Phoenix NMR design, manufacture and service solid state NMR probes.

TalaveraScience is the sales agency for Phoenix NMR throughout Europe, in Australasia and India.

Phoenix NMR has many years of experience in design of and making solid state NMR probes as the team originally working at Chemagnetics which was first acquired by Varian (1997) and then by Agilent Technologies (2009). Phoenix NMR probes are based on the latest version of Transmission Tuning Tube Technology (T3 Technology) to make very RF-efficient narrow bore (NB or SB) solid state NMR probes. These probes have a variety of tuning configurations such as the Phoenix HXY probe with HXY and HFXY configuration and with interchangeable probe heads including 1.2, 1.6, 2.5, 3.2, 4, 5, 6 mm and static probe head options and the Phoenix HX probe with a fixed probe head with

the option of HFX performance providing a very cost effective double resonance probe. These probes are available for wide bore and standard/narrow bore magnets and are a high performance accessory for any NMR spectrometer, solids or liquids.

Recently, Phoenix NMR have developed the 2.5 mm HFXY solid state DNP NMR probe (wide bore format) with automated sample insert eject in order to change frozen samples.

Please read on for more information...

Please contact info@talaverascience.com for further details.

Phoenix HXY Probe Features...

Interchangeable Probe Heads

Phoenix HXY 1.6 mm Probe Head

Interchangeable Phoenix HXY Probe Heads are available for static horizontal samples, 1.2 mm, 1.6 mm, 2.5 mm, 3.2 mm (pictured to the left), 4 mm, 5 mm and 6 mm. There is a lock channel option available for the 1.6 mm probe heads.

The VT exhaust is visible on the top of the probe head and interfaces with an exhaust chimney which passes through the solution state spinner assembly in the magnet. The VT input is located on the Phoenix HXY Probe Base (see right). The nominal VT range is -125 to +125° C.

The probe is compatible with the simultaneous 1H and 19F accessory turning the probe into a HFXY 4-channel probe. Similar technology is available for looking at closer nuclei X- pairs. The probe is compatible with the low gamma accessory allowing tuning of a X-channel to 14 MHz.

Phoenix HXY Probe Base

The Phoenix HXY Probe Base, depicted below, shows the available RF connections, the CamLock mechanism for holding the probe in the probe frame, the distinctive VT input with heat sink (the black item on the left) to avoid condenstaion and ice formation when running cold, Tachometry is compatible with most NMR spinning speed controllers (if not please see below for the Phoenix NMR spinning speed controller) making the probe highly versatile and future proof.

Phoenix HXY Probe Base

Please contact us if you would like to receive specifications and example manuals at info@talaverascience.com.

Phoenix HX NMR Probe Features

Phoenix HX Probe Top

Phoenix HX Probe Spinning System

The Phoenix HX Probe is a cost effective high performance solids MAS double resonance probe ideal for narrow (standard) bore magnets with or without high power amplifiers (100 W 1H and 300 W X amplifiers provide almost enough power to approach the maximum RF amplitude specifications) and is compatible with all of the manufacturers' NMR spectrometers. Ideal for solids capability on liquid state NMR spectrometers when equipped with the Phoenix NMR spinning speed controller.

Depicted on the left is an example of the fixed probe head spinning system. The Phoenix HX Probe is available from 400 to 700 MHz (higher frequencies available on request) with spinning systems including 1.2 mm, 1.6 mm, 2.5 mm, 3.2 mm, 4 mm, 5 mm, 6 mm and for static samples. The VT exhaust which interfaces with the VT funnel can be seen on the top of the spinning system as for the Phoenix HXY probe.

The 1H channel is tunable down to 19F with the simultaneous 1H/19F option to give the Phoenix HX probe a HFX configuration! The X-channel is tunable from 31P to 15N and to 15 MHz with the low gamma accessory.

Phoenix HX Probe Base

Phoenix HX NMR Probe Base

In the picture above the RF channels and various connections are shown on the Phoenix HX probe base. Variable temperature operation is similar to that of the Phoenix HXY Probe with a slightly reduced temperature range of -75°C to +100° C for all spinning modules. As with the Phoenix HXY Probe, there is a minimal temperature offset and gradient.

Please contact us if you would like to receive specifications and example manuals at info@talaverascience.com.

