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Avance II+ 800 further info

Avance II+ - 800 MHz

This is the highest field NMR spectrometer operating in Portugal and it is configured for two distinct applications: high resolution liquid NMR spectroscopy (HR-NMR) and magic angle spinning NMR spectroscopy (MAS-NMR).

 

Using the HR-NMR configuration, the AvanceII+ 800 spectrometer is particularly suitable for structural studies of small to medium size molecules, and especially for the determination of three dimensional structures of proteins in solution. For HR-NMR acquisition, the spectrometer is equipped with three 5 mm inverse detection probe-heads (QXI-z C/N/P, TXI-z C/N and BBI-z, with broadband decoupling of X nuclei in the range from 31P to 109Ag). This set of probe-heads allows the acquisition of conventional multidimensional correlation spectra, such as COSY, NOESY, TOCSY, HSQC, HMQC, HMBC or combinations such as HSQC-TOCSY or HSQC-NOESY, and common triple resonance spectra like HNCA, HNCOCA, HNCB, HNCACB, etc., with or without the TROSY detection scheme for higher resolution in medium sized proteins. Apart from the experiments directed to structure determination, it is also possible to perform dynamic studies using relaxation data, fast proton/deuterium exchange (CLEANEX sequence), diffusion spectroscopy (DOSY), and J-resolved spectroscopy.

 

This spectrometer is also equipped with a 10 mm QNP C/N/P probe-head mainly intended for metabolomics and in vivo NMR studies in microorganisms, cells, tissues or small organs (those that will fit into 10 mm tubes) as well as a 5 mm BBO-z, with broadband decoupling of X nuclei (in the range from 31P to 109Ag) allowing the direct observation of less common nuclei such as Fluorine, Sodium, Potassium, and Cobalt, among others.

In its role as a MAS-NMR spectrometer, the AvanceII+ 800 is suitable for studies of liquid suspensions, semi-solid and solid samples of either biological or inorganic origin (for instance: conventional very small volume liquid samples, lipids, polymeric gels, biological tissues, plants, food samples, resins, glasses, ceramics, polymers, etc.).

 

For this purpose, the spectrometer is equipped with four probe-heads: a 4 mm HR MAS Triple H/C/N probe-head, specific for high resolution liquid or semi-solid samples, and three other probe-heads more appropriate for studies related with materials sciences (TriGamma MAS 3.2, TriGamma MAS 2.5 and LowGamma MAS 3.2 tunable for low frequency nuclei in the range of 49Ti to 23Na). Performing as solid state NMR spectrometer, high resolution homonuclear and heteronuclear correlation spectra can be acquired on the AvanceII+ 800 by applying MQ-MAS, CP/MAS techniques and heteronuclear X/Y correlation spectroscopy (for instance: REDOR, TEDOR, MQ-MAS HETCOR, etc.), taking advantage of the double broadband profile technology of some of these probe-heads.

 

Description and history of the equipment:

The spectrometer was acquired by the Rede Nacional de RMN (National NMR Network) in December 2006, and its installation completed in March 2007. The equipment, controlled via Topspin V.3.2 software installed on a PC with the LINUX operating system, comprises an AVANCE II+ double bay console and an 800 MHz compact Ultra-Shield-Plus Magnet with a 54 mm diameter bore. The 5 Gauss magnetic field safety line is described by an ellipsoid with a horizontal and vertical radius of 1.5 m and 2.5 m, respectively, from the magnetic center.

 

Three systems are available for low temperature operation:

  1. BCU-05 - a nitrogen gas cooling system (exit gas temperature of -20ºC) allowing working temperatures down to approximately 0ºC;
  2. BCU-EXTREME - a nitrogen gas cooling system (exit gas temperature of -70ºC) allowing working temperatures down to approximately -45ºC;
  3. A nitrogen gas cooling system operating by heat exchange with liquid nitrogen allowing working temperatures down to -120ºC.

 

 

Table of sensitivities (signal to noise ratios) for HR probe-heads:

Avance 800 II+

1H

13C

15N

31P

QXI-z (5 mm)

1593

351

15

160

TXI-z (5 mm)

1892

-

-

-

BBI-z (5 mm)

1736

303

5

212

BBO-z (5 mm)

662

523

76

301

QNP (10 mm)

6

1486

117

819

 

Table of sensitivities (signal to noise ratios) for MAS probe-heads:

Avance 800 II+

1H

13C

15N

31P

29Si

HR MAS (4 mm)

208.5

-

-

-

 

TriGamma MAS (3.2 mm)

-

96

25

9593

156

TriGamma MAS (2.5 mm)

-

37.7

26

5384

47.3

LowGamma MAS (3.2 mm)

-

71

40

-

61.5

 

 

QXI-z H-C/N/P

The QXI-z H-C/N/P-D (5mm) is a probe-head with inverse detection (optimized for 1H observing), designed to operate at four fixed frequencies (1H, 13C, 15N and 31P), with pulse-field gradients along Z axis and automatically tunable. This probe-head allows the acquisition of multi-dimensional triple resonance spectra from triple-labelled protein samples as well as less complex data from double- single- or non-labelled samples. In addition, the presence of a 31P channel allows the acquisition of multi-dimensional correlation data from phosphorylated compounds containing samples.

