This new facility features a 400 MHz WB Bruker Ascend Magnet with an AVANCE NEO Bruker Spectrometer, a Bruker H/X 4mm MAS probe, and a Phoenix NMR H/X high-temperature/high-pressure 5mm probe. This instrumentation allows us to perform state-of-the-art in-situ NMR experiments on a wide variety of samples. For details on potential applications, click here.
Magnet
The 400 MHz Bruker ASCEND NMR magnet enables the analysis of molecular structures at a moderate resolution. Its stable magnetic field yields precise chemical shift measurements, making it well-suited for a variety of solid-state NMR experiments.
- 400 MHz WB Bruker Ascend
- Bore size: 90 mm
- Homogeneity < 1 ppb
Spectrometer
The BRUKER AVANCE NEO spectrometer, running TopSpin 4.1.4, enables sophisticated pulse sequences and acquisition methods crucial for complex NMR experiments.
- Bruker AVANCE NEO
- Runs TopSpin 4.1.4
- MAS III Controller
Bruker MAS Probe
This probe is designed by Bruker and allows for the performance of state-of-the-art solid-state NMR experiments. It’s ability to consistently maintain spinning stabilities as low as +/- 1 Hz enables the execution of experiments that rely on spinning frequency dependent pulse sequences.
- Bruker 400 MHz 1H/X MAS probe with interchangeable sample coils
- 1H/19F channel, 500 W
- Broadband X (15N-31P) channel, 1000 W
- Maximum temperature: 150 C
- Maximum spinning frequency: 14,000 Hz
Phoenix NMR MAS Probe
This specialized probe is specially fabricated by Phoenix NMR to withstand high temperatures up to 250 C. The ability to reach these temperatures enables the ability to study a wide range of reactions related to catalysis, materials science, geochemistry, and membrane transport.
- High Temperature/Pressure 400 MHz 1H/X MAS probe
- 1H/19F channel, 500 W
- Broadband X (15N-31P) channel, 1000 W
- Maximum temperature: 250 C
- Maximum pressure: 400 bar at 20 C; 200 bar at 250 C
- Maximum spinning rate: 12,000 Hz at 20 C / atmospheric pressure; 5,000 Hz at 250 C / 200 bar
Specially Designed Rotors for High Temperature and High Pressure NMR
The rotors used in our high-temperature/pressure system were designed at Pacific Northwest National Laboratories and commercialized by Phoenix NMR. These 5 mm, pencil-style rotors are made with a zirconium sleeve. They are capable of holding pressure up to 400 bar (6,000 psi) at 20 C, and up to 200 bar (3,000 psi) at 250 C, enabling the in-situ study of reactions of multi-phase systems, even at harsh conditions.
- (A) Empty rotor sealed with spacer and drive tip
- (B) Sample chamber filled with solid and liquid sample components
- (C) Bushing with two o-rings is inserted to cap the other end of the rotor
- (D) A locking screw compresses the o-rings against the rotor walls, preventing the escape of gases
- (E) A pressure vessel holds the rotor when pressurizing with gas
- (E’-E”) Pressurized gas fills the rotor until it is equalized with the pressure in the vessel
- (F-F’) The pressurized rotor with the check valve maintaining pressure
Rotor Pressurization Manifold
The rotor pressurization manifold, equipped with a syringe pump, allows for controlled pressurization of specialized Phoenix NMR rotors with one gas at a time. This setup is crucial for experiments requiring high pressure conditions.
- A Syrixus 500X Syringe pump from Teledyne Isco chamber is filled with gas from a typical gas cylinder
- The syringe pump pressurizes the rotors through a stainless steel gas tubing manifold
- The rotor is pressurized inside of a small stainless steel chamber fabricated by Swagelok, which holds the pressurized gas while it equilibrates inside and outside of the rotor
