Huber

Yes, but we need to know the serial number of the unit first please.  If you don’t have it yet, we can send you an example CE declaration for the model.

Our standard jacketed lab reactors have the following connections for Huber (or other circulator) hoses:

• Reactor-Ready and Reactor-Ready Duo: M24 male
• Reactor-Ready Pilot: M30 male
• Lara (current model): M24 male
• Lara (older version): M16 male

Huber units (or other circulators) have fittings for connecting to the hoses (referred to as pump connections) of a particular size for that Huber model, as stated in its technical data, e.g. M24, M30 or M16. These are always male. If your jacketed lab reactor has the same size fittings as your Huber unit (e.g. they are both M24), you can use a hose of that size (M24 in this case), and no size adapters are required. (Huber hoses are always female at both ends.) If your jacketed lab reactor has different size connections to your Huber (e.g. Reactor-Ready is M24 and your Huber is a Petite Fleur, which is M16), you could potentially use a hose of either size (e.g. M16), but you will need a size adapter where the size changes (in this example, between the M24 Reactor-Ready and the M16 hose). The descriptions of size adapters match the adapters themselves, not what they connect to. You always need male joining to female. For example, to connect M24 male Reactor-Ready to a M16 female hose, you need an M24 female to an M16 male adapter, part number HB6724. There are a range of size adapters listed in the Huber catalogue. Please contact us if you require further assistance. N.B. The full names of these M fittings are:

• M16x1 or M16/1
• M24x1.5 or M24/1.5
• M30x1.5 or M30/1.5

They have been abbreviated in this post for clarity. The short names are commonly used.

You can control a new Huber unit with Pilot ONE controller via a PLC/DCS etc. It is possible to send setpoint commands and receive temperature readings, and also stop the Huber if a particular temperature is exceeded. There are different methods of communication available, but RS232 is commonly used. You can refer to the Huber data communications manuals – PB commands (recommended) or PP and LAI commands (older). The RS232 cable for new Unistats with Pilot ONE is HB55018 (with a 15-pin end for connecting to the Huber).  For other units, a 9-pin RS232 cable is offered, part number HB6146.  Please feel free to ask if you have any queries. For information on the Ethernet and AIF (4-20 mA) options for new Huber units with Pilot ONE, please refer to the separate FAQ entries. For older Huber models, please contact us with the serial number of your unit, and we can advise on your options.

You can control a new Huber unit with Pilot ONE controller via a PLC/DCS etc. There are different methods of communication possible, including 4-20 mA using an analogue interface (AIF).  The 4-20 mA communication can be used to send signals to the Huber unit (control it) in addition to receive signals (monitor it). The analogue interface has one programmable input channel (e.g. for setpoint), and three output channels (setpoint, external temperature, and programmable).  If you want to control multiple parameters, we would advise you consider another method of communication. You would need to purchase an Com.G@te (optional accessory) to have an analogue interface.  Please search the FAQs for further details of the Com.G@te. We can supply a cable for connecting to the analogue interface on the Com.G@te, part number HB9353.  This has an open end, for wiring into your application.

External Com.G@te (part number HB6915)

You could either connect it with a 3 m cable (part number HB16160), or alternatively use a shorter cable and a bracket to mount it on the unit (different part numbers for different Huber models).

Internal Com.G@te (part number HB31217)

There are a number of ways you can add a Pt100 temperature probe, normally used with AVA to automate a circulator (thermoregulator, e.g. Huber).

Connection to circulator and PID control via circulator – recommended

Physically connect the Pt100 probe to the circulator. In the AVA Apparatus window, add a circulator, and in its settings, for ‘External temperature probe connected to circulator?’, select ‘Yes’; the temperature probe will now be shown in AVA.  Tr (controlling the temperature of the reactor via the external probe) is now possible.  The circulator itself will be responsible for the PID control.

