What’s New

7/20/10 In vivo 7 Tesla MRI Non Human Primate Atherosclerosis Imaging
with a Doty Scientific 150 mm I.D. quadrature volume RF coil.
We wish to thank the Center for Biomolecular Imaging & Department of Pathology Section for Lipid Sciences,
Wake Forest University School of Medicine for sharing their results.


12/4/09 Doty Diffusion probe used to perform Oscillating Gradient Spin Echo (OGSE)
A Doty Diffusion probe was used at Vanderbilt University to perform Oscillating Gradient Spin Echo (OGSE) methods to probe ultra short diffusion times as low as ~0.13 ms, corresponding to characteristic diffusion lengths of ~0.7μm.

8/01/09.
Recent results from an 800 MHz Doty Vertical Bore Imaging Probe with Model 26-40 Three Axis MRI Gradients
Some impressive mouse imaging results have been reported from the Magnetic Resonance Research Center at Arizona State University using a Doty Scientific vertical bore 800MHz imaging probe.

11/11/08 . Extending the Sample Temperature on the OptiMAS Probe to 86K
Requirements for low sample temperature for DNP and other experiments have prompted us to push to lower sample temperatures on our probes. Recent low temperature (86 K) MAS spectra obtained on our NB DI4 OptiMASTM Probe is presented on the OptiMAS page.

10/27/08 . Factor of 4 INCREASE in S/N with CryoMASTM Probe
Natural Abundance 15N NMR spectra show a factor of 4 gain in S/N with the DOTY CryoMAS probe when the RF coils were cooled to 25 K. Another factor of 2 gain in S/N is expected with a cold preamp. The sample, glycine, was maintained at room temperature, undergoing 7 kHz MAS, 10 µs 15N π/2, in an 11.7 T widebore JEOL NMR spectrometer.

The probe currently includes a triple resonance (1H/13C/15N) RF circuit, a 3 mm insulated ceramic spinner that allows independent maintenance of the sample temperature, a vacuum insulated coil and capacitor region that allows cryogenic cooling to 25 K, cryogen free operation with commercial closed loop GM cryo-cooler, and reliable automatic sample eject. The CryoMAS probe has demonstrated a spinning speed of 18 kHz, high RF power tolerance, and factor of 4 gain in S/N on room temperature glycine with cryogenic cooling of the sample coils and circuit (note the preamps were not cooled in this test). Please see the link above, for an update on development progress.

3/03/08 .  Development of the PISEMA probe
Doty's PISEMA probe for high power triple-resonance experiments is under development. Please see the link above, for an update on development progress.

1/28/08 .   Recent results from Doty XC MAS probes
These results from XC4 and XC5 MAS probes demonstrate the fast and stable spinning of the XC probes as well as rf performance for the most demanding experiments.

1/28/08 .   Preprint available Probe Design and Construction.
Download a preprint of “Probe Design and Construction”, by F. David Doty, published in [Encyclopedia of Magnetic Resonance - Article posted online (www.interscience.wiley.com) on 12/15/07, Copyright © 1996, 2000, 2002, 2007 John Wiley & Sons, Ltd. All rights reserved, DOI: 10.1002/9780470034590.emrstm1000].

Abstract: A brief review of some interesting aspects of the history of NMR probes is presented, followed by an overview of the basics of NMR probe design and optimization for liquids, solids, and imaging applications. Simple analytical methods are presented for signal-to-noise optimization of single, double-, and triple resonance circuits based on Q-values, magnetic filling factor, and circuit efficiency. Effects of non-ideal components and some data on construction materials are presented. Thermal engineering challenges, with reference to some recent solids probes, are also introduced.

1/28/08 .   Preprint available Solid State NMR Probe Design.
Download a preprint of “Solid State NMR Probe Design”, by F. David Doty, published in [Encyclopedia of Magnetic Resonance - Article posted online (www.interscience.wiley.com) on 12/15/07, Copyright © 1996, 2000, 2002, 2007 John Wiley & Sons, Ltd. All rights reserved, DOI: 10.1002/9780470034590.emrstm1001].

Abstract: An overview is presented of the special requirements for components found in NMR probes for solid samples, including high-power ceramic capacitors, variable capacitors, coils, construction materials, and spinner assemblies. Key data, including magnetic susceptibility and dielectric properties, are tabulated for the various ceramics, plastics, composites, and alloys often preferred in probe construction. Overviews are presented of the primary types of solids probes, including wideline, magic angle spinning, single crystal, and switched angle spinning. Some of the special design challenges are discussed in more detail, including spinner design, triple resonance high-power rf circuits, and operation at extreme temperatures.

