Enhanced multi-nucLEar Generation, Acquisition, and Numerical Treatment of Nuclear Magnetic Resonance Spectrometer:
The ELEGANT NMR Spectrometer

with Real-Time In Situ Analysis

diameter of only 1 inch and length of about 10 inches

suitable for NS29 ground glass joint,

(industrial solutions up to 100 Bar are available upon request)

including all electronics



Patents pending: US62674050, US62677010, US15990662, US15990666, US15990667, EP18400012, EP18400013


Beginning with its inception over 60 years ago, Nuclear Magnetic Resonance (NMR) technology has been a powerful method for investigating the chemical compositions of matter and even the atomic structure of molecules. Currently, conventional NMR spectrometers are large, expensive, and very complex to operate.

Our innovations in numerical algorithms and hardware design have made it possible to produce an easy-to-use, pocket-sized NMR spectrometer, which we call the Elegant NMR Stick.

Now, NMR technology is available for:

  • universities and research institutions: for real-time monitoring of chemical synthesis
  • the chemical industry: for real-time, in situ monitoring of chemical processes and reactions
  • the oil and gas industry: for real-time droplet size and quality control
  • the beer/wine/soft drinks industries: for real-time quality control
  • the medical and pharmaceutical industry: for real-time, in situ quality control.

In addition to these uses, many other industrial facilities can profit from the use of a simple, robust, and affordable NMR spectrometer!

Elegant NMR Stick can work at temperatures up to 480℉/250℃

Suitable for nearly all chemical reactions, the Elegant NMR Stick provides real-time, in situ monitoring of key information for an advanced understanding and control of reactions without the need for extractive sampling.

The comprehensive nature of the data makes it especially useful for kinetic analyses. The elegant NMR Stick delivers in-depth reaction information, assisting organic chemists and scientists in their research and development of chemical compounds, synthetic chemical pathways, and chemical processes.

Key Idea

One of the biggest disadvantages of low-field NMR spectrometers is the high fluctuation of their magnetic fields. If the magnets are small (of a size appropriate to a portable device), the intensity and direction of the external magnetic field may be adversely affected. Even turning a 1.5 T NMR spectrometer to an angle about six degrees perpendicular to the Earth's magnetic force lines will ruin any measurements, and the device will have to be recalibrated. Even a slight movement of the table on which a spectrometer is placed may significantly disturb the spectra generated. Another related difficulty is that currently available spectrometers usually require high temperature stability (of the order of 0.01C), which is incompatible with chemical production equipment and in-situ measurements in chemical reactions.

To overcome these difficulties, we invented the following method: we should simultaneously perform measurements of at least two non-zero-spin isotopes or same non-zero-spin isotope in two different magnetic field with correlated oscillators:


where
S.1 Low-pass filter block that is used in parallel with all passed signals,
S.2 Receiver coil,
S.3 One or more sequentially-connected amplifiers,
S.4 A marker - a substance/mixture containing at least one non-zero-spin isotope with a priori known spectra and concentration - which is either:
  • situated in the measured substance, or
  • incorporated as the reference unit inside coils S.2, or
  • incorporated in the walls of the measuring NMR camera;
S.5 One or several frequency generators and their signals, delayed on 1/4 period. Each frequency generator has fixed ratio (An/Bn) to the main frequency generator;
S.6 A set of mixer pairs with each mixer pair receiving an appropriate pair of signals and delivering their products.
S.7 A processing block that incorporates the method described at FIG. 1.
S.8 A block that continuously supplies pipeline data u from S.7 into local storage and delivers it to processing block S.9.
S.9 A processing block that solves said minimization problem.

Ones this measurements occur, you may apply appropriate numerical algorithm and get out deviation of magnetic field and oscillators out of your measurements!

Detailed description of this method together with the algorithm as well as previously published important research papers are available at:

Additionally this fact opens possibility to perform 2D and multi-dimensional NMR spectra right out of this hardware and it is available by default from our hardware and software.

Background

All chemical elements are composed of one or more isotopes. Every isotope is either a zero-spin isotope or a non-zero-spin isotope.

Nuclear magnetic resonance (NMR) is a physical phenomenon in which non-zero-spin isotopes absorb and re-emit electromagnetic radiation (energy) when placed in an external magnetic field.

NMR occurs at a specific resonance frequency; this frequency has a linear relationship with the strength of the permanent magnetic field and the magnetic properties of isotopes in the target field. Resonance occurs when the absorbed alternate magnetic field is transmitted orthogonally in the direction of the permanent magnetic field.

NMR spectrometers and magnetic resonance imaging (MRI) devices generally comprise one or more magnets that produce a strong magnetic field within a test region. These magnets are usually superconducting magnets, thus NMR applications are restricted to laboratory environments. Currently, anisotropic permanent magnets, i.e. having all parts magnetized in one direction, can achieve magnetic fields of only 1.5 T in strength compared to the 23 T of superconductor magnets. The NMR signal response grows quadratically with regard to the magnetic field strength used in the experiment, which highly constrains the sensitivity and informativity of spectra produced by NMR spectrometers and/or MRI devices that have permanent magnets. NMR devices with permanent magnets are often referred to as low-field NMR spectrometers.

