will. Upgrades will be given free of charge upon purchase of a Gas Module.
41. What else do I need to use the Gas Module with the H-Cube?
You will need a gas cylinder with a pressure regulator on attached. The external fitting should be able to connect to a 1/8 stainless steel tube.
42. What is the maximum pressure the cylinder can be set without damaging the Gas Module?
A maximum of 200 bar should be applied.
44. Can I use the Phoenix Flow Reactor without connecting it to any other device?
No, the Phoenix Flow Reactor requires liquid feed and a back pressure supplier to maintain the introduced liquid in solution phase. We recommend connecting the Phoenix Flow Reactor with either an H-Cube Pro, H-Cube, X-Cube or H-Cube Midi.
45. What is the difference between connecting it to an H-Cube/X-Cube/H-Cube Midi compared to connecting it to an H-Cube Pro?
If the Phoenix Flow Reactor is connected to an H-Cube/X-Cube/H-Cube Midi, then the Phoenix Flow Reactor is operated separately from the H-Cube/X-Cube/H-Cube Midi. The liquid flow and reaction pressure are set on the H-Cube/X-Cube/H-Cube Midi, just as usual, while the temperature of the Phoenix Flow Reactor is set on the Phoenix Flow Reactor, using the PID controllers on the front panel of the system.
If the Phoenix Flow Reactor is connected to an H-Cube Pro, the software of the H-Cube Pro controls the Phoenix Flow Reactor completely.
46. Can I introduce gas into the Phoenix Flow Reactor?
Yes. The best way to do so in case of a hydrogenation reaction is if you connect the Phoenix Flow Reactor to an H-Cube Pro/H-Cube. In case of other types of gas reactions, the addition of a Gas Module is recommended.
47. What types of chemistry can be performed with the Phoenix Flow Reactor?
Both homogeneous and heterogeneous (bi and triphasic) reactions.
48. Can I do multistep reactions when the Phoenix Flow Reactor is connected to the H-Cube Pro/H-Cube/X-Cube/H-Cube Midi?
Yes, it is possible to run a reaction either first in the Phoenix Flow Reactor then in the cartridge of the other device or first in the other device followed by a reaction in the Phoenix Flow Reactor.
49. What is the maximum temperature and pressure that can be reached?
450°C and 100 bar, please check specifications of the heated elements and ensure you use solvents below the boiling at any pressure.
50. What type of heated elements can be placed into the Phoenix Flow Reactor?
Both columns and loops can be placed into the heated area.
51. What type of columns can be placed into the Phoenix Flow Reactor and what are the limits of these columns in terms of temperature and pressure?
1.) Graphite sealed H-Cube Pro type CatCarts: 250 °C and 100 bar
2.) High Temperature Metal-Metal sealed columns: 450°C and 100 bar
3.) MidiCarts: 150°C and 100 bar
52. What is the basic set up of the system?
The general setting up contains 4 main parts:
Dual pump system
53. Can I use more pumps?
Yes, and it can be controlled by the control unit as well.
54. Are there any preferred configurations?
By default the control unit provides you the following predefined configuration:
Ozonolysis (2 pumps are used and the Ozone Module)
2 pumps 1 reactor zone (2 pumps and the main reactor zone are in use)
3 pumps 2 reactor zones (3 pumps and both reactor zones are in use)
55. Can I add my own configurations?
Yes, you can built in your own configuration in the software.
56. How easy is it to make the system ready physically for these configurations e.g. change from mixture of 2 liquids to mixing liquid with ozone for ozonolysis?
You only need to include a mixer and other Teflon tubing to supply either a liquid or a gas, which takes only a few minutes to do.
57. What happens if I get a blockage?
Standard Teflon tubing is utilized, so this may be cheaply replaced using a pair of scissors instead of having to buy a new expensive glass reactor.
58. How can you vary the reaction zone for scaling up?
You can change to another reaction volume easily in seconds. The length or internal diameter of the reaction line may be changed by swapping over reactor plates.
59. What does the reaction area look like?
You can use either 1/8” or 1/16” Teflon tubes embedded in a plate. The plate has grooves so changing the coil takes only few minutes and is much cheaper than buying a new chip reactor.
60. What solvents can be used?
All the wetted parts of the system is made of Teflon, which can tolerate even strong acids.
61. Can I perform reactions require inert conditions?
Yes, e.g. lithiation where the BuLi require inert atmosphere has been already successfully run.
62. Can you react other gases to perform different reactions?
You can introduce other gases to perform e.g. oxidation under pressure up to 6 bar.
63. Can I directly replace this Micro HPLC Pump with the existing one I am currently using with my H-Cube/H-Cube Pro?
Yes, both the H-Cube and the H-Cube Pro can control the new, Micro HPLC Pump
64. Can I use the Micro HPLC Pump with the Manual Injection System?
Yes, exactly in the same way as with your current pump.
65. What is the flow rate range of the Micro HPLC Pump?
Independently from the H-Cube or H-Cube Pro systems the pump flow rate range is: 0.01-10 mL/min. When the pump is connected to the H-Cube, then it is limited to 0.1-3 mL/min. With the H-Cube Pro it is 0.3-3 mL/min.
66. Was the stability of the minimum flow rate tested?
Yes, and we found that the Micro HPLC Pump has a high accuracy in flow rate even when the flow rate is 0.15 mL/min
67. What is the maximum pressure that can be used without fluctuation when the flow rate is set to 0.1 mL/min?
According to the tests we run we recommend the use of a maximum 80 bar reaction pressure with a flow rate of 0.1 mL/min?
68. How often shall I use the self flushing option?
The self flushing occurs continuously while the pump is working normally. We don’t recommend that the pump is used without this feature.
69. What solvents can be used with the Micro HPLC pump?
All portions of the Micro HPLC Pump that contact the liquid are manufactured of type 316 stainless steel, ceramic, sapphire, or ruby. Even THF can be used.
Solvents not recommended to be used:
· Aqua Regia
· Chlorine Anhydrous
· Copper Chloride
· Ferric Chloride Iodine
· Ferrous Chloride
· Freon 12 (wet)
· Hydrobromic Acid
· Hydrofluoric Acid
· Hydrofluorsilicic Acid
· Hydrogen Peroxide
· Mercuric Chloride