2/16/07 .   Preprint available RF Coil Technology for Small-Animal MRI.
Download a preprint of “RF Coil Technology for Small-Animal MRI”, by F. David Doty, George Entzminger, Jatin Kulkarni, Kranti Pamarthy and John P. Staab, published in [NMR Biomed. 2007; 20: 304-325, published online in Wiley Interscience, at www.interscience.wiley.com, DOI: 10.1002/nbm.1149].

Abstract: A review of the theory, technology, and practice of RF coils for small-animal MRI is presented that includes a brief overview of MR S/N analysis and discussions of the various coils commonly used in small-animal MR – surface coils, linear volume coils, birdcages, and their derivatives. The scope is limited to mid-range coils – coils where the product (fd) of the frequency f and the coil diameter d is in the range of 2-30 MHz-m. Common applications include mouse brain and body coils from 125 MHz to 750 MHz, rat body coils up to 500 MHz, and small surface coils at all fields. In this regime, all the sources of loss (coil, capacitor, sample, shield, and transmission lines) are important. All such losses may be accurately captured in some modern full-wave 3D EM software, and new simulation results are presented for a selection of surface coils using Microwave Studio (MWS) 2006 by Computer Simulation Technology (CST), showing the dramatic importance of the “lift-off effect”. Standard linear circuit simulators have been shown to be useful in optimization of complex coil tuning and matching circuits. There appears to be considerable potential for trading S/N for speed using phased arrays, especially for a larger field of view. Circuit simulators are shown to be useful for optimal mismatching of ultra-low-noise preamps based on the E-PHEMT (Enhancement mode Pseudomorphic High Electron Mobility Transistor) for optimal coil decoupling in phased arrays. Cryogenically cooled rf coils are shown to offer considerable opportunity for future gains in S/N in smaller samples.

9/8/06 .   55% gain in S/N in OptiMASTM probe with DI-4 Spinner.
The earlier reported S/N gain of ~80% upon cooling of the Cold Zone in the OptiMAS probe to ~90 K was known to be partially due to sample cooling, but the exact amount was not accurately known due to thermometry limitations. The thermometry problems were fully solved, as reported on 8/31/06, and the glycine S/N experiments were repeated, this time with CP and high-power 1H decoupling. Without Cold Zone cooling, the S/N on this 300 MHz probe with the standard preamp (system NF~1.1 dB) was 64:1 on 13C, natural-abundance glycine, triple-tuning, 32 scans, RT, 7 kHz MAS. (This is a little less than on prior XC4 probes, as there are increased losses from the longer leads needed to accommodate auto sample exchange. Also the sample was not all α-glycine.) Upon cooling the cold zone to 85 K with the sample still at RT, the S/N increased 42% to 91:1. Then, upon changing to an ultra-low-noise preamp (system NF~0.7 dB), the S/N increased to 99:1. The benefit of a 0.4 dB drop in NF is much less (only ~4%) when all the coils and capacitors are at RT.

8/31/06 .   Dramatically improved MAS thermometry in the DI-4.
Problems with the previous VT gas flow control and thermocouple placement led to poor sample temperature accuracy when the Cold Zone in the first OptiMAS probe was cooled for S/N enhancement. The latest spinner revisions have completely solved these problems, and thermometry is now much better on the new 4mm “Drop-in” spinner, the DI-4, than on any of our previous MAS spinners. When the cold zone was at 85 K with the sample near RT, the difference between the temperature indicated by the sample thermocouple and the actual sample temperature, as measured by the chemical shift in PbNO3, was only ~3oC prior to calibration. The experiments were done in a triple-resonance fully equipped OptiMASTM probe at 7 T.

6/26/06 .   Preprint available Reducing Decoupler heating.
Download a preprint of “Using a Cross-coil to Reduce RF Heating by an Order of Magnitude in Triple-resonance Multinuclear MAS at High Fields”, by F. David Doty, Jatin Kulkarni, Christopher Turner, George Entzminger, and Anthony Bielecki, accepted for publication in Journal of Magnetic Resonance.

Abstract: Four different coil designs for use with MAS in triple-resonance multi-nuclear experiments at high fields are compared, using a combination of finite element analysis (FEA) software and NMR experiments, with respect to rf field strength per unit power and relative sample heating, as governed by mean E/B1 within the sample region. A simplified treatment of rf heating in NMR MAS samples is derived and shown to agree with the NMR experimental results within about 5% for two representative stator designs. The coil types studied include (1) a variable-pitch solenoid outside a ceramic coilform, (2) a conventional solenoid very closely spaced to the MAS rotor, (3) a scroll coil, and (4) a segmented saddle cross coil (XC) for 1H with an additional solenoid over it for the two lower-frequency channels. The XC/solenoid is shown to offer substantial advantages in reduced decoupler heating, improved S/N, and improved compatibility with multinuclear tuning and high-power decoupling.