Phoenix HFXY NMR DNP Probe Spinning at 105 K with Sample Changer

The movie below demonstrates the spinning performance and sample changing at 105 K, using the Bridge12 Heat Exchanger, for the Phoenix NMR 2.5 mm HFXY DNP solid state NMR Probe.


Novel Sample Insert and Eject Technology

Phoenix NMR solid state DNP NMR probe head and sample inert/eject mechanism

Phoenix NMR's novel sample/insert eject design (see the picture to the right) uses a standard Eppendorf Tube to present the rotor to the insert mechanism. Operating the insert function loads the rotor into the spinning module which is, unconventionally, mounted upside down and a small amount of drive provides enough Bernoulli effect to capture the rotor.

Freezing the sample to form the optimal glass can be done externally to the probe and with the appropriate preparation can be introduced to the insertion mechanism to minimise any temperature increase and not to have any manual handling of the rotor.  The whole sample changing time, while operating at DNP temperatures, can be as short as 3 minutes with about a 7 K sample temperature increase.

Sample ejection is the reverse of the insertion and is facilitated through the Phoenix NMR MAS controller (PMAS).

The spinning module remains fixed during sample changing to avoid disturbing the magic angle setting. The rotor passes through a swept path to-and-from the spinning module. The microwave radiation is delivered by a Bridge12 corrugated waveguide and transversely illuminates the rotor.


Densely Tuned RF Channels

Phoenix NMR solid state DNP NMR probe head drawing

The swept path taken by the rotor can be envisaged in the drawing to the left.  The picture also shows the series tuning elements and the trap which connects the third, Y, RF channel to the RF circuit. The probe uses the same tuning tubes as the Phoenix HXY NMR probe with the same tuning range and characteristics. With the shorted tuning tube and the low gamma accessory, the probe can be used for low gamma nuclei down to 15 MHz. The independent 19F channel is added by utilising the same diplexer technology as for the Phoenix NMR HXY and HX probes.

Closer tuning, less than 20%, can potentially be provided with the use of diplexers to create, e.g., a X/X' RF channel depending on the frequency separation of the two nuclei of interest.


Cryogenic VT Operation for solid state DNP NMR

Phoenix NMR MNAS in DNP Mode

The Phoenix NMR 2.5 mm HFXY solid state DNP NMR probe package is provided with the Phoenix NMR PMAS, as discussed above, and with the Phoenix NMR VT controller. The display of the PMAS is depicted to the right showing all of the important experimental parameters including the drive and bearing pressures, VT and probe purge flow rates, spinning speed, sample set temperature and other information.

Bridge12 provide an efficient counter flow heat exchanger which is designed and engineered to avoid LN2 condensing in the exchange gas stream (which is not good for stable spinning!) consisting of the specially designed transfer lines shown below and a 50 litre dewar which, when filled, lasts 36 hours and can be refilled without interupting the solid state DNP NMR experiment. There is an option that allows dry N2 gas to be generated from the LN2 in the dewar for use as the VT exchange gas.

The dewar and counter flow heat exchanger are designed to be efficient on the use of cryogenic consumables such as LN2 and the whole probe package delivers a reduced running cost alternative as far as this cryogen is concerned.

Bridge12 Counterflow Heat Exchanger

Bridge12 Microwave Components

Bridge12 corrugated waveguide

The internal microwave components are designed and manufactured by Bridge12, exploiting  their experience with corrugated waveguides and solid state DNP NMR applications. The figure to the left depicts such a waveguide.

The probe can be connected to the high power microwave source either directly through a coupling waveguide or via a quasi optical mirror which reflects the microwaves from the coupling wave gudie into the probe waveguide for transmission to the sample.

Other Bridge12 products are also useeable with this probe and this includes the modular (cw, pulsed and AWG) High Frequency EPR Spectrometer, equiped with its own sweepable source, which couples to the coupling waveguide and uses the solid state DNP NMR probe as the EPR probe and is useful for determining the EPR spectrum of the label, optimising the magnet field strength for optimal DNP enhancements and determining the T1e of the label.

Also available from Bridge12 is the gyrotron frequency measurement system to accurately determine the source's output frequency.

See more details on our Bridge12 webpage!

Zirconia and saphhire rotors are available for the solid state DNP NMR probe.

 

Complete Solid State DNP NMR Capability for existing and new solid state NMR spectrometers

Lastly, a complete solid state DNP NMR accessory is available with the addition of a Bridge12 gyrotron and coupling wave guide to the Phoenix NMR solid state DNP NMR probe package and is avaiable for 400-600 MHz 1H solid state NMR systems equipped with wide bore magnets.


