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ECZR NMR spectrometer

ECZR NMR spectrometer FT NMR systems

The ECZR NMR spectrometer (JNM-ECZR series), a member of the ECZ series of instruments, is a new research system that fully incorporates the latest digital and high frequency technologies.

rosette_wraply reliable, yet in a more compact size made possible by incorporating advanced integrated circuits, it supports even greater expandability options than current models for multi-channel operation, high power amplifiers and other accessories.

The bus line for control of attachments has been upgraded to even higher speed and enables highly accurate and rapid control.

Spectrometer Control Computer

The ECZ spectrometer control computer(SCC) is a high performance computer with large capacity hard disc, and is used for execution of pulse sequences, signal-to-noise calculation during measurement, storage of data, data processing, etc. are all possible and independent of the workstation.

All measured data is written to the SCC hard disc without fail, thus the SCC also serves as a data server.

Even if there is any kind of failure to the workstation computer or network during sequential measurements, all measurements that were submitted will be executed normally and the results will be written to the SCC’s disc.

Even in a multi-user environment where many users require different measurements and processing, stable operation of the instrument is assured.

Multi-Sequencer

The sequencer controls RF, lock and PFG channels during pulse sequence execution. The ECZR spectrometer can use multiple slave sequencers which control each of these channels, and a master sequencer which synchronizes all slave sequencers. Individual slave sequencers can execute pulse sequences irrespective of synchronous or asynchronous. Thus, by controlling several slave sequencers by the master sequencer, any NMR pulse sequence can be carried out.

Hence, the ECZR spectrometer can accommodate up to 8 nuclei, 32 frequency sources and PFG simultaneously. It can compile and execute any complex pulse sequence, even those that may be developed in the future.

STS (Smart Transceiver System)

The Smart Transceiver System (STS) is a highly advanced integration of RF sequencer, DDS (Direct Digital Synthesizer), FSU (Frequency Synthesizer Unit), transmitter, receiver, acquisition unit and gate control unit into a single transceiver board. This is equivalent to integrating the basic composition of an NMR system onto one board.

The standard instrument composition is one source with 2 nuclei, 8 frequencies and one receiver.

The ECZR spectrometer can accommodate up to four RF transceiver boards, and so can support 8 nuclei, 32 frequencies and 4 receivers.

Highly Precise Digital Control

The STS used in the ECZR spectrometer realizes control at the highest speed for frequency, phase and amplitude modulation, with a control time resolution of just 5ns. This high speed digital control is extremely useful for high speed phase modulation pulses which are required for the most recent NMR pulse sequences. The same time control performance is offered for various external systems.

  • 周波数変調

    ECZ Frequency modulation
    0 ( without modulation) → 10 MHz (with modulation)

  • 振幅変調

    ECZ Amplitude modulation
    0→100 %

  • 位相変調

    ECZ Phase modulation
    0→180°

High Performance DDS

The DDS (Direct Digital Synthesizer) unit of the ECZ spectrometer available from the STS, can create a very wide offset range.

Using an appropriate probe, this enables a “pseudo 3 nucleus” measurement with the standard instrument. For example, 13C{1H}{19F} measurement is possible with the standard configuration of ECZ spectrometers.

TFH Composition Example

TFH Composition Example

RF of 1H and 19F can be output at the same time.

  • 13C{1H}{19F − 80ppm}{19F − 212ppm}

  • 13C{1H}

13C spectrum of CF3CH(F)CF2OCH2CH3 measured on ECZ400S (one RF module only) and TFH probe.

Receiver

The receiver of the ECZ spectrometer is controlled by the sequencer. A reference frequency generated in the receiver can be dynamically modulated for phase and amplitude even during FID sampling.

DQD (Digital Quadrature Detection) by high speed A/D conversion at 16 bit 100 Msps, not only improves the effective dynamic range for quantized noise, but also reduces unwanted signals such as IMD, by over-sampling at high rates.

In addition, the digital receiver filter optimized for NMR ensures accurate quantitative results.

The high dynamic range of the ECZ spectrometer enables the observation of very small signals. The 13C satellite signals of acetone in a mixed sample of H2O:DMSO:Acetone=18570:104::1 (approx.10 % D2O) are clearly observed (approx.1/3400000).

Frequency characteristic of digital receiver 300 Hz step, 10 kHz range

As 13C satellite signals are 1.1 % at natural abundance, (approx. 0.55 % for each satellite peak) shows that a dynamic range of 1:3,400,000 has been achieved.

Multi-sequencer and Multi-dimensional NMR measurement

The ECZR spectrometer can control up to four RF sources, thus 8 nuclei and 32 frequencies, using the multisequencer method, with each RF source controlling 2 nuclei and 8 frequencies. Intelligent control of multiple RF sources enables not only highly precise execution of complex multi-dimensional NMR measurements, but allows the use of parallel expressions within the pulse sequence. In addition, by using conditional statements within a pulse sequence, more than one experiment is possible using the same pulse sequence program.

Digital NMR Lock Circuit

Hetero spin echo measurement of 1 % chloroform.

Application of STS technology provides high precision and high speed digital control of the 2H lock. This new digital feedback circuit offers extremely efficient control of the magnetic field against external modulation.

The precise digital lock feedback mechanism thus enables highly stable operation for protracted measurements.

Shimming

The gradient shim capability of the ECZ series is not limited to observation of deuterium (2H) as is normally used, but also other nuclei such as 1H or 19F. Such functionality is useful for “No-D NMR™” and can also be used for measurement of solids.