4/20/06 .   OptiMAS Update.
We completed NMR experiments this week showing an increase in 13C S/N in the OptiMAS probe of 83% upon cooling of the Cold Zone to ~90 K. The increase was somewhat larger than expected, primarily because the sample and sample coil were also cooled more than expected. This probe included all the features planned for this product (as previously described) except the MAG coil, which will be added in the near future. Automatic sample exchange was shown to work very well.

2/24/06 .   OptiMAS Update.

We are expecting to have preliminary NMR data on the next-generation OptiMAS probe by the ENC in April 23.  

Our next-generation NMR MAS probe for fields up to 950 MHz will combine:

(1)   The highest S/N (we’ve been 30-80% beyond the competition*, now we’re taking it up another 50%);

(2)   Automatic sample exchange;

(3)   Order-of-magnitude lower decoupler heating than the solenoid (or half that of the scroll coil);

(4)   Highest resolution in a solids probe;

(5)   Highest spinner stability (axial vibrations under 2 microns rms);

(6)   Quad-resonance, multi-nuclear, H/X/Y/lock;

(7)   High-performance Magic Angle Gradient coil (250 G/cm at 500 MHz);

(8)   Extended VT range;

(9)   Outstanding tuning stability and robustness;

(10)   Lowest phase transients.

 

*The low-end of this S/N advantage range refers to low-loss samples.   For example, our XC-MAS gets over 200:1 on natural-abundance 13C glycine in a triple-resonance 750 MHz narrow-bore (or standard bore) probe, while competitors apparently get about 120-150 in such probes, depending on various probe features. We understand a competitor's 900 MHz 2.5 mm probe gets 50:1 on this same test.

Click here for a recent technical progress poster.

Click here for a copy of a presented talk on reducing decoupler heating in MAS by an order of magnitude.

 

 

2/5/06 .   Dramatically Improved Lineshape in Diffusion Probes.

We’ve not worried too much about the resolution and lineshape in our probes for self-diffusion measurements in liquids, as it’s usually not important in conventional diffusion experiments.   However, with the growing interest in diffusion-ordered spectroscopy (DOSY) and other HR techniques needing very high performance gradients, we realized we needed to better address the resolution and lineshape issues in diffusion probes.   We’ve re-designed the gradient coils with precise magnetic compensation and developed the needed precision magnetic compensation technology for the rf coils in liquids probes.   We anticipate NMR data (from both 5 mm and 10 mm diffusion probes) demonstrating resolution and lineshape in our diffusion probes (with 2000 G/cm gradients) that are competitive with state-of-the-art liquids probes.  

 

 

1/20/06 .   Improved Surface Coil Optimization.

Small surface coils at moderate fields (especially, for frequency-diameter products less than 5 MHz-m, such as a 25 mm coil at 200 MHz or less) were found to benefit much more than was previously expected from an increase in the conductor cross section.   The S/N benefit is greater than is indicated by either of the simple Q metrics commonly used (Q0/QL, or simply QL), as the larger conductor cross-section also improves magnetic filling factor from the reduction in the field intensity very near the conductor surface.   Going with a significantly heavier conductor makes it necessary to utilize zero-susceptibility conductors to minimize magnetic susceptibility artifacts.

 

Another important surface coil matter is decoupling from the transmit field.   We have switched from a simple diode clamp to a numerically optimized passive detuning network for more effective surface coil isolation from the transmitter.   We are considering beginning to develop pre-amp decoupling to allow surface coils to be positioned arbitrarily for array reception.


1/10/06 .   Ultra-stable MAS Spinner for Auto Sample Exchange.

A novel inflow Bernoulli axial bearing for MAS has been developed that provides exceptional axial stability as well as compatibility with automatic sample exchange.   Typical axial oscillations are under 2 microns rms (an order of magnitude improvement) over a wide range of spinning conditions.   The 3 mm rotor was spun to 30 kHz MAS, and the 4 mm rotor was spun to 23 kHz, as well as 0.5 Hz spectral resolution on 1H with liquids-like line shape.   The spinner designs are compatible with extended VT ranges, automatic sample exchange, ultra-low-E cross-coils, a magic-angle-gradient coil, and a ceramic dewar suitable for CryoMAS in which the sample is above RT and the coils are at 25 K. The improved axial stability is beneficial in improving spectral resolution and is essential in most gradient methods.