It is also possible to perform D decoupling using the deuterium channel from the lock system, together with the other three specific nuclei, allowing the decoupling up to four nuclei in only one pulse sequence.

 

Minimum sample volume: 500 ul
Working temperature range: +150 to -150ºC
Purchase date: 2007

 

TXI-z H-C/N

The TXI-z HH-C/N-D (5mm) is a probe-head with inverse detection (optimized for 1H observing), designed to operate at three fixed frequencies (1H, 13C and 15N), with pulse-field gradients along Z axis and automatically tunable. This probe-head allows the acquisition of multi-dimensional double resonance spectra from double-labelled protein samples as well as less complex data from single- or non-labelled samples. The tune/match range was modified by the manufacturer in order to deal with high salinity samples, like intracellular extracts, and allowing the best performances during structural analysis of low molecular weight compounds proceeding from metabolomics.

It is also possible to perform D decoupling using the deuterium channel from the lock system, together with the other two specific nuclei, allowing the decoupling up to three nuclei in only one pulse sequence.

 

Minimum sample volume: 500 ul
Working temperature range: +150 to -150ºC
Purchase date: 2007

 

BBI-z H-X

The BBI-z H-X-D (5mm) is a probe-head with inverse detection (optimized for 1H observing) and wide range frequency decoupling possibility (from 31P to 109Ag), with pulse-field gradients along Z axis and automatically tunable. It can be used for structural studies based on homonuclear (e.g., COSY, NOESY, TOCSY, etc.) or heteronuclear (e.g., HSQC, HMQC, HMBC, etc.) correlations and their combined forms. Also, this probe-head is frequently used for 1H-NMR experiments requiring heteronuclear decoupling and/or solvent suppression.

It is also possible to perform D decoupling using the deuterium channel from the lock system, together with a specific nucleus, allowing the decoupling of two nuclei in only one pulse sequence.

 

Minimum sample volume: 500 ul

Working temperature range: +150 a -150ºC
Purchase date: 2007

 

BBO-z X-H

The BBO-z X-H-D (5mm) is a wide frequency range direct observing (from 31P to 15N) and 1H decoupling probe-head, equipped with pulse-field gradients along Z axis and automatically tunable. Being optimized for X nuclei direct observation, it can lead to excellent results when studying compounds containing low natural abundance nuclei such as 13C, 29Si, 77Se, 119/117Sn, 111/113Cd, 185Re, etc.

 

Minimum sample volume: 500 ul

Working temperature range: +180 a -150ºC
Purchase date: 2007

 

QNP C/N/P-H

The QNP C/N/P-H-D (10mm) is a quadruple probe-head designed for direct observation of three fixed X nuclei frequencies (13C, 15N and 31P) and 1H decoupling if applicable. The possibility to accommodate 10mm NMR tubes allows performing in vivo NMR studies using cellular suspensions, small organs, etc. The probe-head is equipped with a pneumatic switching accessory for automatic changing of observed NMR frequency.

 

Minimum sample volume: 2.5 ml
Working temperature range: +150 a -130ºC
Purchase date: 2006

 

HR MAS H/C/N/D

The HR MAS Triple H/C/N/D (4mm) is a high-resolution triple resonance probe-head with Magic Angle Spinning rotation (max. rate: 15 kHz) designed for 1H, 13C and 15N direct observation and/or decoupling, and with pulse-field gradients along Z axis.. High-resolution NMR spectra of semi-solid (e.g.: paste, gels, resins, etc.) or liquid samples, from any origin (biological, organic or inorganic), can be obtained using this probe-head.

 

Maximum speed rotation: 15 kHz
Maximum sample volume: 50 ul

Working temperature range: +70 a -20ºC
Purchase date: 2010

 

TRIGAMMA MAS H/X/Y

The TriGama MAS H/X/Y (two different models for 3.2mm and 2.5mm rotors) is a solid state NMR probe-head with Magic Angle Spinning rotation and three acquisition independent channels; one channel exclusive for 1H-NMR acquisition and two broadband tunable channels (X/Y). The X channel can be used in the frequency range between 13C and 31P, while the Y channel can be used in the frequency range between 15N and 29Si. Specially build-up for MQ-MAS or CP/MAS techniques, it can also be used for the acquisition of heteronuclear X/Y correlation spectra and experiments like REDOR, TEDOR or HETCOR, combining a wide range of nuclei important on material science structural studies (27Al, 23Na, 17O, 31P, 29Si, 13C, 15N, etc.).

 

Model BL3.2:

Maximum speed rotation: 24 kHz
Maximum sample volume: 30 ul

Working temperature range: +100 a -50ºC
Purchase date: 2007

 

Model BL2.5:

Maximum speed rotation: 35 kHz
Maximum sample volume: 12 ul

Working temperature range: +50 a -50ºC
Purchase date: 2008

 

LOWGAMMA MAS H/X

The architecture and capabilities of LowGama MAS H/X (3.2mm) probe-head are similar to TriGamma MAS. Instead of two broadband channels, there is just one X channel tunable for low frequency nuclei (from 49Ti to 23Na).

 

Maximum speed rotation: 24 kHz
Maximum sample volume: 30 ul

Working temperature range: +100 a -50ºC
Purchase date: 2007