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.
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.
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 15 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.
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
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° to +100° C for all spinning modules. As with the Phoenix HXY Probe, there is a minimal temperature offset and gradient.
Phoenix NMR 2.5 mm HFXY MAS DNP Solid State NMR Probes
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'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
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
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.
PhoenixNMR provides an efficient cryogenic 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.
The cryogenic heat exchanger is 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. The cryogenic heat exchanger is also available
for users wanting to run at low temperatures on the standard PhoenixNMR HXY probe as well. The picture below shows the cryogenic heat exchanger in operation with PhoenixNMR 600 MHz 2.5 mm HFXY probe at the New York Structural Biology Center, USA
Bridge12 Microwave Components
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.
Custom solid state NMR probes are available including:
widebore MAS NMR probes;
eFree static NMR probes as developed at the National High Field Magnetic Field Laboratory (NHMFL) by Peter Gor'kov and his team who are well known for technical innovation, high performance and exceptional craftsmanship;
custom spinning module development such as high temperature MAS or for narrow bore magnets;
custom probe development such as the dynamic angle spinning (DAS) probe (see DAS NMR probe depicted to the right).
Please contact us to discuss your custom probe interests to see if we can assist you!
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.
High pressure MAS NMR using standard Chemagnetics, Varian, Agilent and Revolution NMR probe technology: Second Generation High Pressure MAS Technology.
The patented second generation high pressure magic angle spinning technology design developed by the team led by David Hoyt and Eric Walter are now exclusively licensed to
Phoenix NMR (passing from Revolution NMR) from Battelle Memorial Institute as operator of the Pacific Northwest National Laboratory (PNNL).
Their design achieves rotor pressures up to 300 bar and at temperatures within the probe range can be achieved through a modified rotor and a set of o-rings along with a pressure source and a simple tool set.
The figure depicted below left demonstrates the assembly sequence of the rotor and the 13C MAS NMR spectra below right demonstrates temperature variation of the ethylene glycol at pressure.
The figure to the right is of the transparent schematic view of the high pressure PENCIL MAS NMR rotors.
The high pressure MAS rotors are available in 5 mm (for both wide bore and narrow bore probes), 6 mm (for narrow bore probes) and 7.5 mm diameters for Chemagnetics, Varian, Agilent and Revolution NMR probes.
The 5 mm rotor is rated at 5 kHz spinning speed at maximum pressure, while the 7.5 mm rotor is rated to 3 kHz. High speeds are possible at lower pressures.
The figure above shows the components of the high pressure rotors and the tools for these including packing the rotor. The High Pressure Transporation Chamber (HPTC) is a vital safety component for transporting
packed and pressurised rotors. The user will need to ensure they have enough HPTCs for the number of pressurised rotors they envisage they will be using at any one moment.
Below is a figure of the simple pressurisation chamber consisting of pressure tubing and unions. The simplest version requires the packed rotor to be placed in the tube and the end cap tightened on. A more sophisticated
version can use a ball valve which gives a quick access to the pressurised rotor. All you need to do is open the valve - place the rotor through the valve into the tube, close the valve and then pressurise the rotor. On completion, return the
chamber to atomospheric and open the valve and tip to remove the rotor. remember to place the pressurised rotor into the HPTC.
Purchase requires a Caution Statement to be signed by the purchaser/user concerning mandatory safety precautions
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 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.
Phoenix Low Loss FTS 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.
BioSolids Sample Packing
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:
15 ml Falcon Tubes: CORNING Falcon 15 ml Polystyrene Centrifuge Tube, Conical Bottom, with Dome Seal Screw Cap (Model No: 352095).
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:
potassium bromide, magic angle setting;
adamantane, 1H, 13C pw90 and 13C lineshape;
15N labelled glycine, 15N pw90, 13C sensitivity for 1.6 mm;
hexamethylbenzene, 13C sensitivity for 3.2 mm and larger rotors;
sodium hexafluorophosphate, 31P, 19F pw90;
silicone powder, 1H shimming (much faster); and, if your probe has a lock channel;
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.
Solid-state NMR probe Service
Phoenix NMR provides service for solid state NMR probes and, with the recent acqusition of Revolution NMR, is the one stop shop for all of the Chemagnetics, Varian, Agilent and Revolution NMR probes!
Please contact us if you have a question about other manufacturers probes, we might be able to help!
Services offered, but not limited to, include all spinning problems, crashed rotors, broken RF traps and other probe issues.
If you have an issue, just contact us to discuss it!
Static eFree NMR Probe Components
Revolution NMR manufactures the coil components and sample holders for Peter Gor'kov's static eFree NMR probes; please contact us for more details!
By the timeof the exit of Agilent Technologies from the NMR market, several solid state NMR groups have accumulated a large number of Chemagnetics, Varian and Agilent MAS NMR probes representing
significant value. Bruker BioSpin and Revolution NMR collaborated (now offered by Phoenix NMR) to produce a kit that allows these probes to be used directly on Bruker NMR spectrometers allowing them to be controlled
by the Bruker spinning speed controller and, where appropriate, the Bruker VT controller. NB,if your
Bruker VT controller only regulates to 200° C then you will require the Bruker VT Booster (BVTB-3500) to regulate to the +250° C upper temperature range of the Chemagnetics, Varian, Agilent and Revolution NMR probes.
One kit is required per spectrometer and comes in two parts:
the MAS A2B electric adapter which allows the Bruker MAS controller to communicate with the tachometer and control spinning;
the variable temperature A2B components which include adapter plates to mount probes to Bruker shim coils, mechanical adapters for the VT-transfer stack,
mechanical adapters for the Johnstone coupling, interface boxes to run the VT stack (N.B., please do not dispose of your VT stack, however, we do offer new heater stacks!).
A checklist is completed to ensure that compatibility is achieved.
The A2B kit is produced and serviced by Phoenix NMR. This can be purchased directly from Bruker BioSpin or Phoenix NMR (through TalaveraScience for Europe).