Click here for a more detailed abstract.

 

 

12/20/05 .   CryoMAS Update.

Steady progress continues in the development of a quad-resonance ( 1 H/ 13C/ 15N/lock) 3 mm CryoMAS probe (for wide-bores only) with full-range VT capability, automatic sample exchange, and high-performance magic-angle gradients.   We are initially expecting a factor-of-five gain in S/N (compared to available 3.2 mm MAS probes with auto sample exchange), and ultimately we anticipate a gain of a factor of eight.   The potential S/N gain in MAS appears to be greater than for the narrow-bore liquids cryoprobes mainly because the extra space available in the widebore allows for more effective minimization of the losses in all the circuit components.

 

We are expecting to have very preliminary NMR test data by the time of the ENC, April 23.  

Click here for a recent technical progress poster.

 

 

12/5/05 .   SAS progress.

Switched Angle Spinning (SAS) techniques are expected to provide useful dynamic control over bicelle alignment in protein structure determinations.   Two SAS probes suitable for such experiments in high-field magnets are into testing – one for wide bore and one for narrow bore magnets.   Each includes the following capabilities: very high efficiency multi-nuclear triple-resonance, field gradient coil, 25 ms sample flipping, and high resolution.   A novel 4 mm spinner compatible with automatic sample exchange demonstrated 10 kHz spinning while flipping in 25 ms.   The 600 MHz 7 mm 1H/X/Y SAS PFG probe achieved 55 kHz 1H decoupling with 120 W.   The latest WB version achieved angle reproducibility of 0.02 degree and lead lifetime of 300,000 flips.  

Click here for a more detailed abstract.

 

 

11/29/05 .   New Silicon-nitride Rotor Material Identified.

Kyocera has developed a very promising, new grade of Si3N4 , SN240, that appears to have better strength and toughness than any previous grade.   We are optimistic that this new material, along with improved processing, will allow us to offer thick-walled rotors rated to higher spinning speeds with greatly reduced chances of failure.   We are expecting to have preliminary test results on thick-walled rotors from this new material in early summer, 2006.  

 

 

11/3/05 .   Improved MAS Turbine Caps.

Glass-fiber-reinforced torlon grade 5030 will now be used on new MAS turbine caps (except for low proton Kel-F caps) for greatly improved VT performance and all-round better reliability and performance.   This new material stands out from the rest with respect to isotropic thermal expansion (only 16E-6/ oC), tensile strength at 200oC (120 MPa), and heat distortion temperature (282oC). It also has rather low moisture absorption, high wear resistance, and high impact strength.

Click here for more detailed information.

 

 

6/25/05.   High-performance Head Gradient Coil passes preliminary tests.

Preliminary tests were satisfactorily completed on a novel prototype head gradient coil.   The coil in all essential respects performed as expected from the detailed simulations.   The coil permits a substantial reduction in acoustic noise, a substantial increase in continuous gradient capability, and substantially reduced nerve stimulation.   The initial tests were performed at 1.5 T, and the coil is being sent to MGH for further testing at 3 T.   Work is beginning on the next generation, which will correct several deficiencies limiting current handling in the first prototype.   The next generation is expected to permit 70 mT/m continuous gradients in fields at least up to 8 T.

Click here for more detailed information.

 

 

4/10/05.   Double-balanced, Double-tuned 125 MHz Head Coil

Preliminary tests were carried out on a novel, double-balanced, double-tuned birdcage which permits more fully minimized sample losses on the high frequency channel than is obtained in prior designs.

Click here for more detailed information.

 

 

11/16/04.   500 MHz, 11 cm, hybrid birdcage.

An 8-section 500 MHz shielded hybrid birdcage of 11 cm diameter was completed and tested on baboon brain.   Performance agreed well with expectations from full-wave simulations using CST MWS 5.1, which showed that the capacitor ratios must be such that the coil is much closer to high-pass than low-pass conditions.   The coil tuned well over a wide range of samples, with excellent channel isolation.

Click here for more detailed information.

 

 

7/28/04.   Highest MAS S/N and Order of Magnitude Lower Decoupler Heating.

Simulation results and preliminary test results at 750 MHz, as reported in April, 2004, at the ENC in Asilomar, showed rf decoupler heating to be lower in the XC MAS probe by at least an order of magnitude compared to conventional solenoid probes.   Now, 13C test results on natural glycine show S/N to exceed 200:1 in the H/X/Y XC4 750 MHz probe.   This apparently exceeds that of competitors’ probes for use in narrow-bore magnets by 30-80%, depending on the various features.