What is gradient shimming?
This is a high speed shimming method that measures the magnetic field distribution (magnetic field map) of the sample, compares it to a standard map then calculates and applies the required shim values for correction so that the magnetic field map becomes uniform.

  • Gradient shimming (2H)

    Gradient shimming

    Spectrum before and after resolution adjustment by gradient shimming. At 49 sec. resolution has improved.

  • Gradient shimming (1H)

    Gradient shimming

    No-D NMR measurement using resolution adjustment by selective pulse gradient shimming where the solvent has multiple signals (top). Solvent signal is automatically suppressed by the ‘WET’ method (bottom).

  • Gradient shimming (19F)

    Gradient shimming

    Resolution adjustment is possible by gradient shimming in the same manner as 2H, by selecting the 19F signal.

Temperature Control System

The temperature control system enables stable measurements using a newly-designed heater with improved response. The ECZ spectrometer allows faster and more stable operation of peripheral devices using the new high speed bus control line.

Chemical shift change of CH2 group and OH group of ethylene glycol with time (40 ℃).

Head Amplifier Chassis

The head amplifier chassis has various functions related to probe and the super conducting magnet. A touch-panel display is located on top of the head amplifier chassis, offering an intuitive user interface. During probe tuning, reflection dip and reflection value are indicated, whilst during cryogen refilling, the actual level of cryogen in the magnet is indicated in real time. It makes the routine maintenance related to probes and super conducting magnet convenient and efficient.

  • Gradient shimming

    Head Amplifier Chassis

  • Gradient shimming

    Indication of reflection dip when probe tuning.

  • Gradient shimming

    Indication of remaining quantity when refilling Helium.

Power Amplifier

The Power Amplifier amplifies the RF pulse and outputs it to the probe. Various models are available depending on the purpose but all power amplifiers exhibit excellent linearity and response performance.

The ECZ spectrometer is designed so that the power amplifier keeps constant thermal stability, regardless of output / non-output of RF pulses. Thus stable RF output is achieved for every kind of measurement, regardless of number of pulses, pulse widths, intervals etc. used within the pulse sequence.

HF (rosette_wrapt Freq.) LF (Low Freq.) Remarks
50W 150W Liquid only (ECZS)
100W 300W Standard liquid & solid
200W 500W Standard liquid & solid
500W 1,000W Advanced solid
1,000W 2,000W Advanced solid

PFG(Pulsed Field Gradient)

PFG (Pulsed Field Gradient) control by STS (Smart Transceiver System) technology offers technical advantages.
The new PFG control offers higher precision and stability for measurements that requires highly precise control such as DOSY, etc.

PFG Amplifier
For the ECZR series, two models of PFG amplifier with different power outputs, 10 A and 30 A. are available. Please discuss with your local JEOL representative which is more suitable for your application.

Improved functionality and unique design

The spectrometer features enhanced functionality, ease of operation,and an attractive design.

Intuitive control software

Incorporating an additional interface for simple, routine operation, the Delta software for spectrometer control and data processing supports both simple and sophisticated applications. A minimum sequence of operation is needed for routine, standard analysis, such as selection of a solvent or measurement mode. For more complicated analysis with numerous conditions, the system will automatically define hardware parameters, including those for the spectrometer and probe, allowing the operator to set up only the conditions specific to the sample or research objective.

Flexible room layout

Compared to the JNM-ECAⅡ series, the spectrometer requires a 67 % more compact size.

All system units, including the magnet and compact auto multi sample changer, can be laid out efficiently in a small room.

Solid measurement

ECZR enables measurement not only of solutions, but also of various solid state NMR samples. The spectrometer is compatible with many optional probes including:-

* world’s fastest sample spinning 0.75mmφ,
* ultra fast 1mmφ MAS probe,
* convenient 4mmφ,
* HXMAS probe 3.2mmφ,
* large capacity 8mmφ,
* FGMAS for semi-solids.

A newly-developed MAS controller controls sample spinning from low speeds to high speeds, safely and stably.
In combination with the highly stable RF control of ECZ, it can accommodate many solid state sample measurements.

Sample:L-histidine HCl H2O
Instrument:JNM-ECA600/ECZ600R

An NMR in the Network Age

With the ECZ series, the spectrometer and workstation each have their own independent computers, being connected through a network. Therefore, measurements are possible by any authorized computer and user on the network.

Since the spectrometer computer executes all measurements and initial data storage, it

Installation Requirements

Power supplies required for installation
Spectrometer Single phase AC100V to 240V, 50/60Hz 3kVA
Data system Single phase AC100V to 240V, 50/60Hz 1kVA
Air Compressor (400MHz) Single phase AC100V, 50/60Hz 30A
Air Compressor
(500MHz or higher)
Three phase AC200V, 50/60Hz 30A
Backup Single phase AC100/120V, 50/60Hz 3kVA
Ground resistance 100Ω or lower

Note : Long term low temperature air supplier (option) needs separate power supply.

Installation room 500MHz
Temperature range 17 to 27 °C (fluctuation:1°C/h or less)
Humidity 70% or less
Ceiling height 2.87 m or more (top of the SCM)
0.5mT position Vertical: 1.15 m from SCM center
Radial: 0.60 m from SCM center

The layout picture above is an example of the ECZR instllation room.Recommend room layout may vary depending on the spectrometer configuration and apparatus in the room.