When permanent magnets are combined with several other parts having appropriate magnetization, it is possible to build a focused magnetic field of greater strength than the maximal field achievable with the permanent magnet alone. One well-known combination is the Halbach structure, introduced by Klaus Halbach in 1980, which makes a 5 T magnetic field possible with permanent magnets. This structure is often used in NMR spectrometers; however, it requires joining an enormous number of magnetized pieces. Doing so may be commercially ineffective, or unreasonably sophisticated when using magnets of small size.

The second problem characteristic of the Halbach structure is the high instability of the generated magnetic field in terms of both time and temperature if the same material is used throughout. Patent US8148988 describes a Halbach system that compensates for this drawback through using several permanent magnets of different materials, albeit it only obtains almost half of the maximally achievable magnetic field strength.

Halbach structures may be roughly classified as follows: 1D - linear, 2D - cylindrical, and 3D - spherical. The maximal achievable magnetic field strength for 1D structures - is 2B, for 2D - is B log Ro/Ri, and for 3D is 4/3 B log Ro/Ri, where B is the maximum achievable magnetic field for an anisotropic structure and Ro and Ri are the outer and inner radiuses of cylinders and/or spheres. This shows that 3D structures deliver the highest possible magnetic field: they are superior to 2D by a factor of 4/3, which increases sensitivity by almost a factor of 2!

At the same time, 3D structures require joining an enormous number of magnetized pieces, compared to 2D and 1D structures. They may be almost impossible to build in the case of small-sized, portable magnets, or they may not achieve the desired magnetic field because the process of gluing and joining reduces magnetic field strength.

In addition, one of the biggest disadvantages of low-field NMR spectrometers is the high fluctuation of their magnetic fields. If the magnets are small (of a size appropriate to a portable device), the intensity and direction of the external magnetic field may be adversely affected. Even turning a 1.5 T NMR spectrometer to an angle about six degrees perpendicular to the Earth's magnetic force lines will ruin any measurements, and the device will have to be recalibrated. Even a slight movement of the table on which a spectrometer is placed may significantly disturb the spectra generated. Another related difficulty is that currently available spectrometers usually require high temperature stability (of the order of 0.01C), which is incompatible with chemical production equipment and in-situ measurements in chemical reactions.

There are two well-known and widely-used primary approaches that improve the sensitivity of NMR measurements: multi-nuclear and multi-dimensional spectra acquisition and dynamic nuclear polarization (DNP).

The acquisition of multi-nuclear spectra usually requires one receiver coil for each type of nucleus and/or calibration of each spectrum to internal standards; this requirement makes it impractical to fit currently available NMR spectrometers into smaller, portable devices.

The DNP method polarizes the spins of electrons in molecules. The normally random spins of the many electrons situated around the nuclei being investigated blur the nuclei's response. DNP forces all electron spins to point in the same direction, enhancing the NMR response from non-zero-spin isotopes. This well-known, widely-established method was first developed by Overhauser and Carver in 1953, but at that time, it had limited applicability for high-frequency, high-field NMR spectroscopy due to the lack of microwave (or gigahertz) signal generators. The requisite generators, called gyrotrons, are available today as turn-key instruments, and this has rendered DNP a valuable and indispensable method, especially in determining the structures of various molecules by high-resolution NMR spectroscopy. However, gyrotrons remain cost-prohibitive because they require expensive components, i.e. high-voltage generators, independent permanent magnetic field generators, and deep vacuum devices such as turbomolecular pumps.

Currently, chemical analysis, particularly portable and benchtop analysis, is usually associated with chromatography devices. Chromatography is a laboratory technique for the separation of a mixture. The mixture is dissolved in a fluid called the mobile phase, which carries it through a structure holding another material called the stationary phase. The various constituents of the mixture have different partition coefficients and thus travel at different speeds, causing them to separate. Separated components are then flowed past a detector that is usually based on either conductivity or optical (UV, IR) absorption measurements. In some very rare cases, NMR may be used as detector or in parallel with a standard optical detector, but this is very restricted in application due to high equipment costs.

Chromatography has better sensitivity than NMR, but is less informative as the response of a chromatograph comprises only a retention time; no additional information about chemical composition is available. If the substance(s) in the mixture are unknown and need to be characterized, one must perform many different measurements, most likely with different chromatography columns and mobile phases, to conclusively identify the components.

In contrast, if NMR analysis is performed on one unknown substance, then a multidimensional NMR spectrum usually is sufficient to get all the information necessary for its identification, including not only its atomic composition but also the real spatial distribution of atoms in the molecule.

