Bringing High Pressure to High Performance NMR

High Pressure NMR

<b>High Pressure NMR</b>

High Pressure NMR

High pressure NMR has a long and storied history in physics, chemistry and biophysics. However, historically the method has been greatly limited by the absence of commercial availability of high performance, large active volume NMR sample tubes capable of safe and sustained operation above 1 kbar pressures. Daedalus Innovations has solved this problem. We are the only source of complete high pressure NMR capability. Utilizing patented and proprietary designs and manufacturing processes, the Daedalus Innovations’ line of zirconia high pressure NMR tubes, titanium manifolds and computer-controlled pressure generator is in a class by itself.

Our customers include leading academic and industrial researchers around the world and are engaged in far-ranging research projects including oil and gas exploration, nuclear chemistry, structural biology, molecular biophysics, and quantum computing.

The Daedalus Innovations’ high pressure NMR cells are truly in a class by themselves. Specialized ceramic materials, proprietary manufacturing and patented tube and manifold designs open the door to high performance NMR spectroscopy at pressures ranging up to 3,000 bar. Used seamlessly with modern cryogenic probes, the high active volume (3 mm ID) gives this tube unmatched NMR performance and reliability.

For lower pressure applications, such as those employed in the reverse micelle encapsulation technique, we offer larger volume zirconia tubes with 3.6 mm ID in a 5 mm OD context.  In addition, we also provide 10 mm OD sapphire tubes mounted in our patented pressure manifold.

The Xtreme 60: Robust and precise control of pressure. Utilizing a large working volume, the Xtreme 60 provides the ultimate in pressure generation and control. Utilizing a high-torque motor and a precise computer control the Xtreme 60 is capable of generating pressures up to 4 kbar utilizing even relatively non-compressible water as the pressure generating fluid.

SNAPSHOT STATS

Tube Specifications

Standard Zirconia5mm OD (3.0 mm ID) × 92 mmVersions to 3,000 bar
Large Volume Zirconia5mm OD (3.6 mm ID) × 92 mm1,000 bar
10 mm Sapphire10mm OD (7.0 mm ID) × 149 mm300 bar

Temperature Range

+5°C to +100°C     (regular seals)
-15°C to +125°C    (optional seals)

Reverse Micelle NMR

Reverse Micelle NMR

Though solution NMR has become a powerful tool for structural characterization of biological macromolecules, particularly proteins, it is fundamentally limited by the so-called ‘tumbling problem.’ Large proteins tumble relatively slowly in solution producing greatly broadened spectral lines as a result of fast transverse relaxation. Increased transverse relaxation not only broadens peaks but also decreases magnetization transfer efficiency, which drastically impedes collection of multi-dimensional data that is often needed for efficient analysis. Several strategies have been developed to mitigate these problems including the use of isotopic labeling schemes to minimize cross-relaxation and simplify spectra, the TROSY effect to reduce the detrimental effects of averaged transverse relaxation and the CRINEPT strategy for more optimal polarization transfer. Unfortunately, limitations inherent to these approaches have restricted the precision of structural models for proteins of significant size.

Encapsulation of proteins within the protective aqueous of core of reverse micelles offers the ability to decrease macromolecular tumbling through preparation in low viscosity solvents such as liquid ethane. Gaining popularity, this novel sample also offers advantages in a variety of other contexts such as studies of integral and anchored membrane proteins, protein-ligand interactions, stabilization of the marginally stable proteins, protein hydration to name but a few applications.

Sample preparation is the key ingredient. Daedalus Innovations provides the only source of integrated sample preparation apparatus and high performance NMR sample tubes capable of seamless operation in modern cryogenic probes at the modest pressures necessary for reverse micelle NMR (generally less than 300 bar).

Liquid ethane is the ultra-low viscosity solvent of choice. The Daedalus Innovations reverse micelle sample synthesizer is the only commercially available apparatus designed specifically for the preparation of solutions of encapsulated proteins dissolved in low viscosity fluids. Designed to work with the X-treme 10 syringe pump and the high volume (3.6mm ID) zirconia high pressure NMR tube, the RM Synthesizer™ directs the creation of solutions of encapsulated proteins with ease.

Don’t think you can make a reverse micelle sample? Try our demonstration kit and convince yourself!

RM Synthesizer Specification Sheet

RM Synthesizer User Manual

RM Tube Specifications

Xtreme Syringe Pump Specifications

Support Equipment

Support Equipment

Safety Box: This acrylic walled box provides protection to users while pressurizing cells. It also helps protect the setup while moving samples from the bench to the spectrometer. It also provides a convenient place to store high pressure cells when not in use. The box is open on the bottom.

Bruker and Varian versions are available.

Cell Setup Tool: The high pressure tubes are not permanently fixed in the cell to allow for tubes to be switched and cleaned independently. This benefit requires some care when assembling the high pressure cell. This tool assists in that process by helping to keep the tube axially aligned with the cell during setup which improves seal integrity and lowers the probability of improper fit in the NMR.

Only one is needed for each cell type (Varian or Bruker)

OTHER CELL COMPONENTS:

High Pressure Seals (TS01): These form the primary seal between the high pressure tube and manifold. They are single use. One version works for all tube and cell combinations.

Ordering

Please contact us for a quotation: 
sales@daedalusinnovations.com

European requests for quotations can be directed to:
David Cross
cross@rototec-spintec.com

Typical Set-Ups

Reverse Micelle NMR

  • (1) Reverse Micelle Synthesizer
  • (1) Xtreme-10 Syringe Pump
  • (1) NMR manifold valve & 3.6 mm i.d. tube
  • (1) Safety Box
  • (1) Cell Setup Tool
  • (10) TCSN Tube Seats
  • (100) TS01 Tube Seals

plus standard high pressure tubing and fittings as required

High Pressure NMR

  • (1) Xtreme-60 Syringe Pump
  • (1) NMR manifold valve & 3.0 mm i.d. tube of desired pressure rating
  • (1) Safety Box
  • (1) Cell Setup Tool
  • (1) Torque wrench
  • (75) TS01 Tube Seals

plus standard high pressure tubing and fittings as required