Connection to Data Hub and PID control via AVA

You can use this option if your circulator does not have a socket for a temperature probe. Physically connect the Pt100 to the Data Hub.  In the AVA Apparatus window, add a circulator, and in its settings, for ‘External temperature probe connected to circulator?’, select ‘No’; then click on the pale grey outline of a temperature probe in the reactor and add a temperature probe.  Tr (controlling the temperature of the reactor via the external probe) is now possible.  However, rather than the circulator being responsible for its own PID, the AVA software will control it.

Additional temperature probe just for monitoring

You could do this if you want to monitor another temperature probe (not related to control of the circulator), such as one for a reflux divider; you can use its reading for a step override, for example. Physically connect the Pt100 to the Data Hub. In the AVA Apparatus window, use the top left zone (pale grey box) to add one temperature probe. (It is also possible to use the top right zone to add further additional temperature probes like this, if you have AVA level 4.)

All our jacketed lab reactors (including Reactor-Ready, Reactor-Ready Duo, Reactor-Ready Pilot and Lara) have an advised temperature range of -70°C to +230°C (thermal fluid temperature, i.e. circulator internal temperature). When working at low temperatures, vacuum jacketed vessels are recommended – please see the separate FAQ entry on vacuum jacketed vessels for further details. In addition, for extreme low temperatures (below -50°C), we suggest that piston O-rings are replaced between every run, because these conditions can cause the O-rings to harden and become brittle, potentially reducing the effectiveness of the seal. For temperatures above +150˚C, for Reactor-Ready Pilot, we recommend the use of high performance Chemraz piston O-rings to minimise the risk of weeping.  The O-rings should be inspected between runs and replaced regularly. We also offer a secondary valve for the run-off (outlet) of the bottom outlet valve (part number RR139098 for Reactor-Ready, Reactor-Ready Duo or Lara; RR139137 for Reactor-Ready Pilot) to catch any liquid that may weep around the piston at temperature extremes.

Additional considerations when working at high or low temperatures are the temperature limits of your circulator (remembering that the temperature range of the process will be narrower than this) and thermal fluid (especially regarding high viscosity at low temperatures and inert gas blanketing at high temperatures). If you chose to work beyond our recommended temperature guidelines, this would be at your own risk.  One potential issue is that PTFE (used for many Reactor-Ready parts) can soften when used at very high temperatures.

Delta T (ΔT) is the difference between two temperatures.  We use this term to refer to the difference between:

• The temperature of the oil in a vessel’s jacket (also called internal temperature) and
• The temperature of the vessel contents (also known as process temperature or reaction temperature).

We usually consider the delta T when a jacketed vessel is being heated or cooled.  The temperature of the vessel contents will lag behind the temperature of the oil in the jacket.  If the delta T is too large, it could stress the glass and lead to breakage. We therefore recommend that the delta T limit is set to 50°C (50K).  With current Huber thermoregulators with Pilot ONE controllers, you can adjust this by Menu → Protection Options → Delta T Limiter → type 50 in ‘New value’ field → tap ‘Ok’ to confirm. In the previous Nuevo controllers the delta T limiter can be found in the ‘Limits’ menu, and in older Unistat controllers it is program 18. Please note, this control can only be achieved if the contents temperature is being monitored. If it is not being monitored (if the vessel is empty, for instance) then great care should be taken to heat or cool the vessel in a controlled, gradual way to prevent thermal shock (e.g. by use of a ramp function).  When using a temperature probe in the vessel (external Pt100), please ensure the end of the Pt100 is always immersed in the vessel contents. Please also be aware that even if a delta T limit is set, it is possible for this limit to be exceeded slightly in practice.  If this poses a problem for you, we recommend you reduce the delta T limit setting to below your desired limit.

Note: for an introduction to delta T, please see the separate FAQ entry ‘What is delta T?’.

Under normal circumstances, you cannot set delta T in AVA – it is not applicable.