The straightforward combination of chromatography for separation with currently available NMR spectrometers for characterization is hindered by the inherent flaws of both methods: separation on a chromatographic column usually takes long periods of time (hours), and there is almost no control over how components separate; furthermore, the separated components are then flowed over the detector, remaining situated in the detector for only a few seconds (or even milliseconds). The vast majority of the time, the detector is filled with a known substance - the mobile phase. NMR detection itself requires a long time, usually hours, so that said straightforward combination of chromatography for separation with currently available NMR spectrometers requires slowing down the flow speed by several orders. These measurements occur on a timescale of several days or even weeks that is unrealistic in regards to commercial applications.

Taken together, prospective inventors of a portable NMR spectrometer for industrial environments and/or MRI devices must overcome the following problems:
  • construct a signal acquisition scheme that is stable despite fluctuations of the permanent magnetic field and/or of the signal generator, or that can work without a signal generator;
  • use NMR to detect all (or most) visible, non-zero-spin isotopes that are present in the investigated area;
  • construct a new device as a DNP polarizer that does not require high voltage generators, expensive deep vacuum devices such as turbomolecular pumps with size constrains, that that preferably use the same permanent magnetic field as the NMR transmitters;
  • construct compact magnets with Halbach or Halbach-like structures that have better magnetic field strengths and are resistant to large temperature range;
  • find an appropriate solution for using chromatography in conjunction with NMR to leverage the advantages of both methods.


Forum

News are now mainly posted at ResearchGate project page and at our forum. Do not hesitate to subscribe at the ResearchGate project for regular updates.

Order

We expect to keep the price low for the Elegant NMR Stick with free software so it can be made available for every user and every scientist. To do this, we request your kind support with advice, beta tests (only for customers that preordered 20+ Spectrometers), and preorders to be able to finish the development of the Elegant NMR Stick and produce them in large quantities.

As of begin of 2018, we have already built and successfully tested several devices, and staying on bugfixing stage and solving problems with discontinued components.



Powering of device is over PoE! New picture will be available soon. PoE adapter is included.

Warranty

Our warranty is 24 months from delivery day. The warranty is void in cases described in a datasheet chapter or in case of any mechanical/chemical/disassembly damage. We cannot provide a warranty for the strength of the magnet, because magnets can be demagnetized when placed in inappropriate conditions, e.g., near electromagnets or large iron parts. Our numerical method ensures that the device will work with different magnetic fields, so, if the magnetic field decays from 1.1 to 0.5 T, the Elegant NMR Stick will still collect data, but the measurement may take more time.

Based on our experience at normal conditions, the magnetic field decays very slowly, i.e., about 5-20% per year, so we do not expect that during first two years of usage you will have issues with the strength of the magnetic field.

New magnets may be ordered separately, or we may provide a refill of the magnets. Please, contact us for such cases.

About Elegant Mathematics

Elegant Mathematics was found in 1991 in the USA, (Washington State), for development and manufacture of linear systems and eigenvalue solvers for vector-pipelined and massively-parallel algorithms, that was requested by the industry of the nineties in the last century, for the solution of mathematical, physical, chemical, aerodynamic and other tasks. Our experts worked on the newest computer facilities of that time: 32 processor vector-pipelined system Cray C90, massively-parallel computers Cray T3D-T3E with 1,024 processors installed in NASA, Cray Research Inc, and the University of Pittsburgh, on many massively-parallel clusters with IRIX, DEC, RS6000, HP, Convex processors in the Hawaiian High-Performance Center, and on a huge amount of Linux clusters worldwide.

In the beginning of the 21st century our company underwent significant changes. There came a new generation of employees, we adjusted to new industrial problems and entered the European market.

In 2006 Elegant Mathematics Ltd moved its activity to Germany where its head office is situated at the present. The staff of our company are highly qualified specialists, who received Master's and PhD degrees on graduating from the worldwide recognized universities. Our mathematicians, physicists, chemists and programmers search out new technologies and directions in the industry. The results of their research and development activities are regularly published in scientific journals, such as Nature, JACS, LAA, etc. Hence, you are assured to find the high standard of scientific knowledge at your disposal.

Since 2017 we reestabliched our US office (Elegant Mathematics LLC) to be closer to our US customers.



Our Contacts

Elegant Mathematics Ltd,
Hanauer Muehle 2,
66564, Ottweiler-Fuerth,
Saarland
Germany
Tel: +49 6858 79 79 858
Email: info at elegant - math dot de


Elegant Mathematics LLC,
82834, WY, USA
Tel: +1 (631) 490 - 0521
Email: info at elegant - mathematics dot com


Legal registration numbers:
USA: Cheyenne 746213
UK: Cardiff 05975337
DE: HRB 16570
Active and registered since 23 Oct 2006
German tax payer's account number 030/146/00565
EU VAT account number DE 257663693
Customs number (EORI) DE 1753525

Our technical support and information office is always available for you. You can contact us at any time from any point of the world by our contact phones, and receive competitive guidance and consulting about our products and services in English and German languages.

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Please, discuss different aspects of Elegant NMR Stick, and general questions in applied mathematics, physics and chemistry related to NMR topics at ResearchGate Project Page or at our forum.