Please contact info@talaverascience.com for further details.

Phoenix NMR MAS Spinning Speed Controller

Phoenix NMR Spinning Speed Controller

The Phoenix NMR MAS Spinning Speed Controller includes a touch screen interfaced pneumatic control system with auto calibration for unknown spinning modules or for extreme conditions with an unlimited number of profiles.

It allows for instant switching between manual and auto modes, full automation from start to finish, automated PID tuning and continuous time stamped logging of all system parameters!

  • Fully compatible with all Chemagnetics, Varian and Agilent solids MAS NMR probes and spinning systems
  • Compatible with Bruker, JEOL and Tecmag MAS probes
  • Speed detection beyond 180 kHz
  • PID teaching mode for non-Phoenix NMR probes
  • Bearing and drive automation
  • Time stamp logging for all parameters
  • Easy transfer between automated and manual spinning modes
  • Simple user updates for new module profiles
  • Compact 14"/356 mm wide x 6"/152 mm tall x 10"/254 mm deep instrument quality case.

Please contact us if you would like to receive additional information at info@talaverascience.com.

Phoenix NMR Accessories and Services

A range of accessories is available including the low-gamma accessory, the Bridge12 CHE for extended low temperature experiments, BioSolids sample packing tools, prepacked NMR standards rotors and probe servicing.


Phoenix Low Loss FTS Adapter

PCS and FTS VT Adapter

The variable temperature adapter connects a FTS trunk to a Phoenix NMR probe and to a Varian or Agilent solids VT stack with minimal loss between the outlet and probe input.

Phoenix NMR Low Gamma Accessory

Phoenix NMR Low Gamma Accessory

The Phoenix NMR Low Gamma accessory is pictured to the right connected to a Phoenix HXY probe and extends the low frequency channel below 15N down to 15 MHz for both the full range of Phoenix HXY and Phoenix HX NMR probes.

If you have a low gamma accessory from your previous T3 probes, such as a Varian or Agilent low gamma accessory, then you will find that these are compatible with the Phoenix HXY and the Phoenix HX NMR probes and vice versa (the Phoenix NMR low gamma accessory is compatible with existing Varian and Agilent T3 probes)!

Please speak to us if you need to access resonance frequencies that are below 15 MHz to see if we can extend the frequency range lower.

BioSolids Sample Packing

Phoenix NMR Biosolids Packing Tools

Phoenix NMR offers BioSolids sample spacers and centrifuge sample packing tools for 1.2 mm, 1.6 mm, 2.5 mm and 3.2 mm rotor sizes.

These tools, along with the moulded silcone spacers make it easy to efficiently transfer your pelleted sample from 200 µl ultracentrifuge tubes into a ready to use rotor that will keep your sample hydrated. The centrifuge tubes our tools are compatible with are:

  • 200 µL ultracentrifuge tubes: Beckman Coulter Centrifuge Tubes (Model Number: 343775)
  • 15 mL Falcon Tubes: CORNING Falcon 15 mL Polystyrene Centrifuge Tube, Conical Bottom, with Dome Seal Screw Cap (Model No: 352095).

Standards

Phoenix NMR offers sample kits in for all narrow bore rotor sizes working with all Phoenix NMR probes as well as Varian and Agilent PENCIL MAS narrow/standard bore probes to calibrate pulse widths, set the magic angle, measure sensitivity and check lineshape. These include:

  1. potassium bromide, magic angle setting;
  2. adamantane, 1H, 13C pw90 and 13C lineshape;
  3. 15N labelled glycine, 15N pw90, 13C sensitivity for 1.6 mm;
  4. hexamethylbenzene, 13C sensitivity for 3.2 mm and larger rotors;
  5. sodium hexafluorophosphate, 31P, 19F pw90;
  6. silicone powder, 1H shimming (much faster); and, if your probe has a lock channel;
  7. D2O, 2H pw90;

utilising the BioSolids silicone sample spacers. An additional rotor is available to initially shim on 1H to aid final lineshape on 13C.

If you are interested in spacers and tools for a different rotor size, please contact us with your request.

Please contact us if you would like to receive additional information at info@talaverascience.com.

The Phoenix NMR Team

The Phoenix NMR Team
PhoenixNMR HXY Probe Heads