• If, as we recommend, you plug the Pt100 temperature probe directly into the circulator (e.g. Huber)
• and have it configured like this in AVA (in the circulator properties box, for ‘External temperature probe connected to circulator?’, ‘Yes’ is selected)
• then the circulator is responsible for the temperature control.  If you implement a Tr (reaction temperature) setpoint/ramp, AVA will send Tr instructions to the circulator, and the circulator will calculate the required Tj (jacket temperature).
• In these circumstances, you should set the delta T limit in the circulator controller itself (not in AVA).  The circulator is responsible for measuring and responding to the delta T.

If the reactor Pt100 is separate from the circulator, you do set delta T in AVA.

• It is possible (e.g. if the circulator does not have a Pt100 socket) to plug the Pt100 for the reactor into the Data Hub instead
• and set up the Apparatus like this in AVA (in the circulator properties box, for ‘External temperature probe connected to circulator?’, select ‘No’, then click on the outline of a temperature probe in the reactor to add a Pt100 there)
• and then when you click on the circulator properties box, you will see that the field ‘Maximum temperature difference Tr – Tj’ has appeared.
• In this case, when you set Tr, AVA calculates the Tj and sends the Tj instructions to the circulator, considering the delta T limit set in AVA.

If your condenser is struggling to contain all the vapour generated in your jacketed reaction vessel, there are a number of steps you can take.

Ensure your condenser is large enough

It’s important to use a condenser that is an appropriate size for your equipment and application, e.g. vessel size.  Here at Radleys we offer a wide range of condensers with different surface areas, and we can also make custom condensers if required. Please contact us and we’ll be happy to advise.

Use appropriate cooling water, e.g. use a suitable chiller set correctly

Ensure you have sufficient cooling water for the condenser.  It may be helpful to use a chiller, if you do not have a suitable chilled water supply (e.g. tap water is too warm).  If you do use a chiller, make sure it has enough cooling power to effectively condense the chemical vapours.  Note that cooling power decreases with set temperature, so it may actually help to increase the temperature the chiller is set to to obtain more cooling power whilst maintaining a large enough temperature difference.  We often recommend +15⁰C; at -20⁰C the chiller will have little cooling power!

Minimise the amount of chemical vapour generated

Do not apply excessive heat to the reaction vessel.  There is no benefit to overheating, as the temperature cannot exceed the solvent boiling point – you simply generate more chemical vapour to be condensed.  If you are refluxing, make sure you aren’t using reactor control (setting temperature via a Pt100 probe in the vessel) and setting the temperature higher than the boiling point, or the jacket temperature could keep increasing in an attempt to raise the reactor temperature, producing too much vapour.  Furthermore, ensure any exothermic reactions are controlled, e.g. by using AVA software.

SilOil is short for silicone oil. The first part of the code is the lower temperature limit (°C) of the oil.  This is the temperature of the fluid where the viscosity has reached 50 centistokes (cSt; equivalent to mm²/s); cooler than this and the oil would be too viscous to pump.  The ‘M’ or ‘P’ before the number refer to minus or plus respectively. The second part of the code (in between two full stops) is the higher temperature limit (°C) of the oil. If there are two figures separated by a ‘/’, the first corresponds to the maximum in an open bath unit (e.g. Ministat) and the second is the maximum in a Unistat. The maximum recommended temperature for a bath unit is below the oil’s flash point, to ensure safety. Unistats are hermetically sealed, so can be used at slightly higher temperatures. The final part of the code is the viscosity at 25°C (around room temperature) in centistokes, cSt (i.e. mm²/s).  The higher the number, the higher the viscosity.

90° bends (90 degree bends) are also known as right angle adapters or elbow adapters.

We recommend them for use with circulators (typically Huber units), one for each hose.  They are inserted between the hose and its respective hose connection on the circulator. Highly insulated circulator hoses are not very flexible, and Huber hose connections point straight out of the side or back of the unit.  Depending on where you want to locate the circulator relative to your reaction system, including the 90° bends can make it easier to position the hoses in the appropriate direction. Choose 90° bends that are the same size as your circulator hose (pump) connections. The part numbers are:

• HB6195: M16/1 90deg Adapter
• HB9256: M24/1.5 90deg Adapter
• HB6461: M30/1.5 90deg Adapter
• HB6699: M38/1.5 90deg Adapter

On Reactor-Ready, Reactor-Ready Duo and Reactor-Ready Pilot, the manifolds you connect the circulator hoses to already have 90° bends as standard, so you do not need to purchase them for the reactor end.

The process to update the firmware of a Huber Pilot ONE controller is called flashing. To do this, download the Huber Pilot ONE Flasher software from the Huber website The download will contain the manual with instructions on how to download the latest firmware from the internet and transfer it to the Pilot ONE controller; this can also be viewed online.

If you have a bath unit or a chiller (such as a Minichiller), then you can potentially use water as thermal fluid. Note that usually a mixture of water and ethylene glycol is used rather than just water, to widen the temperature range – adding glycol reduces the freezing point.  (Search these FAQs for ‘glycol’ to find the entry ‘Do I dilute ethylene glycol for use in a circulator? By how much?’ for further details.) Please be advised that if you have a Huber Unistat, you should not use water or water-glycol as thermal fluid – select a suitable silicone oil for the temperature range instead.

The Lara drain-down button facilitates the draining of thermal fluid back into the circulator. When the button is depressed, air is allowed to enter the circulator system through a gold-coloured filter situated above the button. This makes the draining process much faster.

You would first need to ensure that the circulator has enough space in its expansion tank to accept the oil.  (An additional external expansion tank can be added to a Huber if required.) The circulator would have to be positioned below the Lara, as gravity is used for drain-down. To drain the Lara vessel jacket:

• Switch off the circulator.
• Press the ‘drain’ button on the left hand side of the triangular Lara framework.
• The button must remain depressed to completely drain the jacket.

Check the technical data sheet for the Huber model. This can be downloaded from the Huber website – search for your model to go to its web page, then click on the ‘Data sheet’ hyperlink. Scroll down to the ‘Accessories and periphery’ section near the bottom.  The parts labelled with a * symbol are included with the unit as standard.

The immersion cooler models with an MPC control panel (shown below) require an external Pt100 temperature probe to operate.

So we can identify exactly which Huber model you have (e.g. since there have been different versions over the years), we often ask for the unit’s serial number. This should be stated on a silver sticker on the unit, such as the one below:

An RS485 interface is available for Pilot ONE Huber units if you purchase a Com.G@te, such as the one shown below.  (You can search these FAQs for ‘Com.G@te’ for further details.)

We can supply a cable for connecting to RS485 interface on the Com.G@te – part number HB6279. This has an open end, for wiring into your application. Further wiring guidance The pinout of the interface is as follows:

• 6 – A with 120Ω-terminating resistor
• 7 – A
• 8 – B

Pins 7 (A) and 8 (B) must be used for connection with the RS485 network. As there are only two wires, they are always connected A to A and B to B, independent of the number of RS485 units. You should typically only use pin 7 and pin 8; pin 6 is not used for normal operation.  If the resistor should be activated for termination, you have to make an additional bridge between 6 and 7 at the corresponding unit.  Please take care that only one termination resistor is connected at each side of the RS485 bus.  This termination resistor is typically required in cases of high baud rates and large distances; please only use the baud rate of 9600 with the RS485 bus.

Communications

Huber RS485 only supports half-duplex mode. If a single Huber unit is connected via RS485, the Huber will be able to understand any of the Huber command sets available – LAI, PP or PB commands, detailed here and here. However, if multiple Huber units are connected via RS485, each unit must have its own unique address, and you have to address each unit separately.  This means you need to use the Huber LAI command set, as only LAI enables you to send address information within the command.  If the PLC/DCS etc. sends a command on the RS485 bus, every connected unit is listening, but only the addressed system can answer. If you want to connect multiple Huber units to your PLC/DCS and it has Ethernet functionality, you may find that method of communication easier, as then you have the option of the PB or PP command sets, and furthermore you wouldn’t need to purchase a Com.G@te for each Huber unit, as an Ethernet socket is included as standard on Pilot ONE controllers.